CN116041601A - Cement paste retarder and preparation method and application thereof - Google Patents
Cement paste retarder and preparation method and application thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
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- 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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Abstract
The invention provides a cement paste retarder, a preparation method and application thereof, wherein the preparation method comprises the following steps: after adding an initiator into the raw material liquid, heating to 60-70 ℃ to initiate polymerization reaction, thereby obtaining the retarder; wherein the raw material liquid comprises styrene sulfonate, an organophosphorus scale inhibitor, hydroxyl (methyl) acrylate, unsaturated dibasic acid, 2-acrylamide-2-methylpropanesulfonic acid and deionized water, and the pH value of the raw material liquid is 6-7. The retarder can be used as a cement slurry component for well cementation of oil and gas wells, can reduce viscosity, delay the thickening speed of cement slurry, prolong pumpable time, and has good well cementation effect without sedimentation under high temperature conditions.
Description
Technical Field
The invention relates to a cement paste retarder, a preparation method and application thereof, and belongs to the field of oilfield chemistry.
Background
Cementing is an important operation in the drilling process. When well cementation operation is carried out, firstly, a sleeve is put into a well, and then cement slurry is injected into an annular space between a well wall and the sleeve. Cement paste mainly plays two roles: firstly, support and protect the sleeve, secondly, form the impermeable cement sheath after hardening in the annular space in the pit, can prevent the fluid at different positions from channeling each other. Currently, oil and gas exploration and development gradually shifts to deep and ultra-deep oil and gas resource exploration directions. In general, the downhole temperature and pressure are positively correlated with the well depth, so that the cementing of deep wells and ultra-deep wells is required to be matched with a cement slurry system with high temperature resistance.
In cement slurry systems, retarders play a vital role. The retarder can reduce the viscosity, delay the thickening speed of cement paste in a circumferential seam, prolong the pumpable time, be favorable for the cement paste to be more uniformly distributed between a well wall and a casing pipe to form a high-strength impermeable cement ring, and effectively play a role in layer interval sealing. The Chinese patent document with publication number of CN115368506A discloses a high-temperature-resistant zwitterionic copolymer retarder and a preparation method thereof, wherein the retarder is prepared from an anionic functional monomer, a cationic functional monomer, a temperature-resistant monomer and a salt-resistant monomer, and experiments prove that the retarder can play a role in reducing the viscosity of cement paste below 150 ℃ and delaying the thickening speed of the cement paste in a circumferential seam. However, in special collection environments including thickened oil thermal recovery and the like, since high-temperature and high-pressure steam huff and puff operations are required to be performed at a temperature higher than 150 ℃ for a period of a recovery life, the retarder at the present stage is obviously not suitable for such severe environments at high temperature and high pressure.
Therefore, further researches on a retarder of well cementing cement slurry capable of tolerating higher temperature are needed to solve the problem that the retarder in the prior art is easy to decline in performance under high temperature conditions, and on the basis, a cement slurry system suitable for high temperature well cementing is developed.
Disclosure of Invention
The retarder obtained by the preparation method is not only beneficial to improving the high-temperature stability of the cement paste, but also can prolong the thickening time of the cement paste, so that the high-efficiency exploitation of high Wen Shenceng and ultra-deep oil gas is facilitated.
The invention also provides the cement paste retarder which is prepared according to the method, so that the characteristics of high-temperature stability and ultra-long thickening time are conducive to coping with high-temperature oil and gas wells with more severe exploitation conditions.
The invention also provides cement paste which comprises the retarder, so that the cement paste has the characteristics of high temperature resistance and long thickening time.
The invention provides a preparation method of a cement paste retarder, which comprises the following steps:
after adding an initiator into the raw material liquid, heating to 60-70 ℃ to initiate polymerization reaction, thereby obtaining the retarder;
wherein the raw material liquid comprises styrene sulfonate, an organophosphorus scale inhibitor, hydroxyl (methyl) acrylate, unsaturated dibasic acid, 2-acrylamide-2-methylpropanesulfonic acid and deionized water, and the pH value of the raw material liquid is 6-7.
