CN107502313B - Slow-release fluid loss agent for seawater well cementation, preparation method and application - Google Patents
Slow-release fluid loss agent for seawater well cementation, preparation method and application Download PDFInfo
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Abstract
The invention discloses a slow-release fluid loss agent for seawater well cementation, a preparation method and application thereof, wherein the preparation method comprises the following steps: reacting the monomer with an initiator to obtain a quaternary anionic copolymer; the monomer is composed of 2-acrylamide-2-methylpropanesulfonic acid, unsaturated carboxylic acid, acrylamide substances and allyl polyethylene glycol; preparing a mixed nitrate deionized water solution as a solution A; preparing a sodium mixture deionized water solution as a B solution; n is a radical of2Under protection, the A, B solutions are respectively and simultaneously dropped into deionized water for reaction to obtain calcium-aluminum type hydrotalcite-like compounds; preparing a quaternary anionic copolymer deionized water solution as a solution C; preparing a calcium-aluminum hydrotalcite-like deionized water dispersion liquid as a D dispersion liquid; in N2And (4) protecting, and mixing and reacting the solution C and the dispersion solution D to obtain the slow-release fluid loss agent for seawater cementing. The preparation method is simple, can obviously improve the fluid loss control effect of the fluid loss agent, and has lasting dispersion capacity on cement slurry.
Description
Technical Field
The invention relates to a seawater well cementation slow release type fluid loss agent, a preparation method and application thereof, and belongs to the field of oil field well cementation fluid loss agents.
Background
Under the condition that inland and offshore oil can be recovered and the recovery rate is gradually exhausted, the exploration and development of oil fields are developed to the ocean and deep wells. However, as part of metal cation electrolyte in seawater can affect the rheological property of cement paste, the performances of the water loss reducing agent in controlling filtration, dispersion, early strength and the like are greatly reduced. Therefore, seawater cementing requires that the fluid loss agent has good fluid loss reducing effect and has dispersing and early strength functions.
In order to solve such problems, a method of introducing a carboxyl group having a strong adsorption effect with cement hydrated particles, a sulfonic acid group having a low cation sensitivity, and a long side chain group having a strong steric hindrance effect into a polymer is generally used. However, such copolymers still have two distinct disadvantages: firstly, carboxyl is introduced, so that the adsorption capacity of a polymer is improved to ensure the water loss control performance, and simultaneously, the cement paste has a strong retarding effect, so that the early strength of the paste is reduced; secondly, long side chain groups are excellent in regulation of the early fluidity of the slurry, but the admixture is gradually consumed along with the progress of the hydration reaction of the cement slurry, so that the fluidity of the slurry at the later stage is difficult to regulate, and the requirement of the whole well cementation process on the dispersibility of the cement slurry is difficult to meet.
In view of the above problems, in recent years, researchers have attracted attention to reports about the preparation of sustained-release additives by the intercalation of calcium-aluminum type hydrotalcite-like compounds with polyanion type additives. On the one hand, the crystal structure of the calcium-aluminum hydrotalcite-like compound is very similar to that of the calcium monosulfide aluminate in the cement hydration product, so that the crystal seed effect of the calcium-aluminum hydrotalcite-like compound is favorable for promoting the early hydration of cement, thereby enhancing the early strength of the slurry; on the other hand, the action mode of the slow-release type admixture is similar to delayed dripping, namely the mode of one-time addition of the traditional admixture is changed into the mode of gradually slowly releasing the traditional admixture into the cement paste from the upper layer plate or the interlayer of the hydrotalcite layer plate, so that the effective utilization of the external admixture is greatly improved, and the water control and fluidity maintaining effects of the admixture are improved. For example, the slow-release dispersant is successfully prepared by intercalation of phenol/formaldehyde polycondensate and calcium-aluminum hydrotalcite-like compound, so that the fluidity of slurry is improved in a relatively long time, and the actual utilization rate of the additive is improved. However, although some progress is made in the preparation of the currently known slow-release type admixture, the preparation method still has the defects that: the research of synthesis mainly focuses on the sustained-release dispersant, and the synthesis of the sustained-release fluid loss agent is rarely reported; on the other hand, the existing slow-release admixture is more suitable for fresh water cement paste, and the investigation on the seawater performance is less.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a slow-release fluid loss agent for seawater well cementation.
