CN115368506A - High-temperature resistant zwitterionic copolymer retarder and preparation method thereof - Google Patents
High-temperature resistant zwitterionic copolymer retarder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature resistant zwitterionic copolymer retarder and a preparation method thereof, belonging to the field of oil and gas well cementing materials and being prepared from the following raw materials in parts by mass: 200 parts of functional monomer, 2-3 parts of initiator and 797-798 parts of water. The high-temperature resistant zwitterionic copolymer retarder can improve the fluidity of cement paste while ensuring the sedimentation stability of the cement paste, has moderate dispersion performance and can resist the high temperature of 150 ℃.
Description
Technical Field
The invention relates to a well cementing material of an oil and gas well, in particular to a high-temperature resistant zwitterionic copolymer retarder and a preparation method thereof.
Background
In recent years, with the continuous increase of the demand of oil and gas resources, shallow easy-to-open oil extraction fields are gradually exhausted, the exploitation of the oil and gas fields gradually develops towards the deep part of the stratum, the number of deep wells and ultra-deep wells is gradually increased, and the exploitation difficulty of the oil fields is gradually increased. Well cementation is an important link in well construction, and the quality of well cementation is related to the method yield and the service life of an oil well.
Under the common conditions, the underground temperature and pressure can be continuously increased along with the well depth, and cement slurry is easy to thicken rapidly under high temperature and high pressure, so that the pumping time is seriously shortened, and the well cementation safety is threatened. The fast thickening cement slurry system is also accompanied with the reduction of other properties, which affects the quality of well cementation engineering. Therefore, in order to ensure the well cementation quality and the construction safety, additives are required to be added into the cement paste to ensure the performance of the cement paste.
The retarder is used as the most common oil well cement additive, and has the main function of adjusting the thickening time of cement paste and ensuring that the cement paste meets the pumping requirement. With the development of oil and gas exploitation towards deep wells, ultra-deep wells and the like, complex geological conditions and environmental conditions put greater requirements on the performance of cement slurry. The retarder used in China generally has the problems of poor temperature resistance, poor salt resistance, abnormal gelation and the like, so that a novel retarder needs to be developed urgently to meet the requirement of modern well cementation.
Through the development of many years, a stable retarder product is provided, and the technical requirement can be met on a common oil well. However, with the increasing shortage of domestic resources, oil field exploration is developed towards deep wells and ultra-deep wells, and under severe bottom hole conditions such as high temperature, high pressure and high mineralization degree, the traditional anionic polycarboxylic acid retarder in the market can cause abnormal gelation phenomenon at high temperature, commonly called as "core wrapping", can cause the layering phenomenon after cement slurry is solidified, seriously influences the structural integrity and sealing integrity of cement stones, and even more can cause well cementation failure.
Disclosure of Invention
The invention aims to: providing a high-temperature resistant zwitterionic copolymer retarder and a preparation method thereof; a special cationic monomer is introduced into the traditional anionic retarder to construct a zwitterionic copolymer retarder, and the electrostatic repulsion between positive and negative ion groups weakens the adsorption of polymer molecular chains on the surfaces of cement particles by utilizing the electrostatic repulsion, the steric hindrance and the lubrication, thereby greatly avoiding the problems that the conventional retarder can cause the cement paste to be wrapped in the core or bulge in the high-temperature and high-pressure environment.
The invention is realized by the following technical scheme:
a high-temperature resistant zwitterionic copolymer retarder is prepared from the following raw materials in parts by mass: 200 parts of functional monomer, 2-3 parts of initiator and 797-798 parts of water.
The functional monomer comprises the following components in parts by mass: 75.8-137.9 parts of salt-tolerant monomer, 27.6-55.2 parts of temperature-tolerant monomer, 27.6-55.2 parts of anionic functional monomer and 6.9-13.8 parts of cationic functional monomer.
