CN111253519A - High-temperature-resistant oil well cement retarder and preparation method thereof - Google Patents
High-temperature-resistant oil well cement retarder and preparation method thereof Download PDFInfo
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- CN111253519A CN111253519A CN202010167148.XA CN202010167148A CN111253519A CN 111253519 A CN111253519 A CN 111253519A CN 202010167148 A CN202010167148 A CN 202010167148A CN 111253519 A CN111253519 A CN 111253519A
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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
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- 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
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Abstract
The invention relates to a high-temperature-resistant oil well cement retarder which comprises 2-methyl-2-acrylamide propyl sulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone, wherein the mass ratio of the 2-methyl-2-acrylamide propyl sulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropyl acrylamide and the N-vinyl pyrrolidone is 90-115: 10-16: 4-10:12-25: 7-15; the preparation method comprises the following steps: weighing the raw materials according to the mass ratio, placing the raw materials in water to be dissolved into a mixed solution, adjusting the pH value of the mixed solution to be 4-7, heating the solution in water bath), gradually dropwise adding an initiator into the solution, and continuously reacting for 2-4 hours to obtain the retarder. The invention has good temperature resistance, good salt resistance, stable chemical property and good compatibility.
Description
Technical Field
The invention belongs to the technical field of oil well cement retarders, and particularly relates to a high-temperature-resistant oil well cement retarder and a preparation method thereof.
Background
The well cementation is a main link in the process of oil well construction, and the quality of the well cementation is directly related to the continuous drilling of an oil well and the quality of various subsequent operations such as well completion, oil extraction, well repair and the like. The well cementing operation has two links, namely casing running and cement injection, and through the cement injection construction, the annular space between the casing and the well hole is filled with oil well cement, and the cement slurry mainly has the functions of isolating fluid from flowing between layers, supporting the casing, preventing corrosion of the pipe wall, isolating a leakage layer or a low-pressure layer and the like.
The cement grout operation process requires that the cement grout has certain pumpability, and the cement grout operation in-process because cement grout constantly to the motion of opening the end, the cement grout temperature constantly risees, and cement grout hydration reaction speed is accelerated, and the cement grout consistency will be increased, and when increasing to a definite value, the cement grout will lose the unable pumping of mobility. Therefore, for the well cementation operation of a high-temperature deep well, the bottom temperature is high, and a retarder for delaying the thickening time of cement paste is added into the cement paste, so that the construction safety is improved.
The conventional retarders used in the well cementation cement slurry at present are of the following types: lignosulfonate and its derivant, can apply to the well cementation operation of the bottom temperature of 150 duC, sulfonate tannin, sodium tannate, this kind of coagulant is made by the root, stem of the plant after sulfomethylation and alkali liquor action, this kind of retarder has obvious influence on cement strength under the high temperature condition, cellulose derivant type retarder has increasing the characteristic of sticking, salt resistance is bad; hydroxycarboxylic acid and salts thereof, including tartaric acid and salts thereof, sugar retarders and organic phosphonic acid, wherein the tartaric acid and salts thereof belong to high-temperature retarders, the addition sensitivity is strong, and the glucose retarders have strong retarding effect and also have the problem of addition sensitivity; other retarders also include inorganic compounds such as boric acid, phosphoric acid, hydrofluoric acid, and salts thereof, oxides of zinc and lead, and the like.
In the longitudinal direction, the existing oil well cement retarder has the defects of large or small size, and obviously adverse effects can be generally generated on other properties of cement paste while the hydration reaction of the cement paste is delayed, such as thinning of the cement paste and influence on the development of cement strength, so that the well cementation quality can not be powerfully ensured.
Therefore, based on the problems, the high-temperature-resistant oil well cement retarder with good temperature resistance, good salt resistance, stable chemical property and good compatibility and the preparation method thereof are provided, and have important practical significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-temperature-resistant oil well cement retarder with good temperature resistance, good salt resistance, stable chemical property and good compatibility and a preparation method thereof.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the high-temperature-resistant oil well cement retarder comprises 2-methyl-2-acrylamido propanesulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone, wherein the mass ratio of the 2-methyl-2-acrylamido propanesulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropyl acrylamide and the N-vinyl pyrrolidone is 90-115: 10-16: 4-10:12-25:7-15.
The preparation method of the high-temperature-resistant oil well cement retarder comprises the following steps:
(1) respectively weighing 2-methyl-2-acrylamido propanesulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone according to the mass ratio, and placing the weighed materials in water to be dissolved into a mixed solution;
(2) adjusting the pH value of the mixed solution in the step (1) to 4-7;
(3) heating the solution in water bath;
(4) and (4) gradually dropwise adding an initiator into the solution obtained in the step (3), and continuously reacting for 2-4 hours to obtain the retarder.
Further, the mass of the water in the step (1) is 230% of the total mass of the 2-methyl-2-acrylamidopropanesulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropyl acrylamide and the N-vinyl pyrrolidone.
Further, the pH value is adjusted in the step (2) by dripping NaOH solution with the concentration of 20%.
Further, the heating temperature of the water bath in the step (3) is 50-80 ℃.
Further, in the step (4), the initiator is ammonium persulfate-sodium bisulfite, and the mass of the initiator is 0.4-2.0% of the total mass of the 2-methyl-2-acrylamidopropanesulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropylacrylamide and the N-vinylpyrrolidone.
In the above scheme, 2-methyl-2-acrylamidopropanesulfonic acid is abbreviated as AMPS, itaconic acid is abbreviated as IA, acrylic acid is abbreviated as AA, N, N-dimethylaminopropylacrylamide is abbreviated as DMAPAA, and N-vinylpyrrolidone is abbreviated as NVP.