The preparation method comprises the following steps of (1) preparing styrene sulfonate, an organophosphorus scale inhibitor, (methyl) acrylic acid hydroxyl ester, unsaturated dibasic acid and 2-acrylamide-2-methylpropanesulfonic acid according to a mass ratio of (6-7): (6-7): (3-5): (1-3): (1-3);
the preparation method comprises the steps that the total mass of the styrene sulfonate, the organophosphorus scale inhibitor, the (methyl) acrylic acid hydroxyl ester, the unsaturated dibasic acid and the 2-acrylamide-2-methylpropanesulfonic acid accounts for 22% -25% of the total mass of the raw material liquid;
the preparation method comprises the steps that the organophosphorus scale inhibitor is one or more of allylphosphonic acid, hydroxyethylidene diphosphonic acid, aminotrimethylene phosphonic acid, ethylenediamine tetramethylene phosphonic acid and salts thereof;
the preparation method as described above, wherein the hydroxy (meth) acrylate is 2-hydroxyethyl acrylate, 2-hydroxyethyl (meth) acrylate; and/or the unsaturated dibasic acid is one or more of itaconic acid and butenedioic acid;
the preparation method comprises the steps of preparing the catalyst, wherein the mass of the initiator is 3% -4% of the total mass of styrene sulfonate, organophosphorus scale inhibitor, hydroxyl (methyl) acrylate, unsaturated dibasic acid and 2-acrylamide-2-methylpropanesulfonic acid;
the preparation method as described above, wherein the polymerization reaction time is 4 to 5 hours;
a retarder as described above, the retarder being prepared according to any one of the preparation methods described above;
a retarder as described above, wherein the particle size thereof is less than 0.3mm;
the invention also provides a cement paste retarder which is prepared by the method according to any of the above. The invention also provides cement paste, which comprises the cement paste retarder of any of the above.
According to the preparation method of the cement paste retarder, proper raw materials are selected and polymerization reaction is carried out under proper conditions, so that the retarder with good high-temperature stability and long thickening time can be obtained, and particularly, the retarder can still stably exist at the temperature of 200 ℃ and further can not be settled in the environment of 220 ℃, and can keep a low-viscosity state at least within 240min without thickening. Therefore, the retarder obtained by the preparation method can still realize higher exploitation efficiency even in a harsher oil and gas exploitation environment, such as the deep well or ultra-deep well exploitation environment or the thickened oil exploitation environment.
Drawings
Fig. 1 is a thickening curve of a cement slurry of the present invention comprising the cement slurry retarder of example 1.
Detailed Description
The present invention will be described in further detail below for the purpose of better understanding of the aspects of the present invention by those skilled in the art. The following detailed description is merely illustrative of the principles and features of the present invention, and examples are set forth for the purpose of illustration only and are not intended to limit the scope of the invention. All other embodiments, which can be made by those skilled in the art based on the examples of the invention without making any inventive effort, are intended to be within the scope of the invention.
The first aspect of the invention provides a preparation method of a cement paste retarder, which comprises the following steps:
after adding an initiator into the raw material liquid, heating to 60-70 ℃ to initiate polymerization reaction, thereby obtaining the retarder;
wherein the raw material liquid comprises styrene sulfonate, an organophosphorus scale inhibitor, hydroxyl (methyl) acrylate, unsaturated dibasic acid, 2-acrylamide-2-methylpropanesulfonic acid and deionized water, and the pH value of the raw material liquid is 6-7.
A feed solution is prepared before the polymerization reaction occurs. The present invention is not limited to the order of addition of the respective raw materials, and for example, the nonaqueous raw materials such as styrene sulfonate, organic phosphorus scale inhibitor, hydroxy (meth) acrylate, unsaturated dibasic acid, and 2-acrylamide-2-methylpropanesulfonic acid may be added to deionized water in any order, or at least two nonaqueous raw materials may be mixed and then added to deionized water together with other nonaqueous raw materials or sequentially. In the process of mixing the raw materials with each other, it is only necessary to ensure uniform dispersion of the non-aqueous raw materials in deionized water.
After the non-aqueous raw materials and the deionized water are mixed, the pH value of the mixed system can be adjusted by selecting a proper pH regulator according to the pH value of the current mixed system, so that the pH value of the mixed system is 6-7. Specifically, the different proportions of the respective raw materials may cause the pH of the mixed system to be different, and therefore, when the pH of the mixed system is acidic, the pH may be adjusted to 6 to 7 by selecting an alkaline pH adjuster, which may be, for example, at least one of sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium hydroxide, potassium hydroxide, or other alkaline substances. Preferably, the pH value of the mixed solution is regulated by using sodium carbonate aqueous solution with the concentration of 2-4 mol/L; more preferably, the pH value of the mixed solution is adjusted by using a sodium carbonate aqueous solution with the concentration of 3 mol/L; when the pH value of the mixed system is alkaline, the pH value of the mixed system can be adjusted to 6-7 by selecting an acidic pH value regulator, and the acidic pH regulator can be at least one of dilute sulfuric acid, dilute hydrochloric acid or other alkaline substances. Preferably, dilute sulfuric acid with the concentration of 2-4mol/L is used for adjusting the pH value of the mixed solution; more preferably, the pH of the mixture is adjusted using dilute sulfuric acid at a concentration of 3 mol/L.