The anion functional monomer is at least one of Itaconic Acid (IA), maleic Acid (MA) or Acrylic Acid (AA); the cationic functional monomer is methacryloyloxyethyl trimethyl ammonium chloride (DMC) or dimethyl diallyl ammonium chloride (DMDAAC); the salt-tolerant monomer is Acrylamide (AM) or 2-acrylamide-2-methylpropanesulfonic Acid (AMPS); the temperature-resistant monomer is at least one of Sodium Styrene Sulfonate (SSS) or N-vinyl pyrrolidone (NVP); the initiator is persulfate.
The total mass of the functional monomers: (mass of initiator + mass of water) = 1.
A preparation method of the high-temperature resistant zwitterionic copolymer retarder comprises the following steps:
step 1, weighing water, and dividing the water into water A and water B;
step 2, weighing the functional monomer for later use;
step 3, continuously stirring the water A, adding the functional monomer weighed in the step 2 into the water A, and obtaining a solution A after the functional monomer is completely dissolved;
step 4, pouring the solution A into a reaction kettle, starting a stirring device according to a set rotating speed, adding NaOH to adjust the pH value of the solution A to 6-8, and setting the temperature of the reaction kettle to be 60-70 ℃ after the adjustment is finished;
step 6, weighing an initiator according to 1-1.5% of the total mass of the functional monomers weighed in the step 2, adding the weighed initiator into the water B, and uniformly stirring to obtain a solution B;
step 7, dropwise adding the solution B into the solution A in the reaction kettle;
and 8, after the solution B is dropwise added, plugging a bottle plug of the reaction kettle, and taking out the solution after the reaction of the solution in the reaction kettle is finished to obtain the high-temperature resistant zwitterionic copolymer retarder.
In the step 4, the set rotation speed is controlled to be between 200RPM and 400 RPM.
In the step 8, the reaction time of the solution in the reaction kettle is 4-5 h.
In the step 3, the anionic functional monomer, the cationic functional monomer, the temperature-resistant monomer and the salt-resistant monomer are sequentially added.
In the step 3, one of the functional monomers is added into the water A and stirred until the functional monomer is completely dissolved, and then the other monomer is added and stirred until the functional monomer is completely dissolved.
In the step 1, the mass of the water A is as follows: (mass of water B + mass of initiator) = 3.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a high-temperature resistant zwitterionic copolymer retarder and a preparation method thereof, wherein the retarding mechanism is as follows:
(1) The adsorption mechanism is as follows: the high-temperature resistant zwitterionic copolymer retarder is added into cement paste and adsorbed on the surface of a hydration product to form an adsorption layer, and the adsorption layer can prevent cement particles from continuously contacting with water, so that the hydration speed is reduced, and the aim of prolonging the thickening time of the cement paste is fulfilled;
(2) The complexing mechanism is as follows: the cement paste contains a large amount of Ca 2+ 、Al 3+ When cations are used, the cations and the high-temperature resistant zwitterionic copolymer retarder generate complexation, so that the generation of crystal nuclei is hindered to a certain extent, the hydration speed is reduced, and the retarding effect is achieved.
Compared with the prior art, the high-temperature resistant zwitterionic copolymer retarder prepared by the invention has the following advantages:
(1) The high-temperature resistant zwitterionic copolymer retarder is simple in manufacturing process, and the adopted raw materials are simple in source, easy to obtain and low in price;
(2) The high-temperature resistant zwitterionic copolymer retarder has moderate dispersion effect on cement paste, and avoids the defect that the fluidity of the cement paste can be greatly changed after the conventional retarder is added into the cement paste;
(3) Cationic functional monomers are introduced into high-temperature resistant zwitterionic copolymer retarder molecules, the adsorption effect of polymer molecular chains on the surfaces of cement particles is weakened by utilizing the electrostatic repulsion effect, the steric hindrance effect and the lubricating effect, and the problems that the existing retarder can cause the cement paste to be wrapped in the core or bulge in the high-temperature and high-pressure environment are greatly solved.
Drawings
FIG. 1 is a graph of the effect of a thickening curve of a blank group of cement paste without a retarder;
FIG. 2 is a graph showing the effect of a cement slurry thickening curve with the addition of a copolymer retarder on the market;
FIG. 3 is a graph showing the thickening curve effect of cement slurries to which the high temperature resistant zwitterionic copolymer retarders of the present invention have been added.