The second purpose of the invention is to provide a preparation method of the slow-release fluid loss agent for seawater well cementation.
The third purpose of the invention is to provide the application of the slow-release fluid loss agent for seawater well cementation.
The technical scheme of the invention is summarized as follows:
the preparation method of the slow-release fluid loss agent for seawater cementing comprises the following steps:
(1) dissolving 20-30g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 4-7; adding an initiator accounting for 0.4-0.8% of the total mass of the monomers, reacting for 2-6h at 60-80 ℃ under stirring, and cooling to room temperature to obtain a quaternary anionic copolymer; the monomer consists of 76 to 82 percent of 2-acrylamide-2-methylpropanesulfonic acid, 3 to 5 percent of unsaturated carboxylic acid, 14 to 16 percent of acrylamide substance and 1 to 3 percent of allyl polyethylene glycol by mass;
(2) dissolving 25-40g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 1-3: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 10-20g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 1-2: NaOH and NaNO of 13Composition is carried out; in N2Respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water under the protection condition, stirring for 24-48 hours at 70-90 ℃, carrying out solid-liquid separation, drying the solid, and grinding or crushing to obtain the calcium-aluminum type hydrotalcite;
(3) dissolving 3-6g of quaternary anionic copolymer in 10 mass times of boiled deionized water to obtain a solution C; dispersing 1-2g of calcium-aluminum type hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protection, mixing the solution C and the dispersion solution D, and reacting for 24-48h at 90-100 ℃ under the condition that the rotating speed is 200-; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and grinding or crushing to obtain the slow-release fluid loss agent for seawater cementing.
The initiator is ammonium persulfate, potassium persulfate or azodiisobutyl amidine hydrochloride.
The unsaturated carboxylic acids are maleic acid, acrylic acid and itaconic acid.
The acrylamide substance is acrylamide or N, N-dimethylacrylamide.
The number average molecular weight of allyl polyethylene glycol is 600-1200.
The reaction time in step (1) is preferably 4 hours.
Preferably, the mixed nitrate is prepared by mixing the following components in a molar ratio of 2: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20.
Preferably, the sodium mixture is prepared by mixing sodium hydroxide and sodium hydroxide in a molar ratio of 2: NaOH and NaNO of 13And (4) forming.
The slow-release fluid loss agent for seawater cementing prepared by the method.
The application of the slow-release type fluid loss additive for seawater well cementation is disclosed.
The invention has the advantages that:
(1) the invention takes water as solvent, has simple preparation method and is easy to realize industrial production.
(2) According to the slow-release type fluid loss agent for seawater cementing, due to the slow-release function, the coprecipitation interference of substances such as magnesium hydroxide in cement paste on the admixture is avoided, so that the actual adsorption quantity between the admixture and cement particles is increased, and the fluid loss control effect of the fluid loss agent can be obviously improved.
(3) According to the slow-release type fluid loss agent for seawater well cementation, the anionic copolymer between the calcium-aluminum type hydrotalcite laminates is subjected to anion exchange reaction with anions formed in the hydration process of cement slurry, so that the slow-release function is realized, and the slow-release type fluid loss agent has more lasting dispersing capacity on the cement slurry.
(4) The crystal structure of the calcium-aluminum hydrotalcite-like compound in the slow-release fluid loss agent for seawater cementing is very similar to that of the monosulfur calcium aluminate in a cement hydration product, so that the crystal seed effect of the calcium-aluminum hydrotalcite-like compound is favorable for promoting the early hydration of cement, and the over-retarding phenomenon of cement paste caused by unsaturated carboxyl in a polyanion additive is relieved.
(5) The slow-release type fluid loss agent for seawater cementing is solid particles, is easy to store and is convenient to transport.
(6) The slow-release type fluid loss agent for seawater well cementation has the functions of dispersion and early strength while ensuring the water loss of cement paste, so that the well cementation cost is reduced to a great extent, and the compatibility problem caused by adding various additives in the well cementation process is fundamentally avoided.
Drawings
FIG. 1 XRD patterns of the calcium-aluminum type hydrotalcite-like compound prepared in example 1 and the slow-release fluid loss additive for seawater cementing.
FIG. 2 is an infrared spectrum of the Ca-Al hydrotalcite-like compound prepared in example 1 and the slow-release fluid loss agent for seawater cementing.
