CN115417950B - Temperature-sensitive fluid loss agent for well cementation cement paste and preparation method thereof - Google Patents
Temperature-sensitive fluid loss agent for well cementation cement paste and preparation method thereof Download PDFInfo
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- CN115417950B CN115417950B CN202211373373.4A CN202211373373A CN115417950B CN 115417950 B CN115417950 B CN 115417950B CN 202211373373 A CN202211373373 A CN 202211373373A CN 115417950 B CN115417950 B CN 115417950B
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- 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
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Abstract
The invention discloses a temperature-sensitive fluid loss agent for well cementation cement paste, 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 agent for the well cementation cement paste. The invention can exert the temperature-sensitive water loss reducing effect for the well cementation cement paste 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 agent for well cementation cement paste and a preparation method thereof.
Background
Along with the continuous increase of energy demand and continuous deep exploration and development of oil fields, a high-temperature deep well and an ultra-deep well gradually become the focus of exploration and development. And the cement paste performance is required to be higher at high temperature and ultrahigh temperature. The following difficulties mainly exist in the high-temperature deep well cementation process: (1) The water loss of cement paste becomes large and even uncontrollable at high temperature and ultrahigh temperature, and construction safety risks exist; (2) The sedimentation stability of cement paste is poor at high temperature and ultra-high temperature, and the solid phase is easy to sediment in the process of stopping the pump, so that potential safety hazard is caused; (3) the cement paste thickening time is difficult to adjust.
Currently, high molecular weight fluid loss additives mainly comprise natural high molecular polymers and synthetic high molecular polymers. The natural high molecular polymer comprises cellulose and cellulose derivatives, lignin, starch and other natural high molecular polymers, has the advantages of easily available materials and low price, but also has the problems of small adaptability in temperature range, poor quality stability of products, easy degradation at high temperature and the like. The synthetic high molecular polymer comprises nonionic, anionic, cationic and zwitterionic polymers, has various types of synthetic high molecular fluid loss agents and excellent performance, but has strong high-temperature dispersibility, too high viscosity of a slurry system, poor compatibility and influences the hydration reaction of cement to reduce the strength of the cement.
Disclosure of Invention
The invention aims at: providing a temperature-sensitive fluid loss agent for well cementing slurry and a preparation method thereof; the preparation method is simple to operate, mild in reaction condition, high in conversion rate, low in equipment and environment requirements, and easy to realize industrialized mass production of the fluid loss agent; the temperature-sensitive fluid loss agent prepared by the method can effectively reduce the water loss, and has good chemical property, high temperature resistance and excellent fluid loss agent performance.
The invention is realized by the following technical scheme:
a temperature-sensitive fluid loss agent for well cementation cement paste is prepared from the following components in percentage by mass: 4.9990 to 19.9960 percent of hydrophilic monomer, 4 to 9.9980 percent of temperature-sensitive monomer, 69.9860 to 89.9910 percent of water and 0.0100 to 0.0400 percent 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-isopropyl acrylamide.
The initiator is at least one of potassium persulfate and ammonium persulfate.
The preparation method of the temperature-sensitive fluid loss agent for the well cementation cement paste comprises the following steps:
step 2, after obtaining a primary reaction liquid, 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, then adding an initiating solution into the intermediate reaction liquid, and reacting for 4-7 hours at a constant temperature to obtain a solution reactant;
and 5, freeze-drying the solution reactant to obtain the temperature-sensitive filtrate reducer for the well cementation cement paste.
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 agent for well cementation cement paste has the dual fluid loss reducing effect. On one hand, the amido and sulfonic acid groups in the molecular structure of the temperature-sensitive filtrate reducer for the well cementing slurry have complexation effect on calcium ions in the cement to form a certain structure, wrap water and play a role in temperature-sensitive filtrate reducer for the well cementing slurry; on the other hand, the water solubility of the hydrophobic groups of the thermosensitive monomer in the thermosensitive fluid loss agent for well cementation cement paste is weakened at high temperature, and the hydrophobic groups are mutually aggregated to form associated hydrophobic micro-areas, so that the formation of a reversible physical network structure is promoted, the physical volume of polymer fluid and the viscosity stability at high temperature are improved, and the thermosensitive fluid loss effect for well cementation cement paste is exerted;
(2) The temperature-sensitive fluid loss agent for well cementation cement paste has excellent temperature resistance, and the highest temperature resistance can reach 200 ℃. In the molecular structure of the temperature-sensitive fluid loss agent for well cementation cement paste, the temperature resistance of the temperature-sensitive fluid loss agent for well cementation cement paste is improved like a network structure.
