CN115417950A - Temperature-sensitive fluid loss agent for well cementation cement slurry and preparation method thereof - Google Patents
Temperature-sensitive fluid loss agent for well cementation cement slurry and preparation method thereof Download PDFInfo
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- CN115417950A CN115417950A CN202211373373.4A CN202211373373A CN115417950A CN 115417950 A CN115417950 A CN 115417950A CN 202211373373 A CN202211373373 A CN 202211373373A CN 115417950 A CN115417950 A CN 115417950A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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- 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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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a temperature-sensitive fluid loss agent for well cementation cement slurry, which belongs to the field of oilfield chemistry and is prepared from the following components in percentage by mass: 4.999-19.996% of hydrophilic monomer, 4-9.998% of temperature sensitive monomer, 69.986-89.991% of water and 0.01-0.04% of initiator. The invention also discloses a preparation method of the temperature-sensitive fluid loss additive for well cementation cement slurry. The invention can play the temperature-sensitive dehydration reducing function for well cementation cement slurry and can improve the temperature resistance.
Description
Technical Field
The invention relates to the field of oilfield chemistry, in particular to a temperature-sensitive fluid loss additive for well cementation cement slurry and a preparation method thereof.
Background
With the increasing demand of energy and the deepening of oil field exploration and development, the high-temperature deep well and ultra-deep well gradually become the focus of exploration and development. High temperature and ultrahigh temperature put higher requirements on the performance of the cement paste. The following difficulties mainly exist in the high-temperature deep well cementing process: (1) The water loss of the cement paste at high temperature and ultrahigh temperature is large and even uncontrollable, so that the construction safety risk exists; (2) The sedimentation stability of the cement slurry under high temperature and ultrahigh temperature is poor, and the solid phase is easy to settle in the pump stopping process, so that potential safety hazards are caused; (3) the cement slurry thickening time is difficult to adjust.
At present, the polymer fluid loss additive mainly comprises natural polymer and synthetic polymer. The natural high molecular polymers including cellulose, cellulose derivatives, lignin, starch and other natural high molecular polymers have the advantages of easily available materials and low price, but have the problems of small temperature range adaptability, poor product quality stability, easy degradation at high temperature and the like. The synthetic high molecular polymer comprises nonionic, anionic, cationic and zwitterionic polymers, and the synthetic high molecular fluid loss agent has various varieties and excellent performance, but has the defects of strong high-temperature dispersibility, too high viscosity of a slurry system, poor compatibility and influence on cement hydration reaction to reduce the cement strength.
Disclosure of Invention
The invention aims to: providing a temperature-sensitive fluid loss agent for well cementation cement slurry and a preparation method thereof; the preparation method has the advantages of simple operation, mild reaction conditions, high conversion rate, low requirements on equipment and environment, and easy realization of industrial batch production of the fluid loss agent; the temperature-sensitive fluid loss agent prepared by the method can effectively reduce the amount of fluid loss, and has good chemical property, high temperature resistance and excellent performance.
The invention is realized by the following technical scheme:
a temperature-sensitive fluid loss agent for well cementation cement slurry is prepared from the following components in percentage by mass: 4.9990-19.9960% of hydrophilic monomer, 4-9.9980% of temperature-sensitive monomer, 69.9860-89.9910% of water and 0.0100-0.0400% of initiator;
the hydrophilic monomer is at least one of sodium p-styrenesulfonate, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and N-vinyl pyrrolidone;
the temperature-sensitive monomer is at least one of N, N-dimethylacrylamide and N-isopropylacrylamide.
The initiator is at least one of potassium persulfate and ammonium persulfate.
A preparation method of the temperature-sensitive fluid loss agent for well cementation cement slurry comprises the following steps:
step 2, after the primary reaction liquid is obtained, introducing nitrogen into the reaction kettle, stirring and heating to 50-70 ℃ to obtain an intermediate reaction liquid;
step 3, adding an initiator into the residual water to obtain an initiating solution;
step 4, heating the intermediate reaction liquid obtained in the step 2, adding an initiating solution into the intermediate reaction liquid, and carrying out heat preservation reaction for 4-7 hours to obtain a solution reactant;
and 5, freeze-drying the solution reactant to obtain the temperature-sensitive fluid loss agent for the well cementation cement slurry.
In the step 4, the intermediate reaction liquid obtained in the step 2 is heated to 50-70 ℃ and is kept at 50-70 ℃.