FIG. 3 is a scanning electron micrograph (d-f) of the calcium-aluminum type hydrotalcite-like compound (a-c) prepared in example 1 and the slow-release fluid loss agent for seawater cementing.
FIG. 4 is a transmission electron microscope image of the slow release type fluid loss agent for seawater cementing prepared in example 1.
FIG. 5 is a hydration isothermal calorimetry curve of the slow-release fluid loss additive for seawater cementing prepared in example 1 and a comparative example under a seawater slurry mixing condition.
FIG. 6 is a scanning electron microscope comparison of pure cement (a-c) and cement slurry (d-f) added with the slow release type fluid loss additive for seawater well cementation in example 1 under different curing time conditions.
Detailed Description
The invention is further illustrated by the following examples and figures, but the scope of the invention is not limited by the examples 1
The preparation method of the slow-release fluid loss agent for seawater cementing comprises the following steps:
(1) dissolving 25g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 6 by using sodium hydroxide; adding ammonium persulfate accounting for 0.6 percent of the total mass of the monomers, reacting for 4 hours at 70 ℃ under stirring, and cooling to room temperature to obtain a quaternary anion copolymer; the monomer consists of 78% of 2-acrylamide-2-methylpropanesulfonic acid, 4% of maleic acid, 15% of N, N-dimethylacrylamide and 3% of allyl polyethylene glycol by mass;
the number average molecular weight of the allyl polyethylene glycol is 600;
(2) dissolving 32g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 2: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 15g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 2: NaOH and NaNO of 13Composition is carried out; in N2Respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water under the protection condition, stirring for 36 hours at 80 ℃, carrying out solid-liquid separation, drying solids, and grinding to obtain calcium-aluminum type hydrotalcite-like compound;
(3) dissolving 4g of quaternary anionic copolymer in 10 mass times of boiled deionized water to obtain a solution C; dispersing 1.5g of calcium-aluminum type hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protecting, mixing the solution C and the dispersion solution D, and reacting for 36 hours at 95 ℃ under the condition that the rotating speed is 400 revolutions per minute; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and grinding to obtain the slow-release fluid loss agent for seawater cementing.
Example 2
The preparation method of the slow-release fluid loss agent for seawater cementing comprises the following steps:
(1) dissolving 20g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 7 by using sodium hydroxide; adding ammonium persulfate accounting for 0.4 percent of the total mass of the monomers, reacting for 6 hours at 60 ℃ under stirring, and cooling to room temperature to obtain a quaternary anion copolymer; the monomer consists of 76% of 2-acrylamide-2-methylpropanesulfonic acid, 5% of maleic acid, 16% of N, N-dimethylacrylamide and 3% of allyl polyethylene glycol by mass;
the number average molecular weight of the allyl polyethylene glycol is 1200;
(2) dissolving 25g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 1: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 10g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 1: NaOH and NaNO of 13Composition is carried out; in N2Under the protection condition, respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water, and stirring for 48 hours at 70 DEG CCarrying out solid-liquid separation, drying the solid and crushing to obtain calcium-aluminum type hydrotalcite;
(3) dissolving 3g of quaternary anionic copolymer in 10 mass times of boiled deionized water to obtain a solution C; dispersing 1g of calcium-aluminum hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protecting, mixing the solution C and the dispersion solution D, and reacting for 48 hours at 90 ℃ under the condition that the rotating speed is 200 revolutions per minute; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and crushing to obtain the slow-release fluid loss agent for seawater cementing.
Example 3
The preparation method of the slow-release fluid loss agent for seawater cementing comprises the following steps:
(1) dissolving 30g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 4 by using potassium hydroxide; adding azodiisobutylamine hydrochloride accounting for 0.8 percent of the total mass of the monomers, reacting for 2 hours at 80 ℃ under stirring, and cooling to room temperature to obtain quaternary anionic copolymer; the monomer consists of 82% of 2-acrylamide-2-methylpropanesulfonic acid, 3% of maleic acid, 14% of N, N-dimethylacrylamide and 1% of allyl polyethylene glycol by mass;
the number average molecular weight of the allyl polyethylene glycol is 1200;
(2) dissolving 40g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 3: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 20g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 2: NaOH and NaNO of 13Composition is carried out; in N2Respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water under the protection condition, stirring for 24 hours at 90 ℃, carrying out solid-liquid separation, drying solids, and grinding to obtain calcium-aluminum type hydrotalcite-like compound;
(3) dissolving 6g of quaternary anionic copolymer in 10 mass times of boiled deionized water to obtain a solution C; dispersing 2g of calcium-aluminum hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protecting, dispersing the solution C and the solution DMixing the solutions, and reacting at 100 ℃ for 24 hours under the condition that the rotating speed is 500 r/min; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and grinding to obtain the slow-release fluid loss agent for seawater cementing.