Drawings
Fig. 1 is a graph of thermal weight loss of a temperature-sensitive filtrate reducer for well cementing slurry prepared in example 1;
fig. 2 is a graph of thermal weight loss of the temperature-sensitive filtrate reducer for well cementing slurry prepared in example 2;
fig. 3 is a graph of thermal weight loss of the temperature-sensitive filtrate reducer for well cementing slurry prepared in example 3;
fig. 4 is a graph of thermal weight loss of the temperature-sensitive filtrate reducer for well cementing slurry prepared in example 4.
Detailed Description
All the features disclosed in this specification, or the steps of all methods or processes disclosed, except for the mutually exclusive features and/or steps, may be combined in any combination, unless specifically stated otherwise, with other equivalents or alternatives having a similar purpose, i.e., each feature is one embodiment of a series of equivalents or similar features, unless specifically stated otherwise.
The invention relates to a temperature-sensitive fluid loss agent for well cementation cement paste, 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 monomers are sodium p-styrenesulfonate, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and N-vinyl pyrrolidone.
The temperature-sensitive monomer is N, N-dimethylacrylamide or N-isopropyl acrylamide.
The initiator is at least one of potassium persulfate and ammonium persulfate.
Unless otherwise specified, the percentages in the examples hereinafter are mass percentages.
Example 1
The invention discloses a preparation method of a temperature-sensitive fluid loss agent for well cementation cement paste, which comprises the following steps:
step 2, after obtaining a primary reaction liquid, 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% ammonium persulfate initiator into the residual 9.9980% water to obtain an initiation 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 continuing to perform heat preservation reaction for 5h at 65 ℃ to obtain a solution reactant;
and 5, sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive filtrate reducer for the well cementation cement paste.
Example 2
The invention discloses a preparation method of a temperature-sensitive fluid loss agent for well cementation cement paste, which comprises the following steps:
step 2, after obtaining a primary reaction liquid, 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% water to obtain an initiation solution;
step 4, after the intermediate reaction liquid in the step 2 is heated to 60 ℃, adding an initiating solution into the intermediate reaction liquid within 10min, and continuing to perform heat preservation reaction for 4h at 60 ℃ to obtain a solution reactant;
and 5, sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive filtrate reducer for the well cementation cement paste.
Example 3
The invention discloses a preparation method of a temperature-sensitive fluid loss agent for well cementation cement paste, 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 regulating the pH value of the solution in the reaction kettle to 10 to obtain a primary reaction solution; wherein the temperature-sensitive monomer is N-isopropyl acrylamide, and 5.9990 percent of hydrophilic monomer comprises 1.9997 percent of sodium p-styrene sulfonate and 3.9993 percent of 2-acrylamide-2-methylpropanesulfonic acid;
step 2: after the 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 an intermediate reaction liquid;
step 3: adding 0.0100% ammonium persulfate initiator into the residual 9.9990% water to obtain an initiation solution;
step 4: after the intermediate reaction liquid in the step 2 is heated to 70 ℃, adding the initiation solution obtained in the step 3 into the intermediate reaction liquid within 30min, and continuing to react at the temperature of 70 ℃ for 4.5h to obtain a solution reactant;
step 5: and sequentially freezing, drying and crushing the solution reactant to obtain the temperature-sensitive filtrate reducer for the well cementation cement paste.
Example 4
The invention discloses a preparation method of a temperature-sensitive fluid loss agent for well cementation cement paste, which comprises the following steps:
step 2, after obtaining a primary reaction liquid, introducing nitrogen into the reaction kettle for 30min, and heating to 50 ℃ under the stirring condition of 500r/min to obtain an intermediate reaction liquid;
step 3, adding 0.0290% of potassium persulfate initiator into the residual 19.9940% of water to obtain an initiation solution;
step 4, after the intermediate reaction liquid in the step 2 is heated to 50 ℃, adding an initiating solution into the intermediate reaction liquid within 60 minutes, and continuing to perform 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 filtrate reducer for the well cementation cement paste.
In the step 4 of the above examples 1 to 4, the synthetic procedures of the thermal insulation reaction are as follows:
performing performance test on the temperature-sensitive fluid loss agent for well cementing cement paste prepared by adopting the embodiment, preparing cement paste according to GB/T19139-2003 standard, and testing the water loss effect, the retarding performance and the strength of the temperature-sensitive fluid loss agent for well cementing cement paste at different temperatures, wherein the formula of the cement paste is as follows: the ratio of the G-grade cement to 35% silica powder to the temperature-sensitive filtrate reducer to retarder to water for well cementing slurry is 0.44.
