CN114395074B - Organic-inorganic hybrid fluid loss agent for oil well cement, preparation method and application - Google Patents
Organic-inorganic hybrid fluid loss agent for oil well cement, preparation method and application Download PDFInfo
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- CN114395074B CN114395074B CN202210053757.1A CN202210053757A CN114395074B CN 114395074 B CN114395074 B CN 114395074B CN 202210053757 A CN202210053757 A CN 202210053757A CN 114395074 B CN114395074 B CN 114395074B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
Abstract
The invention discloses a preparation method and application of an organic-inorganic hybrid fluid loss agent for oil well cement, wherein the preparation method comprises the following steps: adding 2-acrylamide-2-methylpropanesulfonic acid, acrylamide monomer, carboxylic acid monomer and sodium p-styrenesulfonate into distilled water, stirring uniformly at normal temperature, and adjusting pH; after adding an initiator, heating for reaction to obtain a liquid anionic polymer fluid loss agent; mixing the liquid anionic polymer fluid loss agent with magnesium-aluminum type hydrotalcite, stirring for 6-8 hours at 65-75 ℃, settling, washing with water, centrifuging, freeze-drying and grinding to obtain the organic-inorganic hybrid fluid loss agent for oil well cement. The water is used as a dispersing medium, the preparation process is simple, the cost is low, the fluid loss agent can effectively reduce the water loss amount of cement paste at high temperature, improves the over-retarding phenomenon of the single polymer fluid loss agent to the cement paste, has better adaptability to oil well cement, and is suitable for being used as the fluid loss agent of the oil well cement.
Description
Technical Field
The invention relates to the technical field of oil well cement additives, in particular to an organic-inorganic hybrid fluid loss agent for oil well cement, a preparation method and application thereof.
Background
In oil gas well cementing engineering, the loss of water of cement slurry can cause the mobility to reduce, the annular space mud cement-water ratio reduces, the oil gas channeling possibility increases the other problems, and in severe cases, the cement slurry can not be pumped, resulting in failure of well cementing. The mud filtrate, if it enters the reservoir, can contaminate the oil and gas products in the deep well. Therefore, the fluid loss agent is required to be added into oil well cement to reduce the water loss of the cement slurry, ensure the fluidity of the cement slurry, and further ensure the safety of well cementation and improve the well cementation efficiency.
The performance of cement additives for well cementing is placing higher demands on the drilling depth, bottom hole pressure and bottom hole temperature as they continue to increase. Under the high temperature condition at the bottom of a deep well, the structure of cement slurry cannot bear the harsh condition, so the cement slurry plays a limited role in a well cementation project, and the well cementation quality is reduced. Most of the currently applied representative fluid loss agents are synthetic polymer fluid loss agents, such as polyvinyl alcohol fluid loss agents; anionic acrylamide copolymer fluid loss agents. In order to meet the harsh requirements of the existing well cementation engineering on the oil well cement fluid loss additive, the two have certain defects: the polyvinyl alcohol fluid loss agent has poor temperature resistance and cannot meet the requirements of the existing well cementation work; for the anionic acrylamide type fluid loss agent, the amide group is very easy to hydrolyze into carboxylic acid group at high temperature, which affects the early strength development of cement and can not meet the requirements of the well cementation of oil and gas wells at the present stage.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the organic-inorganic hybrid fluid loss additive for oil well cement, which has strong fluid loss reducing capability on oil well cement slurry.
The second purpose of the invention is to provide a preparation method of the organic-inorganic hybrid fluid loss agent for oil well cement.
The third purpose of the invention is to provide the application of the organic-inorganic hybrid fluid loss agent for the oil well cement.
The technical scheme of the invention is summarized as follows:
a preparation method of an organic-inorganic hybrid fluid loss agent for oil well cement comprises the following steps:
(1) Weighing 12 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 2-4 parts of acrylamide monomer, 0.5-1.5 parts of carboxylic acid monomer and 3-5 parts of Sodium Styrene Sulfonate (SSS) by mass, adding into 75-85 parts of distilled water, stirring uniformly at normal temperature, and adjusting the pH to 4-7; adding 0.1-0.15 part of initiator at 55-65 ℃, heating to 65-75 ℃, and keeping reacting at 65-75 ℃ for 1.5-2.5h to obtain a liquid anionic polymer fluid loss agent;
(2) Mixing 150-250 parts of the liquid anionic polymer fluid loss agent obtained in the step (1) with 2-4 parts of magnesium-aluminum type hydrotalcite by mass, stirring at 65-75 ℃ for 6-8 hours, settling, washing with water, centrifuging, freeze-drying and grinding to obtain the organic-inorganic hybrid fluid loss agent for oil well cement.