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, with other alternative features which are equivalent or similar in purpose, i.e. each feature is an embodiment of a range of equivalent or similar features, unless expressly stated otherwise.
Example 1
The invention relates to a preparation method of a high-temperature resistant zwitterionic copolymer retarder, which comprises the following steps:
step 1, weighing 798 parts by mass of deionized water, and dividing the deionized water into 600 parts by mass of deionized water A and 198 parts by mass of deionized water B;
step 2, weighing 75.8 parts by mass of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 55.2 parts by mass of Sodium Styrene Sulfonate (SSS), 55.2 parts by mass of Itaconic Acid (IA) and 13.8 parts by mass of methacryloyloxyethyl trimethyl ammonium chloride (DMC) for later use;
step 3, continuously stirring deionized water A, adding the four functional monomers weighed in the step 2 into the deionized water A according to the sequence of Itaconic Acid (IA), methacryloyloxyethyl trimethyl ammonium chloride (DMC), sodium Styrene Sulfonate (SSS) and 2-acrylamide-2-methyl propanesulfonic Acid (AMPS), and marking as a solution A after the four functional monomers are completely dissolved;
step 4, pouring the solution A into a reaction kettle, starting a stirring device at a set rotating speed of 200RPM, adding a certain amount of NaOH to adjust the pH value of the solution A to 6, and setting the temperature of the reaction kettle to 60 ℃ after the adjustment is finished;
step 6, weighing 2 parts by mass of potassium persulfate, adding the potassium persulfate into the deionized water B in the step 1, and uniformly stirring to obtain a solution B for later use;
step 7, opening a bottle stopper of the reaction kettle, and dropwise adding the solution B obtained in the step 6 into the solution A in the reaction kettle;
and 8, after the solution B is dropwise added, plugging a bottle stopper of the reaction kettle, taking out the solution after the solution in the reaction kettle reacts for 5 hours, and obtaining the light yellow viscous solution, namely the product of the invention.
Example 2
The invention relates to a preparation method of a high-temperature resistant zwitterionic copolymer retarder, which comprises the following steps:
step 1, weighing 797 parts by mass of deionized water, and dividing the deionized water into 600 parts by mass of deionized water A and 197 parts by mass of deionized water B;
weighing 137.9 parts by mass of Acrylamide (AM), 27.6 parts by mass of N-vinyl pyrrolidone (NVP), 27.6 parts by mass of Acrylic Acid (AA) and 6.9 parts by mass of dimethyl diallyl ammonium chloride (DMDAAC) for later use;
step 3, continuously stirring deionized water A, adding the four functional monomers weighed in the step 2 into the deionized water A according to the sequence of Acrylic Acid (AA), dimethyl diallyl ammonium chloride (DMDAAC), N-vinyl pyrrolidone (NVP) and Acrylamide (AM), and marking the solution A as a solution A after the four functional monomers are completely dissolved;
step 4, pouring the solution A into a reaction kettle, starting a stirring device at a set rotating speed of 400RPM, adding a certain amount of NaOH to adjust the pH value of the solution A to 8, and setting the temperature of the reaction kettle to 70 ℃ after the adjustment is finished;
step 6, weighing 2 parts by mass of ammonium persulfate and 1 part by mass of potassium persulfate, adding into the deionized water B in the step 1, and uniformly stirring to obtain a solution B for later use;
step 7, opening a bottle stopper of the reaction kettle, and dropwise adding the solution B obtained in the step 6 into the solution A in the reaction kettle;
and 8, after the solution B is dropwise added, plugging a bottle stopper of the reaction kettle, taking out the solution after the solution in the reaction kettle reacts for 4 hours, and obtaining the light yellow viscous solution, namely the product of the invention.