Example 4
The preparation method of the slow-release fluid loss agent for seawater cementing comprises the following steps:
(1) dissolving 30g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 4 by using potassium hydroxide; adding potassium persulfate accounting for 0.8 percent of the total mass of the monomers, reacting for 2 hours at 80 ℃ under stirring, and cooling to room temperature to obtain a quaternary anion copolymer; the monomer consists of 82% of 2-acrylamide-2-methylpropanesulfonic acid, 3% of acrylic acid, 14% of N, N-dimethylacrylamide and 1% of allyl polyethylene glycol by mass;
the number average molecular weight of the allyl polyethylene glycol is 600;
(2) dissolving 40g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 3: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 20g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 2: NaOH and NaNO of 13Composition is carried out; in N2Respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water under the protection condition, stirring for 24 hours at 90 ℃, carrying out solid-liquid separation, drying solids, and crushing to obtain calcium-aluminum type hydrotalcite-like compound;
(3) dissolving 6g of quaternary anionic copolymer in 10 mass times of boiled deionized water to obtain a solution C; dispersing 2g of calcium-aluminum hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protecting, mixing the solution C and the dispersion solution D, and reacting for 24 hours at 100 ℃ under the condition that the rotating speed is 500 revolutions per minute; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and grinding or crushing to obtain the slow-release fluid loss agent for seawater cementing.
Example 5
The preparation method of the slow-release fluid loss agent for seawater cementing comprises the following steps:
(1) dissolving 30g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 4 by using potassium hydroxide; adding potassium persulfate accounting for 0.8 percent of the total mass of the monomers, reacting for 2 hours at 80 ℃ under stirring, and cooling to room temperature to obtain a quaternary anion copolymer; the monomer consists of 82% of 2-acrylamide-2-methylpropanesulfonic acid, 3% of itaconic acid, 14% of acrylamide and 1% of allyl polyethylene glycol by mass;
the number average molecular weight of the allyl polyethylene glycol is 1200;
(2) dissolving 40g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 3: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 20g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 2: NaOH and NaNO of 13Composition is carried out; in N2Respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water under the protection condition, stirring for 24 hours at 90 ℃, carrying out solid-liquid separation, drying solids, and grinding to obtain calcium-aluminum type hydrotalcite-like compound;
(3) dissolving 6g of quaternary anionic copolymer in 10 mass times of boiled deionized water to obtain a solution C; dispersing 2g of calcium-aluminum hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protecting, mixing the solution C and the dispersion solution D, and reacting for 24 hours at 100 ℃ under the condition that the rotating speed is 500 revolutions per minute; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and grinding to obtain the slow-release fluid loss agent for seawater cementing.
Comparative example 1
A preparation method of AMPS-NNDMA-MA (ANM) ternary short-side-chain anionic fluid loss agent comprises the following steps:
dissolving 31.2g of 2-acrylamide-2-methylpropanesulfonic acid, 1.2g of maleic acid and 6g N, N-dimethylacrylamide in sequence in 110mL of deionized water;
stirring uniformly at normal temperature, and adjusting the pH value of the solution to 6 by using sodium hydroxide; adding ammonium persulfate accounting for 0.6 percent of the total mass of the monomers, stirring and reacting for 4 hours at 70 ℃, cooling to room temperature, and carrying out vacuum freeze-drying to obtain the short side chain anionic fluid loss agent ANM.