The acrylamide monomer is preferably acrylamide or N, N-dimethylacrylamide.
The carboxylic acid monomer is preferably maleic anhydride, acrylic acid or itaconic acid.
The initiator is preferably ammonium persulfate, potassium persulfate or azobisisobutyramidine hydrochloride.
The organic-inorganic hybrid fluid loss agent for oil well cement prepared by the method.
The application of the organic-inorganic hybrid fluid loss agent for oil well cement is provided.
The invention has the advantages that:
(1) The invention takes water as a dispersion medium, has simple preparation process and low cost, and is easy to realize industrial production.
(2) The fluid loss agent can effectively reduce the water loss amount of cement paste at high temperature, improve the over-retarding phenomenon of the single polymer fluid loss agent on the cement paste, has better adaptability on oil well cement, and is suitable for being used as the fluid loss agent of the oil well cement.
(3) From the perspective of molecular structure design, the polymer fluid loss agent has excellent water loss control performance, and the prepared organic-inorganic hybrid fluid loss agent is suitable for higher use temperature by combining the high temperature resistance of hydrotalcite.
(4) According to the invention, the inorganic hydrotalcite and the organic polymer fluid loss agent are intercalated in an anion exchange mode, so that the early hydration of cement is promoted while the water loss of cement paste is reduced, and the early strength of the cement paste is improved.
(5) The invention makes the intercalation filtrate reducer slowly release the polymer filtrate reducer when reacting with cement slurry through anion exchange, and changes the one-time direct contact action mode into an intelligent response regulation action mode.
Drawings
FIG. 1 is an infrared spectrum of the organic-inorganic hybrid fluid loss additive for oil well cement prepared in example 4.
FIG. 2 is a scanning electron microscope image of the organic-inorganic hybrid fluid loss additive for oil well cement prepared in example 4.
FIG. 3 is a thermogravimetric plot of the organic-inorganic hybrid fluid loss additive for oil well cement prepared in example 4.
Detailed Description
The present invention will be further described with reference to the following examples.
The magnesium-aluminum type hydrotalcite is prepared by the following method:
dissolving 8-12 parts by mass of magnesium nitrate hexahydrate and 6-8 parts by mass of aluminum nitrate nonahydrate into 80-85 parts by mass of ultrapure water, and marking as solution A; dissolving 3-4 parts of sodium hydroxide in 90-95 parts of ultrapure water, and marking as a solution B; in thatN 2 Under the protection condition, 20-25 parts of the solution A and 20-25 parts of the solution B are dropwise added into 50-60 parts of ultrapure water, stirred at 85-95 ℃ for 20-30 hours, settled, washed, centrifuged, freeze-dried and ground to obtain the magnesium-aluminum type hydrotalcite, which is recorded as: mgAl-NO 3 -LDH。
Example 1
The magnesium-aluminum type hydrotalcite is prepared by the following method:
10.26g of magnesium nitrate hexahydrate and 7.5g of aluminum nitrate nonahydrate are dissolved in 82.24g of ultrapure water and marked as solution A; dissolving 4g of sodium hydroxide in 93g of ultrapure water, and marking as a solution B; in N 2 Under the protection condition, dropwise adding the 23g A solution and the 23g B solution into 55g of ultrapure water, stirring at 90 ℃ for 25 hours, settling, washing with water, centrifuging, freeze-drying and grinding to obtain the magnesium-aluminum type hydrotalcite, which is recorded as: mgAl-NO 3 -LDH-1。
Example 2
The magnesium-aluminum type hydrotalcite is prepared by the following method:
dissolving 8g of magnesium nitrate hexahydrate and 8g of aluminum nitrate nonahydrate in 80g of ultrapure water, and marking as A solution; dissolving 3g of sodium hydroxide in 90g of ultrapure water, and marking as a solution B; in N 2 Under the protection condition, dropwise adding the 20g A solution and the 25g B solution into 60g of ultrapure water, stirring at 85 ℃ for 30 hours, settling, washing with water, centrifuging, freeze-drying and grinding to obtain the magnesium-aluminum type hydrotalcite, which is recorded as: mgAl-NO 3 -LDH-2。
Example 3
The magnesium-aluminum type hydrotalcite is prepared by the following method:
dissolving 12g of magnesium nitrate hexahydrate and 6g of aluminum nitrate nonahydrate in 85g of ultrapure water, and marking as A solution; dissolving 4g of sodium hydroxide in 95g of ultrapure water, and marking as a solution B; in N 2 Dropwise adding the 25g A solution and the 20g B solution into 50g of ultrapure water under the protection condition, stirring at 95 ℃ for 20 hours, settling, washing with water, centrifuging, freeze-drying and grinding to obtain the magnesium-aluminum type hydrotalcite, which is recorded as: mgAl-NO 3 -LDH-3。
Example 4
A preparation method of an organic-inorganic hybrid fluid loss agent for oil well cement comprises the following steps:
(1) 24g of 2-acrylamide-2-methylpropanesulfonic acid, 6g of acrylamide, 2g of acrylic acid and 8g of sodium p-styrenesulfonate are weighed and added into 160g of distilled water, the mixture is stirred uniformly at normal temperature, and the pH value is adjusted to 5; adding 0.24g of ammonium persulfate at 60 ℃, heating to 70 ℃, and keeping the reaction at 70 ℃ for 2 hours to obtain a liquid anionic polymer fluid loss agent, which is marked as AAAS;
(2) 200g of the liquid anionic polymer fluid loss additive obtained in step (1) and 4g of MgAl-NO prepared in example 1 3 And (3) mixing the-LDH-1, stirring for 6 hours at 70 ℃, settling, washing, centrifuging, freeze-drying and grinding to obtain the organic-inorganic hybrid fluid loss agent for oil well cement, which is recorded as MgAl-AAAS-LDH.
Example 5
A preparation method of an organic-inorganic hybrid fluid loss agent for oil well cement comprises the following steps:
(1) 24g of 2-acrylamide-2-methylpropanesulfonic acid, 4g of N, N-dimethylacrylamide, 1g of maleic anhydride and 6g of sodium p-styrenesulfonate are weighed and added into 150g of distilled water, the mixture is stirred uniformly at normal temperature, and the pH value is adjusted to 4; adding 0.2g of potassium persulfate at 55 ℃, heating to 65 ℃, and keeping the reaction at 65 ℃ for 2.5 hours to obtain a liquid anionic polymer fluid loss agent, which is marked as ADMS;
(2) 150g of the liquid anionic polymer fluid loss additive obtained in step (1) and 2g of MgAl-NO prepared in example 2 3 And (3) mixing the-LDH-2, stirring for 8 hours at 65 ℃, settling, washing, centrifuging, freeze-drying and grinding to obtain the organic-inorganic hybrid fluid loss agent for oil well cement, which is recorded as MgAl-ADMS-LDH.
Example 6
A preparation method of an organic-inorganic hybrid fluid loss agent for oil well cement comprises the following steps:
(1) 24g of 2-acrylamide-2-methylpropanesulfonic acid, 8g of acrylamide, 3g of itaconic acid and 10g of sodium p-styrenesulfonate are weighed and added into 170g of distilled water, the mixture is stirred uniformly at normal temperature, and the pH value is adjusted to 7; adding 0.3g of azodiisobutyl amidine hydrochloride at 65 ℃, heating to 75 ℃, and keeping the reaction at 75 ℃ for 1.5 hours to obtain a liquid anionic polymer fluid loss agent, which is marked as AAIS;
(2) 250g of the liquid anionic polymer fluid loss additive obtained in step (1) and 3g of MgAl-NO prepared in example 3 3 And (4) mixing-LDH-3, stirring at 75 ℃ for 6 hours, settling, washing, centrifuging, freeze-drying and grinding to obtain the organic-inorganic hybrid fluid loss agent for oil well cement, which is recorded as MgAl-AAIS-LDH.