In the step 4, the synthesis process of the heat preservation reaction is as follows:
in the step 5, the solution reactant is sequentially frozen, dried and crushed to obtain the product.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) The temperature-sensitive fluid loss additive for well cementation cement slurry has double fluid loss reducing effects. On one hand, the amido and sulfonic acid groups in the molecular structure of the temperature-sensitive fluid loss additive for well-cementing cement slurry have a complexing effect on calcium ions in cement to form a certain structure, so that water is wrapped and the temperature-sensitive fluid loss effect for the well-cementing cement slurry is exerted; on the other hand, in the temperature-sensitive fluid loss agent for well-cementing cement slurry, the water solubility of hydrophobic groups of temperature-sensitive monomers is weakened at high temperature, and the temperature-sensitive monomers are mutually aggregated to form associated hydrophobic micro-regions, so that a reversible physical network structure is promoted to be formed, the hydrodynamic volume of a polymer and the viscosity stability at high temperature are improved, and the temperature-sensitive fluid loss effect for well-cementing cement slurry is exerted;
(2) The temperature-sensitive fluid loss agent for well cementation cement slurry has excellent temperature resistance, and the temperature resistance can reach 200 ℃ at most. In the molecular structure of the temperature-sensitive fluid loss agent for well cementation cement slurry, the temperature resistance of the temperature-sensitive fluid loss agent for well cementation cement slurry is improved by being similar to a network structure.
Drawings
FIG. 1 is a graph showing the thermogravimetric loss of the temperature-sensitive fluid loss agent for well-cementing slurry prepared in example 1;
FIG. 2 is a graph showing the thermogravimetric loss curve of the temperature-sensitive fluid loss agent for well cementation cement slurry prepared in example 2;
FIG. 3 is a graph showing the thermogravimetric loss curve of the temperature-sensitive fluid loss agent for well cementation cement slurry prepared in example 3;
FIG. 4 is a graph showing the thermogravimetric loss of the temperature-sensitive fluid loss additive for well-cementing cement slurry prepared in example 4.
Detailed Description
All of the features disclosed in this specification, or all of the steps of any method or process so disclosed, may be combined in any combination, except features and/or steps which are mutually exclusive, unless expressly stated otherwise, or alternatively, any other feature which is equivalent or which serves the same purpose may be substituted for the alternative features shown, i.e. each feature may be embodied in only one embodiment in a single series of equivalent or similar features, unless expressly stated otherwise.
The invention relates to a temperature-sensitive fluid loss agent for well cementation cement slurry, which is prepared from the following components in percentage by mass: 4.9990-19.9960% of hydrophilic monomer, 4-9.9980% of temperature-sensitive monomer, 69.9860-89.9910% of water and 0.0100-0.0400% of initiator.
The hydrophilic monomer is sodium p-styrenesulfonate, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and N-vinyl pyrrolidone.
The temperature-sensitive monomer is N, N-dimethylacrylamide and N-isopropylacrylamide.
The initiator is at least one of potassium persulfate and ammonium persulfate.
The percentages in the following examples are by mass unless otherwise specified.
Example 1
The invention relates to a preparation method of a temperature-sensitive fluid loss agent for well cementation cement slurry, which comprises the following steps:
step 2, after the primary reaction liquid is obtained, introducing nitrogen into the reaction kettle for 10min, and heating to 65 ℃ under the stirring condition of 200r/min to obtain an intermediate reaction liquid;
step 3, adding 0.0200% of ammonium persulfate initiator into the residual 9.9980% of water to obtain an initiating solution;
step 4, after the intermediate reaction liquid in the step 2 is heated to 65 ℃, adding an initiating solution into the intermediate reaction liquid within 10min, and continuously carrying out heat preservation reaction for 5 hours at 65 ℃ to obtain a solution reactant;
and 5, sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive fluid loss agent for well cementation cement slurry.
Example 2
The invention relates to a preparation method of a temperature-sensitive fluid loss agent for well cementation cement slurry, which comprises the following steps:
step 2, after the primary reaction liquid is obtained, introducing nitrogen into the reaction kettle for 10min, and heating to 60 ℃ under the stirring condition of 200r/min to obtain an intermediate reaction liquid;
step 3, adding 0.0400% ammonium persulfate initiator into the residual 9.9960% of water to obtain an initiating solution;
step 4, after the temperature of the intermediate reaction liquid in the step 2 is raised to 60 ℃, adding an initiating solution into the intermediate reaction liquid within 10min, and continuously carrying out heat preservation reaction for 4 hours at the temperature of 60 ℃ to obtain a solution reactant;
and 5, sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive fluid loss agent for well cementation cement slurry.