Example 3
The invention relates to a preparation method of a high-temperature resistant zwitterionic copolymer retarder, which comprises the following steps:
step 1, weighing 797.5 parts by mass of deionized water, and dividing the deionized water into 600 parts by mass of deionized water A and 197.5 parts by mass of deionized water B;
step 2, weighing 117.2 parts by mass of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 41.4 parts by mass of N-vinyl pyrrolidone (NVP), 27.6 parts by mass of Maleic Acid (MA) and 13.8 parts by mass of dimethyl diallyl ammonium chloride (DMDAAC) for later use;
step 3, continuously stirring deionized water A, adding the four functional monomers weighed in the step 2 into the deionized water A according to the sequence of Maleic Acid (MA), dimethyl diallyl ammonium chloride (DMDAAC), N-vinyl pyrrolidone (NVP) and 2-acrylamide-2-methyl propanesulfonic Acid (AMPS), and marking the mixture as a solution A after the four functional monomers are completely dissolved;
step 4, pouring the solution A into a reaction kettle, starting a stirring device at a set rotating speed of 300RPM, adding a certain amount of NaOH to adjust the pH value of the solution A to 7, and setting the temperature of the reaction kettle to 65 ℃ after the adjustment is finished;
step 6, weighing 2.5 parts by mass of ammonium persulfate, adding into the deionized water B in the step 1, and uniformly stirring to obtain a solution B for later use;
step 7, opening a bottle stopper of the reaction kettle, and dropwise adding the solution B obtained in the step 6 into the solution A in the reaction kettle;
and 8, after the solution B is dropwise added, plugging a bottle stopper of the reaction kettle, taking out the solution after the solution in the reaction kettle reacts for 5 hours, and obtaining the light yellow viscous solution, namely the product of the invention.
Example 4
The invention relates to a preparation method of a high-temperature resistant zwitterionic copolymer retarder, which comprises the following steps:
step 1, weighing 797 parts by mass of deionized water, and dividing the deionized water into 600 parts by mass of deionized water A and 197 parts by mass of deionized water B;
step 2, weighing 95.3 parts by mass of Acrylamide (AM), 55.2 parts by mass of Sodium Styrene Sulfonate (SSS), 40.2 parts by mass of Acrylic Acid (AA) and 9.3 parts by mass of methacryloyloxyethyl trimethyl ammonium chloride (DMC) for later use;
step 3, continuously stirring deionized water A, adding the four functional monomers weighed in the step 2 into the deionized water A according to the sequence of Acrylic Acid (AA), methacryloyloxyethyl trimethyl ammonium chloride (DMC), sodium Styrene Sulfonate (SSS) and Acrylamide (AM), and marking the solution A as a solution A after the four functional monomers are completely dissolved;
step 4, pouring the solution A into a reaction kettle, starting a stirring device at a set rotating speed of 350RPM, adding a certain amount of NaOH to adjust the pH value of the solution A to 7, and setting the temperature of the reaction kettle to 70 ℃ after the adjustment is finished;
step 6, weighing 1.5 parts by mass of ammonium persulfate and 1.5 parts by mass of potassium persulfate, adding into the deionized water B in the step 1, and uniformly stirring to obtain a solution B for later use;
step 7, opening a bottle stopper of the reaction kettle, and dropwise adding the solution B obtained in the step 6 into the solution A in the reaction kettle;
and 8, after the solution B is dropwise added, plugging a bottle stopper of the reaction kettle, taking out the solution after the solution in the reaction kettle reacts for 4 hours, and obtaining the light yellow viscous solution, namely the product of the invention.
The high-temperature resistant zwitterionic copolymer retarder prepared in the embodiment is subjected to cement paste performance test.
Preparing cement paste according to the GB/T19139-2003 standard, and testing the retardation performance, the compression strength at 150 ℃ for 24h and the compression strength at 90 ℃ for 48h of (1); (2) standing the cement paste in an environment of 90 ℃ for 2 hours, and then testing the difference between the upper density and the lower density of the cement paste to judge the sedimentation stability of the cement paste; (3) placing the cement paste in an atmospheric pressure densifier, prefabricating the cement paste at 90 ℃ for 20min, taking out the cement paste, and reading the cement paste by a six-speed viscosity tester to judge the fluidity of the cement paste. The formula of the cement paste is as follows:
common Jiahua grade G cement: 600 parts by mass; water: 280 parts by mass; quartz sand: 210 parts by mass; micro silicon: 5 parts by mass; self-made fluid loss agent: 42 parts by mass; the high-temperature resistant zwitterionic copolymer retarder of the invention comprises: 24 parts by mass; mixing the above materials.