It can be understood that the reaction system needs to be post-treated after the reaction is finished, so as to separate and obtain the target product with higher purity. In the present invention, the post-treatment includes an operation of subjecting the sequential reaction system to a purification treatment and a drying treatment. Illustratively, the drying process is carried out at a temperature of 105 ℃ + -2deg.C for a time of 24 h+ -1 h.
The retarder prepared according to the technical scheme provided by the invention has good stability under a high-temperature environment. When the additive is added into cement paste, the cement paste can not only be settled at 220 ℃ but also be kept in a low-viscosity state within 240min without thickening. The cement paste added with the retarder can still realize higher efficiency in a severe mining environment. As described above, in the process of preparing the retarder, the mass ratio of the styrene sulfonate, the organophosphorus scale inhibitor, the (methyl) acrylic acid hydroxyl ester, the unsaturated dibasic acid and the 2-acrylamide-2-methylpropanesulfonic acid in the raw material liquid is not excessively limited. In one specific embodiment, when the mass ratio of the styrene sulfonate, the organophosphorus scale inhibitor, the (methyl) acrylic acid hydroxyl ester, the unsaturated dibasic acid and the 2-acrylamide-2-methylpropanesulfonic acid is (6-7): (6-7): (3-5): (1-3): (1-3), preferably, the mass ratio of the five compounds is 6.5:6:4:2:2, the high-temperature stability of the retarder and the characteristic of prolonging the thickening time of cement paste are more outstanding.
Further, the reaction efficiency of the polymerization reaction can be further improved by controlling the mass ratio of the non-aqueous raw material to the deionized water. Specifically, when the total mass of the styrene sulfonate, the organophosphorus scale inhibitor, the (methyl) acrylic acid hydroxyl ester, the unsaturated dibasic acid and the 2-acrylamide-2-methylpropanesulfonic acid accounts for 22-25% of the total mass of the raw material liquid, the polymerization reaction rate is favorably controlled, and the relevant post-treatment operation is also facilitated by the proper volume of the reaction system.
The invention does not limit various nonaqueous raw materials in the raw material liquid too much, for example, the styrene sulfonate is at least one selected from the group consisting of lithium styrene sulfonate, sodium styrene sulfonate, potassium styrene sulfonate and ammonium styrene sulfonate; the organic phosphorus scale inhibitor is at least one selected from allyl phosphonic acid, hydroxyethylidene diphosphonic acid, amino trimethylene phosphonic acid, ethylenediamine tetramethylene phosphonic acid and salts formed by the four acids; the (methyl) acrylic acid hydroxy ester is selected from at least one of acrylic acid-2-hydroxy ethyl ester and (methyl) acrylic acid-2-hydroxy ethyl ester; the unsaturated dibasic acid is at least one selected from itaconic acid and butenedioic acid. When the five types of compounds are respectively a mixture of a plurality of specific compounds, the proportion of each specific compound is not excessively limited in the invention.
It will be appreciated that in polymerizing the above-described raw material liquid system, it is also necessary to add an initiator to the raw material liquid system. The present invention is not limited to the specific type of initiator, and may be at least one of potassium persulfate, sodium persulfate, and ammonium persulfate, for example.
When the initiator is added, in order to ensure the efficient progress of the polymerization reaction and avoid the influence of excessive addition of the initiator on the performance of the retarder, the mass of the initiator can be controlled to be 3-4% of the total mass of styrene sulfonate, organophosphorus scale inhibitor, hydroxyl (meth) acrylate, unsaturated dibasic acid and 2-acrylamide-2-methylpropanesulfonic acid, and more preferably 3.5%.
Further, in order to ensure efficient progress of the polymerization reaction, the reaction may be carried out in an inert atmosphere. The inert gas is selected from at least one of helium, argon, and nitrogen, for example.