Example 3
The invention relates to a preparation method of a temperature-sensitive fluid loss agent for well cementation cement slurry, which comprises the following steps:
step 1: adding 79.9920% of water into a reaction kettle, adding 4.0000% of temperature-sensitive monomer and 5.9990% of hydrophilic monomer into the reaction kettle, stirring and dissolving completely, and adjusting the pH value of the solution in the reaction kettle to 10 to obtain primary reaction liquid; wherein, the temperature-sensitive monomer is N-isopropyl acrylamide, 5.9990 percent of hydrophilic monomer comprises 1.9997 percent of sodium p-styrene sulfonate and 3.9993 percent of 2-acrylamide-2-methyl propanesulfonic acid;
and 2, step: after primary reaction liquid is obtained, introducing nitrogen into the reaction kettle for 10min, and heating to 70 ℃ under the stirring condition of 200r/min to obtain intermediate reaction liquid;
and 3, step 3: adding 0.0100% of ammonium persulfate initiator into the remaining 9.9990% of water to obtain an initiating solution;
and 4, step 4: after the intermediate reaction liquid in the step 2 is heated to 70 ℃, adding the initiating solution obtained in the step 3 into the intermediate reaction liquid within 30min, and continuously carrying out heat preservation reaction for 4.5h at 70 ℃ to obtain a solution reactant;
and 5: and (4) sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive fluid loss agent for the well cementation cement slurry.
Example 4
The invention relates to a preparation method of a temperature-sensitive fluid loss agent for well cementation cement slurry, which comprises the following steps:
step 2, after primary reaction liquid is obtained, introducing nitrogen into the reaction kettle for 30min, and heating to 50 ℃ under the stirring condition of 500r/min to obtain intermediate reaction liquid;
step 3, adding 0.0290% of potassium persulfate initiator into the residual 19.9940% of water to obtain an initiating solution;
step 4, after the temperature of the intermediate reaction solution in the step 2 is raised to 50 ℃, adding an initiating solution into the intermediate reaction solution within 60min, and continuously carrying out heat preservation reaction for 7 hours at 50 ℃ to obtain a solution reactant;
and 5, sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive fluid loss agent for well cementation cement slurry.
In step 4 of the above examples 1 to 4, the synthesis process of the incubation reaction is as follows:
the temperature-sensitive fluid loss agent for well cementation cement paste prepared by the embodiment is subjected to performance test, cement paste is prepared according to the GB/T19139-2003 standard, the temperature-sensitive fluid loss agent for well cementation cement paste prepared by the method is tested for the fluid loss effect, the retardation performance and the strength at different temperatures, and the formula of the cement paste is as follows: g-grade cement, 35% of silica powder, a temperature-sensitive fluid loss additive for well cementation cement slurry, a retarder and water, wherein the water-cement ratio is 0.44.
Table 1 Table of cement slurry performance test results prepared by adding the temperature-sensitive fluid loss additive for well cementation cement slurry obtained in examples 1 to 4
As can be seen from the test results in Table 1, the temperature-sensitive fluid loss control agents for well cementation cement slurries obtained in examples 1 to 4 have good rheological control over the cement slurries, and have stable fluid loss control, and the API fluid loss can be controlled below 50ml under the conditions of 150 ℃ and 200 ℃. The high-pressure water loss at 150 ℃ is between 26 and 42mL, and most of the water loss is less than 40mL; the thickening time is proper; the compressive strength is higher between 20 and 26MPa, and most of the compressive strength is more than 22MPa; the sedimentation stability is good at 0.1-0.2 g/cm 3 The sedimentation stability of most of them was 0.1 g/cm 3 (ii) a The fluidity is better between 21 cm and 22.5cm at normal temperature, and most of the fluidity is more than 22cm.
For the structural characterization of the temperature-sensitive fluid loss agent for well-cementing cement slurry, fig. 1 shows the thermal weight loss curve of the temperature-sensitive fluid loss agent for well-cementing cement slurry prepared in example 1.