TABLE 1 Cement paste Performance test results Table prepared by adding temperature-sensitive filtrate reducer for well cementing cement paste obtained in examples 1-4
From the test results in table 1, it can be seen that the temperature-sensitive fluid loss agent for well cementing cement slurry obtained in examples 1-4 has better rheological control on cement slurry, and the fluid loss control is stable, and the API fluid loss at 150 ℃ and 200 ℃ can be controlled below 50 ml. The high-pressure water loss at 150 ℃ is 26-42mL, and most of the water loss is less than 40mL; the thickening time is proper; the compressive strength is higher than 20-26MPa, and the majority is more than 22MPa; the sedimentation stability is better than 0.1-0.2 g/cm 3 Most of the sedimentation stability was 0.1 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The fluidity at normal temperature is well between 21 cm and 22.5cm, and most of the fluidity is more than 22cm.
For structural characterization of the temperature-sensitive fluid loss agent for well cementing cement slurry, fig. 1 shows a thermal weight loss graph of the temperature-sensitive fluid loss agent for well cementing cement slurry prepared in example 1.
As can be seen from FIG. 1, (1) the mass fraction of the polymer molecules lost by heating at 22.91-116 ℃ at this stage is about 7.47%, which is caused by the fact that part of hydrophilic groups exist on the polymer molecular chain, which are liable to absorb water and wet, and the crystallization water contained in the polymer molecules volatilizes when heated; (2) 116-250.14 ℃, the polymer molecules at the stage are not greatly changed when heated, and the mass fraction of heat loss is about 1.29%; (3) 250.14-485.86 ℃, the main chain of the polymer is broken when heated at this stage, and the mass fraction of the polymer molecules lost when heated is about 47.06%; (4) 485.86-600 ℃, the mass fraction of the polymer molecules lost by heating at this stage is about 5.52%, mainly due to carbonization of the polymer molecular chains 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 paste has good high temperature resistance.
FIG. 2 is a thermogravimetric curve of the temperature-sensitive fluid loss agent for well cementing slurry prepared in example 2, wherein the molecular chain of the temperature-sensitive fluid loss agent for well cementing slurry has no obvious fracture decomposition phenomenon before 272 ℃; FIG. 3 is a thermogravimetric curve of the temperature-sensitive fluid loss agent for well cementing slurry prepared in example 3, wherein the molecular chain of the temperature-sensitive fluid loss agent for well cementing slurry has no obvious fracture decomposition phenomenon before 264 ℃; fig. 4 is a thermogravimetric curve of the temperature-sensitive fluid loss agent for well cementation cement paste prepared in example 4, wherein the molecular chain of the temperature-sensitive fluid loss agent for well cementation cement paste has no obvious fracture decomposition phenomenon before 260 ℃.
As can be seen from the thermal weight curve data of the four embodiments, the temperature resistance of the temperature-sensitive fluid loss agent for well cementing cement paste is higher than 250 ℃, and the temperature resistance is very good.
The foregoing 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 modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.
Claims (6)
1. The temperature-sensitive fluid loss agent for the well cementation cement paste 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 sodium p-styrenesulfonate; the temperature-sensitive monomer is at least one of N, N-dimethylacrylamide and N-isopropyl acrylamide.
2. The thermosensitive fluid loss agent for well cementation cement paste according to claim 1, wherein the initiator is at least one of potassium persulfate and ammonium persulfate.
3. A method for preparing a temperature-sensitive fluid loss agent for well cementing slurry according to any one of claims 1 to 2, which is characterized by comprising the following steps:
step 1, adding part of water into a reaction kettle, adding hydrophilic monomers and temperature-sensitive monomers into the reaction kettle, stirring and dissolving completely, and adjusting the pH value of the solution in the reaction kettle to 9-11 to obtain a primary reaction solution;
step 2, after obtaining a primary reaction liquid, 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, then adding an initiating solution into the intermediate reaction liquid, and reacting for 4-7 hours at a constant temperature to obtain a solution reactant;
and 5, freeze-drying the solution reactant to obtain the temperature-sensitive filtrate reducer for the well cementation cement paste.
4. The process according to claim 3, wherein in step 4, the intermediate reaction solution obtained in step 2 is heated to 50 to 70℃and kept at 50 to 70 ℃.
5. The method according to claim 3, wherein in the step 4, the thermal insulation reaction synthesis process is as follows:
6. the preparation method according to claim 3, wherein in the step 5, the solution reactant is sequentially frozen, dried and crushed to obtain the product.
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