In addition, the high temperature resistance of the retarder and the thickening time of cement paste can be further improved by controlling the polymerization time. Generally, the polymerization reaction time is controlled to be 4-5 hours, so that the proper polymerization degree of the retarder can be basically ensured, and further, the retarder has more excellent performance. In the actual preparation process, the polymerization inhibitor is generally added to the reaction system to stop the reaction.
In a second aspect, the invention provides a cement paste retarder prepared according to the method of the first aspect.
As described above, the cement paste is stable at 200 ℃ and even 220 ℃ without sedimentation and can maintain a low viscosity state within 240 minutes without thickening when the retarder is added to the cement paste.
Further, in order to facilitate the dispersion of retarder in cement slurry, it may be ground until it passes through a sieve having a pore diameter of 0.3mm, i.e., the particle diameter of retarder particles is controlled to be less than 0.3mm. The retarder can be uniformly mixed into the cement slurry only when the dried retarder is crushed to the particle size smaller than 0.3mm, so that the technical effects of enhancing the high-temperature stability of the cement slurry and prolonging the thickening time of the retarder are realized.
A third aspect of the present invention provides a cement slurry comprising the cement slurry retarder of the second aspect.
The invention is not limited to other compositions of cement slurries, and may be those commonly known in the art. For example, including class G cements, silica sand, fluid loss agents, retarders, water.
In the specific application process, the mass percentage of retarder in the cement slurry is 0.1-5%. The mass percent of retarder added is preferably increased correspondingly with the increase of temperature.
Example 1
The preparation method of the retarder of the embodiment comprises the following steps:
1) Mixing sodium styrenesulfonate, allyl phosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid with deionized water and uniformly stirring, and then regulating the pH value of the mixed system to 6 by using a 3mol/L sodium carbonate aqueous solution to obtain a raw material liquid;
wherein, the total mass of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid accounts for 23 percent of the total mass of the raw material liquid, and the mass ratio of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid is 6.5:6:4:2:2;
2) Slowly adding potassium persulfate into the raw material liquid to react at 60 ℃ in a nitrogen atmosphere; wherein the mass of the potassium persulfate is 3.5% of the total mass of sodium styrene sulfonate, 3-dimethylamino allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid;
3) After 5h of reaction, hydroquinone was added and the slightly viscous liquid product was cooled to room temperature. Purifying and drying the liquid product, and crushing to a particle size less than 0.3mm to obtain the powdery polymer retarder.
Example 2
The preparation method of the retarder of the embodiment comprises the following steps:
1) Mixing sodium styrenesulfonate, allyl phosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid with deionized water and uniformly stirring, and then regulating the pH value of the mixed system to 6 by using 2mol/L sodium carbonate aqueous solution to obtain raw material liquid;
wherein, the total mass of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid accounts for 23 percent of the total mass of the raw material liquid, and the mass ratio of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid is 6:6:3:1:1, a step of;
2) Slowly adding potassium persulfate into the raw material liquid to react at 55 ℃ in a nitrogen atmosphere; wherein the mass of the potassium persulfate is 3% of the total mass of sodium styrene sulfonate, 3-dimethylamino allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid;
3) After 4h of reaction, hydroquinone was added and the slightly viscous liquid product was cooled to room temperature. Purifying and drying the liquid product, and crushing to a particle size less than 0.3mm to obtain the powdery polymer retarder.
Example 3
The preparation method of the retarder of the embodiment comprises the following steps:
1) Mixing sodium styrenesulfonate, allyl phosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid with deionized water and uniformly stirring, and then regulating the pH value of the mixed system to 6 by using 4mol/L sodium carbonate aqueous solution to obtain raw material liquid;
wherein, the total mass of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid accounts for 23 percent of the total mass of the raw material liquid, and the mass ratio of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid is 7:7:5:3:3, a step of;
2) Slowly adding potassium persulfate into the raw material liquid to react at 65 ℃ in a nitrogen atmosphere; wherein the mass of the potassium persulfate is 4% of the total mass of sodium styrene sulfonate, 3-dimethylamino allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid;
3) After the reaction had proceeded for 6 hours, hydroquinone was added and the slightly viscous liquid product was cooled to room temperature. Purifying and drying the liquid product, and crushing to a particle size less than 0.3mm to obtain the powdery polymer retarder.