Table 1 different cement paste performance test meter
| Thickening time/ |
150 ℃ x 24h compressive strength/MPa | Compressive strength/MPa at 90 ℃ for 48h | Upper and lower density difference/g cm -3 | |
| Blank set without retarder | 54 | 35.2 | 20.7 | 0.01 |
| Adding a copolymer retarder on the market | 274 | 28.4 | 15.7 | 0.21 |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 1 was added | 309 | 29.5 | 15.4 | 0.02 |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 2 was added | 282 | 30.7 | 17.1 | 0.02 |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 3 was added | 324 | 28.1 | 14.6 | 0.02 |
| Addition of the high temperature resistant prepared in example 4Zwitterionic copolymer retarder | 294 | 27.9 | 15.0 | 0.02 |
Table 2 six-speed viscosity test data table for different cement slurries
| Rotational speed of rotational viscometer (r/min) | 3 | 6 | 100 | 200 | 300 | 600 |
| Blank set without retarder | 2 | 3 | 37 | 240 | \ | \ |
| Adding a copolymer retarder on the market | 1 | 2 | 60 | 123 | 172 | \ |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 1 was added | 2 | 3 | 78 | 172 | 234 | \ |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 2 was added | 2 | 3 | 72 | 164 | 220 | \ |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 3 was added | 2 | 3 | 72 | 158 | 217 | \ |
| The high temperature resistant zwitterionic copolymer retarder prepared in example 4 was added | 2 | 3 | 76 | 165 | 229 | \ |
Analysis of tables 1 and 2 reveals that:
compared with certain anionic copolymer retarders on the market, the high-temperature resistant zwitterionic copolymer retarder has better thickening performance than that of the anionic copolymer retarder, has lower influence on the later strength of set cement, and can ensure the top strength of a cement sheath. Compared with a certain anionic copolymer retarder on the market, the difference of the upper density and the lower density of the cement slurry added with the high-temperature resistant zwitterionic copolymer retarder is far smaller than that of the cement slurry added with the certain anionic copolymer retarder on the market, meanwhile, the data change of the cement slurry added with the certain anionic copolymer retarder on the market is larger compared with the cement slurry without retarder blank group, and the data change of the cement slurry added with the high-temperature resistant zwitterionic copolymer retarder is moderate, so that the high-temperature resistant zwitterionic copolymer retarder provided by the invention is capable of improving the fluidity of the cement slurry while ensuring the sedimentation stability of the cement slurry, and the dispersion performance is moderate.
Analysis of fig. 1, 2 and 3:
referring to the thickening curve (figure 1) of the blank group without any retarder, the initial consistency of the cement slurry (figures 2 and 3) added with the retarder is remarkably reduced, which shows that the cement slurry has a proper dispersion effect, meanwhile, the thickening curve of the cement slurry (figure 2) added with an anionic copolymer retarder on the market has a phenomenon of 'waving' in a temperature curve, because the cement slurry is flocculated at high temperature, flocculates are wound on a blade under the action of high-speed stirring of the blade, and the temperature system of a thickener cannot timely convey the correct temperature of the cement slurry and cannot stably maintain the temperature of the cement slurry due to the inconsistency of the heat transfer speed of the flocculated substances and the cement slurry, and the thickening curve is reflected as 'waving' of the temperature curve on a thickening curve graph, namely the characteristic of the 'core wrapping' phenomenon. The thickening curve (figure 3) of the cement paste added with the high-temperature resistant zwitterionic copolymer retarder is stable in temperature curve and consistency curve, and the phenomenon that the cement paste is not subjected to core wrapping at high temperature is shown.
Compared with the existing anionic copolymer retarder, the amphoteric copolymer retarder formed by introducing the cationic functional monomer can effectively avoid the problems of 'core wrapping' and 'bulging', and can ensure that the field well cementation construction is safely and smoothly carried out.