Comparative example 1
A preparation method of a ternary anionic fluid loss agent comprises the following steps:
weighing 30g of 2-acrylamide-2-methylpropanesulfonic acid, 7.5g of acrylamide and 2.5g of acrylic acid, adding the weighed materials into 160g of distilled water, stirring the materials uniformly at normal temperature, and adjusting the pH value to 5; after 0.24g of ammonium persulfate is added at 60 ℃, the temperature is raised to 70 ℃, and the reaction is maintained for 2 hours at 70 ℃ to obtain a ternary anionic fluid loss agent, which is marked as AAA.
Comparative example 2
The liquid anionic polymer fluid loss additive, obtained from the preparation of step (1) of example 4, is designated as AAAS.
And (3) testing the performance of the organic-inorganic hybrid fluid loss agent for oil well cement.
The preparation of cement paste and the performance test method are carried out according to GB/T19139-2012 'oil well cement test method'. The performance of the fluid loss additives prepared in example 4 and comparative examples 1 and 2 in terms of water loss and compressive strength was evaluated, and the evaluation results are shown in tables 1 and 2.
TABLE 1 static water loss test results of cement slurry with water loss reducing agent added after 240 deg.C curing
Note: the formula of the cement paste is as follows: 500G Jiahua G grade oil well cement +35% quartz sand +2% microsilica +1% high temperature stabilizer BCS-410S +0.5% high temperature stabilizer SW-91+0.3% aldehyde ketone polycondensate dispersant USZ +4% retarder GH-9+57% saline +1.6% fluid loss reducer. (BCS-410S from Chengdu Bo Wei science and technology, inc., SW-91 from Dezhou Ruifu oilfield additives science and technology, inc., USZ, GH-9 Wei Hui City, inc.)
TABLE 2 set of Cement containing fluid loss additive at 60 ℃ compressive Strength test results
Note: the formula of the cement paste is as follows: 500G Jiahua grade G oil well cement and 1.6 percent fluid loss additive.
Table 1 shows that the static water loss test of the cement paste is carried out after the water loss agent is added into the cement paste and cured at 240 ℃, so that the water loss control performance of the water loss agent is evaluated. As is clear from table 1, the organic-inorganic hybrid fluid loss additive for oil well cement prepared in example 4 has superior fluid loss reduction ability as compared with comparative examples 1 and 2.
Table 2 shows the compression strength of the set cement after curing the fluid loss additive added with cement paste at 60 ℃ for different days. As can be seen from Table 2, the cement comprising AAAS in comparative example 2 has a higher compressive strength than the cement comprising AAA in comparative example 1. After the MgAl-AAAS-LDH of example 4 was added to the cement, the strength of the set cement was greater than that of the pure cement. The cement stones cured for 3 and 7 days show the same rule. Therefore, the organic-inorganic hybrid fluid loss agent for oil well cement can improve the negative influence of a pure polymer fluid loss agent on the cement strength.
FIG. 1 is an infrared spectrum of the organic-inorganic hybrid fluid loss additive for oil well cement prepared in example 4. In the figure, a is MgAl-NO 3 1380cm in-LDH-1 -1 In hydrotalcite of NO 3 - B is 1650cm in MgAl-AAAS-LDH -1 The peak at (a) is the peak of C = O in AAAS; at 1550cm -1 The peak is the C-N stretching vibration peak in AAAS; at 1040cm -1 The peak at (A) is the stretching vibration peak of S = O and is at 1010cm -1 A small peak corresponding to the peak of flexural vibration of C-H in the benzene ring of sodium styrene sulfonate in AAAS appears. The infrared spectrum of MgAl-AAAS-LDH shows that the absorption peak of nitrate anions is weaker, which indicates that most anions of nitrate ions are replaced by polymer AAAS, and AAAS has been successfully intercalated into MgAl-NO 3 Of the-LDH-1, mgAl-AAAS-LDH was successfully synthesized.
FIG. 2 is a scanning electron microscope image of the organic-inorganic hybrid fluid loss agent for oil well cement prepared in example 4: (a) MgAl-NO 3 LDH-1 (b) MgAl-AAAS-LDH. As can be seen from the figure, mgAl-NO in (a) 3 The crystal grains of the LDH-1 are hexagonal, regular, ordered and comparatively dispersed. (b) The close packing of the platelets of MgAl-AAAS-LDH and the smaller voids shown in the figure may be due to interactions resulting from the proximity of the grains to each other due to the insertion of the molecules of the fluid loss agent copolymer between the hydrotalcite platelet structures, the grain boundaries between the grains being less pronounced but the grains still being in a lamellar distribution.