Example 4
The preparation method of this example is substantially identical to that of example 1, except that: in step 1) of this example, the mass ratio of sodium styrenesulfonate, allylphosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid, 2-acrylamide-2-methylpropanesulfonic acid was 3:9:1:5:2.
example 5
The preparation method of the retarder of the embodiment comprises the following steps:
1) Mixing sodium styrenesulfonate, hydroxyethylidene diphosphonic acid, 2-hydroxyethyl acrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid with deionized water, uniformly stirring, and then regulating the pH value of the mixed system to 6 by using a 3mol/L sodium carbonate aqueous solution to obtain a raw material liquid;
wherein the total mass of sodium styrenesulfonate, hydroxyethylidene diphosphonic acid, 2-hydroxyethyl acrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid accounts for 23% of the total mass of the raw material liquid, and the mass ratio of sodium styrenesulfonate, hydroxyethylidene diphosphonic acid, 2-hydroxyethyl acrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid is (4:6:1:3:5);
2) Slowly adding potassium persulfate into the raw material liquid to react at 60 ℃ in a nitrogen atmosphere; wherein the mass of the potassium persulfate is 3.5 percent of the total mass of sodium styrene sulfonate, hydroxyethylidene diphosphonic acid, 2-hydroxyethyl acrylate, butenedioic acid and 2-acrylamide-2-methylpropanesulfonic acid;
3) After the reaction is carried out for 5 hours, hydroquinone is added, the slightly viscous liquid product is cooled to room temperature, and the purification, drying and crushing are carried out until the particle size is less than 0.3mm, thus obtaining the powdery polymer retarder.
Example 6
The preparation method of the retarder of the embodiment comprises the following steps:
1) Mixing sodium styrenesulfonate, aminotrimethylene phosphonic acid, 2-hydroxyethyl methacrylate, butenedioic acid and 2-acrylamide-2-methylpropanesulfonic acid with deionized water and uniformly stirring, and then regulating the pH value of the mixed system to 6 by using a 3mol/L sodium carbonate aqueous solution to obtain a raw material liquid;
wherein the total mass of the sodium styrenesulfonate, the aminotrimethylene phosphonic acid, the 2-hydroxyethyl methacrylate, the butenedioic acid and the 2-acrylamide-2-methylpropanesulfonic acid accounts for 23 percent of the total mass of the raw material liquid, and the mass ratio of the sodium styrenesulfonate to the 2-hydroxyethyl methacrylate to the butenedioic acid to the 2-acrylamide-2-methylpropanesulfonic acid is (5:7:2:3:2);
2) Slowly adding potassium persulfate into the raw material liquid to react at 60 ℃ in a nitrogen atmosphere; wherein the mass of the potassium persulfate is 3.5 percent of the total mass of sodium styrenesulfonate, aminotrimethylene phosphonic acid, 2-hydroxyethyl methacrylate, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid;
3) After 5h of reaction, hydroquinone was added and the slightly viscous liquid product was cooled to room temperature. Purifying and drying the liquid product, and crushing to a particle size less than 0.3mm to obtain the powdery polymer retarder.
Example 7
The preparation method of this example is substantially identical to that of example 1, except that: in step 1) of this embodiment, the total mass of the five raw materials accounts for 10% of the total mass of the raw material liquid.
Example 8
The preparation method of this example is substantially identical to that of example 1, except that: in step 1) of this embodiment, the total mass of the five raw materials accounts for 50% of the total mass of the raw material liquid.
Comparative example 1
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;
2) Weighing 75.8 parts by mass of 2-acrylamide-2-methylpropanesulfonic acid, 55.2 parts by mass of sodium p-styrenesulfonate, 55.2 parts by mass of itaconic acid and 13.8 parts by mass of methacryloyloxyethyl trimethyl ammonium chloride for later use;
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 the methylene succinic acid, the methacryloxyethyl trimethyl ammonium chloride, the sodium p-styrenesulfonate and the 2-acrylamide-2-methylpropanesulfonic acid, and marking the four functional monomers as a solution A after the four functional monomers are completely dissolved;
4) Pouring the solution A into a reaction kettle, starting a stirring device according to the set rotating speed of 200rpm, adding a certain amount of NaOH to adjust the pH of the solution A to 6, and setting the temperature of the reaction kettle to 60 ℃ after the adjustment is finished;
5) Heating to 60 ℃ to keep the temperature constant, then introducing nitrogen into the reaction kettle for 10min, and plugging the bottle mouth of the reaction kettle by a plug after the introduction is finished to isolate air;
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;
7) Opening a bottle cap of the reaction kettle, and dripping the solution B in the step 6 into the solution A in the reaction kettle;
8) After the solution B is dripped, the bottle stopper of the reaction kettle is plugged, the solution in the reaction kettle is taken out after the reaction is carried out for 5 hours, and the obtained light yellow viscous solution is obtained, thus obtaining the product of the invention.