Comparative example 2
A preparation method of AMPS-NNDMA-MA-APEG (ANMA) quaternary long side chain anionic fluid loss agent comprises the following steps:
dissolving 25g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 6 by using sodium hydroxide; adding ammonium persulfate accounting for 0.6 percent of the total mass of the monomers, reacting for 4 hours at 70 ℃ under stirring, and cooling to room temperature to obtain a quaternary long side chain anionic fluid loss additive (anionic copolymer ANMA); the monomer consists of 78% of 2-acrylamide-2-methylpropanesulfonic acid, 4% of maleic acid, 15% of N, N-dimethylacrylamide and 3% of allyl polyethylene glycol by mass;
the number average molecular weight of the allyl polyethylene glycol is 600;
evaluation of Cement slurry Properties according to the national Standard SY/T5504.2-2013 oil well Cement Admixture evaluation method part 2: the method of fluid loss agent was used for the relevant experiments.
The fluid loss agents of examples and comparative examples were evaluated for their properties of fluid loss, fluidity and compressive strength, and the results of the evaluation are shown in tables 1, 2 and 3.
TABLE 1 water loss test results of slow-release type fluid loss additive for seawater cementing under fresh water or seawater slurry mixing conditions
Note: the formula of the cement paste is as follows: 800g G grade Jiahua oil well cement, 4 percent fluid loss additive and 44 percent fresh water or seawater. (/% is the percentage content of bulk fluid loss additive in G-grade Jiahua oil well cement)
Table 2 test results of fluidity of slow-release fluid loss additive for seawater cementing at different hydration times under the condition of seawater slurry mixing
Note: the formula of the cement paste is as follows: 800g G grade Jiahua oil well cement, 4 percent fluid loss additive and 44 percent seawater. (/% is the percentage content of the fluid loss agent in G-level Jiahua oil well cement)
Table 3 results of testing compressive strength of slow-release fluid loss additive for seawater well cementation in different curing times under condition of seawater slurry mixing
Note: the formula of the cement paste is as follows: 500g G grade Jiahua oil well cement, 4% fluid loss additive and 44% seawater. The curing conditions are as follows: 60 ℃ water bath under normal pressure, (/% is the percentage content of the fluid loss additive in G-grade Jiahua oil well cement)
As can be seen from Table 1, the difference between the water loss control effect of the cement slurry containing the fluid loss agent of the invention and the water loss control effect of the comparative example under the condition of stirring the slurry with fresh water is small, which indicates that all three fluid loss agents can be applied to the condition of stirring the slurry with fresh water; under the condition of mixing the slurry with seawater, the water loss control effect of the cement slurry containing the fluid loss agent of the embodiments 1-5 is obviously better than that of a comparative example sample, which shows that the fluid loss agent of the invention has good water loss control performance under the condition of mixing the slurry with seawater.
As can be seen from table 2, the fluidity of the fluid loss agent of the present invention corresponding to different hydration times is slightly decreased in the early stage of hydration, as compared with the comparative example, but after the anionic copolymer located between the calcium-aluminum type hydrotalcite laminate in the fluid loss agent of the present invention is gradually released, the fluidity gradually increases, and the fluidity is always maintained at 200mm or more within 120min, which indicates that the fluid loss agent of the present invention has better continuous dispersion performance for cement paste under the condition of seawater mixing.
As can be seen from Table 3, the strength development of the cement paste containing the fluid loss additive of examples 1-5 at 60 ℃ is closer to that of pure cement and the development trend is more stable, which indicates that the fluid loss additive of the present invention can effectively alleviate the over-retardation of the cement paste caused by the carboxyl group in the copolymer under the condition of seawater mixing.
In conclusion, the slow-release type water loss reducing agent for seawater cementing has a better water loss control effect than a comparative sample under the condition of seawater slurry mixing, and can more effectively disperse cement particles in a relatively long time period due to the slow-release function, so that the aim of continuous dispersion is fulfilled. Compared with a comparative example, the crystal seed effect of the calcium-aluminum hydrotalcite-like compound in the fluid loss agent disclosed by the invention promotes the hydration reaction of cement, and greatly relieves the over-retarding phenomenon of cement paste caused by carboxyl in the copolymer. The water loss reducing agent of the invention has the advantages of dispersion and early strength while ensuring the water loss effect under the condition of mixing the seawater with the slurry.