As can be seen from FIG. 1, (1) 22.91-116 ℃, the mass fraction of the polymer molecule loss by heat at this stage is about 7.47% due to the fact that part of hydrophilic groups exist on the polymer molecular chain, which are easy to absorb water and damp, and the crystal water contained in the polymer molecule volatilizes when heated; (2) 116-250.14 ℃, the polymer molecules are not greatly changed by heating in the stage, and the mass fraction of heat loss is about 1.29 percent; (3) 250.14-485.86 ℃, the main chain of the polymer is broken by heating at the stage, and the mass fraction of the polymer molecule loss by heating is about 47.06%; (4) 485.86-600 ℃, the mass fraction of the polymer molecule lost by heat at this stage is about 5.52%, mainly because the polymer molecular chain is carbonized at high temperature, and the final residual mass fraction of the polymer is 38.76%. In conclusion, the molecular chain of the polymer has no obvious fracture decomposition phenomenon before 250.14 ℃, and the temperature-sensitive fluid loss agent for well cementation cement slurry has good high temperature resistance.
FIG. 2 is a thermogravimetric curve of the temperature-sensitive fluid loss additive for well-cementing cement prepared in example 2, wherein the molecular chain of the temperature-sensitive fluid loss additive for well-cementing cement does not have obvious fracture decomposition phenomenon before 272 ℃; FIG. 3 is a thermogravimetric curve of the temperature-sensitive fluid loss additive for well-cementing cement prepared in example 3, wherein the molecular chain of the temperature-sensitive fluid loss additive for well-cementing cement does not have obvious fracture decomposition phenomenon before 264 ℃; fig. 4 is a thermogravimetric curve of the temperature-sensitive fluid loss additive for well-cementing cement prepared in example 4, wherein the molecular chain of the temperature-sensitive fluid loss additive for well-cementing cement has no obvious fracture decomposition phenomenon before 260 ℃.
The thermogravimetric curve data of the four embodiments show that the temperature resistance of the temperature-sensitive fluid loss additive for well cementing cement slurry is above 250 ℃, and the temperature-sensitive fluid loss additive has good high-temperature resistance.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modifications and equivalent variations of the above embodiment according to the technical spirit of the present invention are within the scope of the present invention.
Claims (6)
1. A temperature-sensitive fluid loss agent for well cementation cement slurry is characterized by being prepared from the following components in percentage by mass: 4.9990-19.9960% of hydrophilic monomer, 4.0000-9.9980% of temperature-sensitive monomer, 69.9860-89.9910% of water and 0.0100-0.0400% of initiator;
the hydrophilic monomer is at least one of sodium p-styrenesulfonate, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and N-vinyl pyrrolidone;
the temperature-sensitive monomer is at least one of N, N-dimethylacrylamide and N-isopropylacrylamide.
2. The temperature-sensitive fluid loss agent for the well cementation cement slurry as claimed in claim 1, wherein the initiator is at least one of potassium persulfate and ammonium persulfate.
3. A preparation method of the temperature-sensitive fluid loss additive for the well cementation cement slurry as claimed in any one of claims 1 to 2 is characterized by comprising the following steps:
step 1, adding part of water into a reaction kettle, adding a hydrophilic monomer and a temperature-sensitive monomer into the reaction kettle, stirring and dissolving completely, and adjusting the pH value of a solution in the reaction kettle to 9-11 to obtain a primary reaction solution;
step 2, after the primary reaction liquid is obtained, introducing nitrogen into the reaction kettle, stirring and heating to 50-70 ℃ to obtain an intermediate reaction liquid;
step 3, adding an initiator into the residual water to obtain an initiating solution;
step 4, heating the intermediate reaction liquid obtained in the step 2, adding an initiating solution into the intermediate reaction liquid, and carrying out heat preservation reaction for 4-7 hours to obtain a solution reactant;
and 5, freeze-drying the solution reactant to obtain the temperature-sensitive fluid loss agent for the well cementation cement slurry.
4. The method according to claim 3, wherein in the step 4, the temperature of the intermediate reaction solution obtained in the step 2 is raised to 50 to 70 ℃ and maintained at 50 to 70 ℃.
5. The preparation method according to claim 3, wherein in the step 4, the synthesis process of the heat preservation reaction is as follows:
6. the preparation method according to claim 3, wherein in the step 5, the solution reactant is sequentially subjected to freezing, drying and crushing to obtain the product.
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