Comparative example 2
The preparation method of this example is substantially identical to that of example 1, except that: in the step 1) of the embodiment, the raw materials are methacrylic acid-2-hydroxyethyl, itaconic acid and 2-acrylamide-2-methylpropanesulfonic acid, and the mass ratio of the three is 2:1:1.
test example 1
The retarders synthesized in examples 1 to 8 and comparative examples 1 and 2 were added to cement paste formulations (105 parts by weight of G-stage cement, 30 parts by weight of quartz sand, 2 parts by weight of a fluid loss agent, 1.5 parts by weight of retarder, and 50 parts by weight of water), and the test was carried out under a thickening condition of 220 ℃ and 90MPa by weight, and the thickening time was shown in Table 1. Fig. 1 is a thickening curve of a cement slurry of the present invention comprising the cement slurry retarder of example 1.
TABLE 1
Conclusion: as can be seen from fig. 1 and table 1, the cement paste added with the retarder prepared according to the preparation method of example 1 maintains a viscosity time of less than 30Bc at 220 ℃ for 264min, and the thickening time of the cement paste added with the retarder prepared according to the preparation method of comparative example 1 can be prolonged in a high temperature environment. As can be seen from the experimental data of other examples and comparative examples, the cement paste retarder with good high-temperature stability and long thickening time is obtained by selecting proper raw materials and carrying out polymerization under proper conditions. The cement paste added with the retarder still keeps stable performance at 220 ℃ without sedimentation, and can provide thickening time of at least 240 min.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The preparation method of the cement paste retarder is characterized by comprising the following steps of:
after adding an initiator into the raw material liquid, heating to 60-70 ℃ to initiate polymerization reaction, thereby obtaining the retarder;
wherein the raw material liquid comprises styrene sulfonate, an organophosphorus scale inhibitor, hydroxyl (methyl) acrylate, unsaturated dibasic acid, 2-acrylamide-2-methylpropanesulfonic acid and deionized water, and the pH value of the raw material liquid is 6-7.
2. The preparation method according to claim 1, wherein the mass ratio of the styrene sulfonate, the organophosphorus scale inhibitor, the hydroxyl (meth) acrylate, the unsaturated dibasic acid and the 2-acrylamide-2-methylpropanesulfonic acid is (6-7): (6-7): (3-5): (1-3): (1-3).
3. The preparation method according to claim 1 or 2, wherein the total mass of the styrene sulfonate, the organophosphorus scale inhibitor, the (meth) acrylic acid hydroxy ester, the unsaturated dibasic acid and the 2-acrylamide-2-methylpropanesulfonic acid accounts for 22% -25% of the total mass of the raw material liquid.
4. The preparation method according to claim 1 or 2, wherein the organophosphorus scale inhibitor is one or more of allylphosphonic acid, hydroxyethylidene diphosphonic acid, aminotrimethylene phosphonic acid, ethylenediamine tetramethylene phosphonic acid and salts thereof.
5. The production method according to claim 1 or 2, wherein the hydroxy (meth) acrylate is 2-hydroxyethyl acrylate, 2-hydroxyethyl (meth) acrylate; and/or the unsaturated dibasic acid is one or more of itaconic acid and butenedioic acid.
6. The preparation method according to claim 1, wherein the mass of the initiator is 3% -4% of the total mass of styrene sulfonate, organic phosphorus scale inhibitor, hydroxyl (meth) acrylate, unsaturated dibasic acid and 2-acrylamide-2-methylpropanesulfonic acid.
7. The process according to claim 1 or 2, wherein the polymerization reaction time is 4 to 5 hours.
8. A cement paste retarder prepared according to the method of any one of claims 1 to 7.
9. A cement paste retarder according to claim 8, wherein the retarder has a powder particle size of no more than 0.3mm.
10. A cement slurry comprising a cement slurry retarder according to claim 8 or 9.
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| CN116675808A (en) * | 2023-06-16 | 2023-09-01 | 山东海嘉石油化工有限公司 | Organic retarded acid and preparation method thereof |
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| CN116675808A (en) * | 2023-06-16 | 2023-09-01 | 山东海嘉石油化工有限公司 | Organic retarded acid and preparation method thereof |
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