Fig. 1 is an XRD pattern of the calcium-aluminum type hydrotalcite-like compound prepared in example 1 and the slow-release fluid loss additive for seawater cementing. As shown in fig. 1b, the diffraction pattern of the calcium aluminum type hydrotalcite-like compound shows a typical layered structure with high crystallinity, and the diffraction peaks thereof are highly consistent with the standard diffraction card (fig. 1a) of the calcium aluminum type hydrotalcite-like compound shown in PDF # 54-0849. After anion exchange intercalation reaction, the diffraction peak of the slow-release fluid loss agent for seawater cementing is obviously moved to a small angle, and the crystallinity is reduced (figure 1 c). And the interplanar spacing corresponding to 1.8nm is much higher than that of the calcium-aluminum hydrotalcite-like compound (d value is 0.8nm), thus proving that macromolecular substances are inserted between the calcium-aluminum hydrotalcite-like compound laminates.
FIG. 2 is an infrared spectrum of the Ca-Al hydrotalcite-like compound prepared in example 1 and the slow-release fluid loss agent for seawater cementing. As shown in FIG. 2a, the calcium-aluminum type hydrotalcite-like compound was found to be 1385cm-1Absorption peaks for nitrate ions in the structure, 790,540 and 430cm-1Corresponding to lattice vibrations of Al-O and Ca-O octahedrons, respectively. The typical absorption peak of the slow-release fluid loss agent for seawater cementing is shown in fig. 2 b: at about 2900cm-1Stretching vibration of C-H bond in alkyl group is detected at 1050cm-1Ether linkages C-O-C were detected in the region and were at 1200cm-1S-O bonds in the sulfonic acid groups were detected. The peak of stretching vibration associated with carboxylic acid appeared at 1560 and 1455cm-1Nearby. Most importantly, when the quaternary anionic copolymer is inserted into the calcium-aluminum hydrotalcite-like interlayer, the absorption peak of nitrate almost disappears, which shows that nitrate ions between the calcium-aluminum hydrotalcite-like interlayers are polyanionic tetra-anionA anionically polymerized copolymer. The infrared data is combined with XRD results to confirm that the quaternary anionic copolymer and the calcium-aluminum hydrotalcite-like compound are subjected to anion exchange intercalation reaction, so that the slow-release fluid loss agent for seawater well cementation is successfully prepared.
FIG. 3 is a scanning electron microscope image of the calcium-aluminum hydrotalcite-like compound prepared in example 1 and the slow-release fluid loss agent for seawater cementing. As shown in fig. 3a, 3b and 3c, the scanning electron micrographs of the calcium aluminum type hydrotalcite-like compound show discrete and regular hexagonal crystal particles. In contrast, the morphology of the slow release fluid loss additive for seawater cementing shows irregular hexagonal plate morphology in fig. 3d, 3e and 3f, and large hexagonal crystal aggregates are formed under the action of the interlayer anionic polymer.
FIG. 4 is a transmission electron microscope image of the slow release type fluid loss agent for seawater cementing prepared in example 1. As shown in the figure, the slow-release fluid loss agent particles for seawater cementing have a typical layered structure, the dark line represents the skeleton of a calcium-aluminum type hydrotalcite-like layer, and the bright area represents the interlayer spacing occupied by the anionic polymer. These results show that the layered structure of the slow-release fluid loss additive for seawater cementing is kept intact after undergoing anion exchange intercalation reaction, thereby creating favorable conditions for the exchange of the slow-release fluid loss additive and anions in cement slurry.
FIG. 5 is a hydration isothermal calorimetry curve of the slow-release fluid loss additive for seawater cementing prepared in example 1 and a comparative example under a seawater slurry mixing condition. As is clear from fig. 5, the three fluid loss additives have different effects on the hydration of cement. On the one hand, adsorption of the comparative fluid loss additive containing unsaturated carboxyl groups on cement hydration products delays cement hydration, causes the main hydration peak in the hydration acceleration period to shift to the right, and reduces the total exotherm of hydration. On the other hand, the crystal structure of the aluminum-type hydrotalcite provided in example 1 is very similar to that of the calcium monosulfide aluminate in the cement hydration product, so that the hydration speed and degree of the cement are promoted, the cement paste hydration rate and the accumulated heat release curve are closer to those of pure cement, and no obvious retardation phenomenon is observed. The slow-release fluid loss agent for seawater cementing is proved to be beneficial to improving the early cement hydration speed.