FIG. 3 is a thermogravimetric plot of the organic-inorganic hybrid fluid loss additive for oil well cement prepared in example 4 (wherein a is the thermogravimetric curve of AAAS prepared in the (1) th step of example 4, and b is the thermogravimetric curve of MgAl-AAAS-LDH prepared in example 4). It can be seen from (a) that the weight loss temperature of AAAS is 330 ℃. (b) It can be seen that the mass loss of the MgAl-AAAS-LDH sample can be mainly divided into three phases: (1) In the range of room temperature to 356 ℃, the weight reduction of the MgAl-AAAS-LDH samples is mainly due to thermal decomposition of free water and interlayer water; (2) The weight reduction of the MgAl-AAAS-LDH samples in the temperature range of 356 to 408 ℃ is mainly due to the decomposition of hydroxyl groups and anionic polymers between hydrotalcite mesolamella plates; (3) The weight reduction of the MgAl-AAAS-LDH samples at temperatures above 408 ℃ is mainly due to the fact that the hydrotalcite layered structure has already started to gradually collapse. The loss in weight of the fluid loss agent AAAS after being inserted into the hydrotalcite layers is started from 356 ℃, so that the hydrotalcite plays a role in protecting the polymer fluid loss agent at high temperature.
Experiments prove that the water loss reducing capacity and the mechanical property of the water loss reducing agents prepared in the examples 5 and 6 in oil well cement are similar to those of the results in the example 4.
The organic-inorganic hybrid fluid loss agent for oil well cement has the advantages of simple preparation process, low cost, easiness in storage and the like. The organic polymer part of the fluid loss agent introduces sodium p-styrenesulfonate monomer, so that the fluid loss control capability of the fluid loss agent is improved at high temperature, and meanwhile, the fluid loss agent introduces hydrotalcite capable of anion exchange between laminates and the fluid loss agent to perform intercalation, so that the temperature resistance of the fluid loss agent is further improved, the polymer in the fluid loss agent is slowly released in cement and exerts the fluid loss performance, and the fluid loss agent can also promote the early hydration process of the cement, so that the early compressive strength of the set cement is improved. In general, the fluid loss agent of the present invention has excellent fluid loss performance in a cement slurry system, and is a high-efficiency fluid loss agent for oil well cement.
Claims (6)
1. A preparation method of an organic-inorganic hybrid fluid loss agent for oil well cement is characterized by comprising the following steps:
(1) Weighing 12 parts by mass of 2-acrylamide-2-methylpropanesulfonic acid, 2-4 parts by mass of acrylamide monomer, 0.5-1.5 parts by mass of carboxylic acid monomer and 3-5 parts by mass of sodium p-styrenesulfonate, adding into 75-85 parts by mass of distilled water, uniformly stirring at normal temperature, and adjusting the pH to 4-7; adding 0.1-0.15 part of initiator at 55-65 ℃, heating to 65-75 ℃, and keeping reacting at 65-75 ℃ for 1.5-2.5h to obtain a liquid anionic polymer fluid loss agent;
(2) Mixing 150-250 parts by mass of the liquid anionic polymer fluid loss agent obtained in the step (1) with 2-4 parts by mass of magnesium-aluminum type hydrotalcite, stirring at 65-75 ℃ for 6-8 hours, settling, washing with water, centrifuging, freeze-drying and grinding to obtain the organic-inorganic hybrid fluid loss agent for oil well cement.
2. The method according to claim 1, wherein the acrylamide monomer is acrylamide or N, N-dimethylacrylamide.
3. The method as claimed in claim 1, wherein the carboxylic acid monomer is maleic anhydride, acrylic acid or itaconic acid.
4. The process as set forth in claim 1, characterized in that said initiator is ammonium persulfate, potassium persulfate or azobisisobutyramidine hydrochloride.
5. An organic-inorganic hybrid fluid loss additive for oil well cement prepared according to the method of any one of claims 1-4.
6. The application of the organic-inorganic hybrid fluid loss additive for oil well cement as a fluid loss additive according to claim 5.
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