It is to be noted that, according to the technical requirements of cement retarders for petrochemical oil wells, retarders with the temperature of over 120 ℃ are high-temperature retarders, and the amphoteric copolymer retarder can resist the temperature of 150 ℃, and belongs to a high-temperature retarder.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. The high-temperature resistant zwitterionic copolymer retarder is characterized by being prepared from the following raw materials in parts by mass: 200 parts of functional monomer, 2-3 parts of initiator and 797-798 parts of water.
2. The high-temperature resistant zwitterionic copolymer retarder of claim 1, characterized in that the functional monomers comprise the following components in parts by mass: 75.8 to 137.9 portions of salt-resistant monomer, 27.6 to 55.2 portions of temperature-resistant monomer, 27.6 to 55.2 portions of anion functional monomer and 6.9 to 13.8 portions of cation functional monomer.
3. The high-temperature resistant zwitterionic copolymer retarder of claim 2, wherein the anionic functional monomer is at least one of Itaconic Acid (IA), maleic Acid (MA), or Acrylic Acid (AA); the cationic functional monomer is methacryloyloxyethyl trimethyl ammonium chloride (DMC) or dimethyl diallyl ammonium chloride (DMDAAC); the salt-tolerant monomer is Acrylamide (AM) or 2-acrylamide-2-methylpropanesulfonic Acid (AMPS); the temperature-resistant monomer is at least one of Sodium Styrene Sulfonate (SSS) or N-vinyl pyrrolidone (NVP); the initiator is persulfate.
4. The high temperature resistant zwitterionic copolymer retarder of claim 1, wherein the total mass of the functional monomers: (mass of initiator + mass of water) = 1.
5. A method for preparing the high-temperature resistant zwitterionic copolymer retarder as defined in any one of claims 2-4, characterized by comprising the following steps:
step 1, weighing water, and dividing the water into water A and water B;
step 2, weighing the functional monomer for later use;
step 3, continuously stirring the water A, adding the functional monomer weighed in the step 2 into the water A, and obtaining a solution A after the functional monomer is completely dissolved;
step 4, pouring the solution A into a reaction kettle, starting a stirring device according to a set rotating speed, adding NaOH to adjust the pH value of the solution A to 6-8, and setting the temperature of the reaction kettle to be 60-70 ℃ after the adjustment is finished;
step 5, heating to 60-70 ℃, keeping the temperature constant, introducing nitrogen into the reaction kettle, and plugging the opening of the reaction kettle by a plug to isolate air after the introduction is finished;
step 6, weighing an initiator according to 1-1.5% of the total mass of the functional monomers weighed in the step 2, adding the weighed initiator into the water B, and uniformly stirring to obtain a solution B;
step 7, dropwise adding the solution B into the solution A in the reaction kettle;
and 8, after the solution B is dropwise added, plugging a bottle plug of the reaction kettle, and taking out the solution after the reaction of the solution in the reaction kettle is finished to obtain the high-temperature resistant zwitterionic copolymer retarder.
6. The method according to claim 5, wherein in the step 4, the set rotation speed is controlled to be between 200RPM and 400 RPM.
7. The preparation method according to claim 5, wherein in the step 8, the reaction time of the solution in the reaction kettle is 4-5 h.
8. The method according to claim 5, wherein in step 3, the anionic functional monomer, the cationic functional monomer, the temperature-resistant monomer and the salt-resistant monomer are added in this order.
9. The method according to claim 5, wherein in step 3, one of the functional monomers is added to water A and stirred until it is completely dissolved, and then the other monomer is added and stirred until it is completely dissolved.
10. The method according to claim 5, wherein in the step 1, the mass of the water A: (mass of water B + mass of initiator) = 3.
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| CN105037625A (en) * | 2015-07-02 | 2015-11-11 | 中国石油大学(华东) | Modified aluminate cement retarder and preparation method thereof |
| US20200239760A1 (en) * | 2019-01-28 | 2020-07-30 | China University Of Petroleum (East China) | High-temperature retarder suitable for oil and gas well cementation, preparation method thereof and cementing slurry |
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