FIG. 6 is a scanning electron microscope comparison of pure cement (a-c) and cement slurry (d-f) added with the slow release type fluid loss additive for seawater well cementation in example 1 under different curing time conditions. As shown in fig. 6a and d, the structure of the slow release type fluid loss additive cement paste for seawater cementing is denser than that of pure cement, and from the comparison graph, it can be seen that more crystals such as ettringite and calcium hydroxide are formed after the slow release type fluid loss additive for seawater cementing provided in example 1 is added to cement hydration (fig. 6b, c, e, f), which is also identical with the previous data of strength development, and it is proved that the slow release type fluid loss additive for seawater cementing is indeed beneficial to relieving the cement paste over-retarding phenomenon caused by unsaturated carboxyl in the polyanion admixture.
Claims (9)
1. The preparation method of the slow-release fluid loss agent for seawater cementing is characterized by comprising the following steps:
(1) dissolving 20-30g of monomer in 110mL of deionized water, stirring uniformly at normal temperature, and adjusting the pH value of the solution to 4-7; adding an initiator accounting for 0.4-0.8% of the total mass of the monomers, reacting for 2-6h at 60-80 ℃ under stirring, and cooling to room temperature to obtain a quaternary anionic copolymer; the monomer consists of 76 to 82 percent of 2-acrylamide-2-methylpropanesulfonic acid, 3 to 5 percent of unsaturated carboxylic acid, 14 to 16 percent of acrylamide substance and 1 to 3 percent of allyl polyethylene glycol by mass;
(2) dissolving 25-40g of mixed nitrate in 100mL of deionized water to prepare solution A; the mixed nitrate is prepared by mixing the following components in a molar ratio of 1-3: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20; dissolving 10-20g of sodium mixture in 100mL of deionized water to prepare a solution B; the sodium mixture is prepared by mixing the following components in a molar ratio of 1-2: NaOH and NaNO of 13Composition is carried out; in N2Respectively and simultaneously dripping the solution A and the solution B into 250ml of deionized water under the protection condition, stirring for 24-48 hours at 70-90 ℃, carrying out solid-liquid separation, drying the solid, and grinding or crushing to obtain calcium-aluminum type hydrotalcite;
(3) dissolving 3-6g quaternary anionic copolymer in 10 times by mass of boiling waterObtaining solution C in the ionized water; dispersing 1-2g of calcium-aluminum type hydrotalcite-like compound in 10 mass times of boiled deionized water to obtain a dispersion solution D; in N2Protection, mixing the solution C and the dispersion solution D, and reacting for 24-48h at 90-100 ℃ under the condition that the rotating speed is 200-; and (3) carrying out solid-liquid separation, washing, carrying out vacuum freeze-drying on the solid, and grinding or crushing to obtain the slow-release fluid loss agent for seawater cementing.
2. The process as claimed in claim 1, wherein the initiator is ammonium persulfate, potassium persulfate or azodiisobutyramidine hydrochloride.
3. The process as set forth in claim 1, characterized in that the unsaturated carboxylic acids are maleic acid, acrylic acid and itaconic acid.
4. The method according to claim 1, wherein the acrylamide compound is acrylamide or N, N-dimethylacrylamide.
5. The process as claimed in claim 1, wherein the allylpolyethylene glycol has a number average molecular weight of 600-.
6. The method as set forth in claim 1, wherein the reaction time in step (1) is 4 hours.
7. The method as set forth in claim 1, characterized in that the mixed nitrate is prepared by mixing the nitrate in a molar ratio of 2: ca of 1 (N0)3)2.4H20 and A1 (N0)3)3.9H20.
8. The method of claim 1, wherein the sodium mixture is prepared by mixing sodium and sodium in a molar ratio of 2: NaOH and NaNO of 13And (4) forming.
9. The slow release fluid loss agent for seawater well cementation prepared by the method of any one of claims 1 to 8.
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| CN111484047A (en) * | 2020-04-20 | 2020-08-04 | 黑龙江大学 | Preparation method and application of environment-friendly concrete surface anti-freezing coating |
| CN112080263B (en) * | 2020-09-21 | 2022-05-20 | 西南石油大学 | Preparation method of slow-release retarder for well cementation |
| CN114395074B (en) * | 2022-01-18 | 2023-01-17 | 天津大学 | Organic-inorganic hybrid fluid loss agent for oil well cement, preparation method and application |
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