The polymer is prepared from 2-methyl-2-acrylamido propanesulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone, wherein the five monomers all contain unsaturated bonds, wherein itaconic acid molecules contain two retarding groups (-COOH), DMAPAA with amino groups is introduced on side chains while the-COOH is grafted to a copolymer main chain to enhance adsorption, AMPS has a large number of side groups and good high temperature resistance and synergy, and sulfonate groups in the copolymer have high temperature resistance, salt resistance and hydration capability, so that the polymer can exist stably at high temperature; each itaconic acid molecule also has two carboxylic acid groups, has good retardation effect, and realizes retardation effect mainly through adsorption and chelation; acrylic acid containing-COOH can also play a role in retarding coagulation, weaken the strong adsorption of itaconic acid and increase the stability of slurry; DMAPAA is unsaturated tertiary amine containing amino group, which can improve the salt resistance of high molecular polymer and the stability of cement slurry; NVP contains a chain rigid group, can enhance the temperature resistance of the polymer, simultaneously improves the slurry stability, and has a synergistic effect together with DMAPAA.
The invention has the advantages and positive effects that:
1. the retarder has good temperature resistance, the temperature resistance reaches 180 ℃, and the thickening time is adjustable; the salt resistance is good, and the adjustment of the thickening time of the cement paste can be realized in the half-saturated saline water; the chemical property is stable, the sensitivity coefficient is low, and the linearity of a thickening curve is good;
2. the retarder can be suitable for large-temperature-difference well cementation, and the strength of the cement stone can be rapidly developed under the medium-low temperature condition; the high-temperature sedimentation stability of the cement paste is good; the compatibility is good, can be compatible with various admixtures, and is suitable for cement of various grades specified by API;
3. the retarder has wide applicable temperature range and excellent performance within 30-180 ℃.
Detailed Description
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, and furthermore, the terms "comprises" and "having", and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
Example 1
The high-temperature-resistant oil well cement retarder comprises 2-methyl-2-acrylamido propanesulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone, wherein the mass ratio of the 2-methyl-2-acrylamido propanesulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropyl acrylamide and the N-vinyl pyrrolidone is 90-115: 10-16: 4-10:12-25:7-15.
In this embodiment, the preparation method of the high temperature resistant oil well cement retarder of the present invention comprises:
weighing 100g of AMPS, 13g of itaconic acid, 6g of acrylic acid, 20g of DMAPAA and 8g of NVP, and dissolving by using water with the mass percent of 230 percent of the total mass of the five monomers; then, dropwise adding a 20% NaOH solution to adjust the pH value of the mixed solution to 5-7, and pouring the adjusted mixed solution into a three-neck flask with a thermometer, a stirrer and a constant-pressure dropping funnel; wherein the thermometer is used for checking the temperature of the solution in the three-neck flask at any time; the stirrer is used for stirring the solution, enhancing the dissolution of various substances in the solution and promoting the chemical reaction of the solution; the constant-pressure dropping funnel is used for assisting the solution to be dropped into the three-neck flask, so that the progress of chemical reaction is controlled; after all the mixed solution is placed in the three-neck flask, placing the three-neck flask in water, and carrying out constant-temperature water bath at the temperature of 60 ℃; when the water bath temperature reaches 60 ℃, gradually dropping an ammonium persulfate-sodium bisulfite initiator into the three-neck flask through a constant pressure dropping funnel, wherein the use amount of the ammonium persulfate-sodium bisulfite does not exceed 2 percent of the total mass of the five monomers of AMPS, IA, AA, DMAPAA and NVP; and under the action of an initiator, continuously reacting the mixed solution in the three-neck flask for three hours to obtain a polymer, namely the high-temperature-resistant oil well cement retarder.
After the high-temperature-resistant oil well water-mixing retarder is prepared, the retarder is applied to oil well cementing construction; taking Jiahua G-grade cement as an example, cement paste with the water cement ratio of 0.44 is prepared according to the API standard, then the retarder sample is added for carrying out the cement paste performance measurement, and the results are shown in Table 1.
TABLE 1 evaluation results of Cement mortar Properties
In table 1, formulas 1-4 are Jiahua grade G cement + retarder + defoamer; the formulation No. 5-13 is Jiahua G-grade cement, 35 percent of silicon powder, retarder and 0.2 percent of defoamer; the 14-15 formula comprises Jiahua G-grade cement, 35% of silicon powder, retarder, 0.2% of defoaming agent and half-saturated saline.
As can be seen from Table 1, the retarder of the invention has wide applicable temperature range, can adjust the thickening time of cement slurry within the range of 30-180 ℃, and has good slurry sedimentation stability; thickening time increases with increasing retarder addition, and is basically linear; the retarder also has strong low-temperature early strength, and is suitable for long sealing section and large temperature difference well cementation operation; in the semi-saturated saline, the addition of the retarder is reduced, the thickening time of the cement paste can be adjusted, the super-retarding phenomenon does not occur, and the better salt resistance is shown.
It should be noted that the index of the pressure resistance in table 1 is not tested under some conditions, and is indicated by "-".
The present invention has been described in detail with reference to the above examples, but the description is only for the preferred examples of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (6)
1. The high-temperature-resistant oil well cement retarder is characterized in that: the adhesive comprises 2-methyl-2-acrylamido propanesulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone, wherein the mass ratio of the 2-methyl-2-acrylamido propanesulfonic acid to the itaconic acid to the acrylic acid to the N, N-dimethylaminopropyl acrylamide to the N-vinyl pyrrolidone is 90-115: 10-16: 4-10:12-25:7-15.
2. The method for preparing the high temperature resistant oil well cement retarder according to claim 1, wherein: the method comprises the following steps:
(1) respectively weighing 2-methyl-2-acrylamido propanesulfonic acid, itaconic acid, acrylic acid, N-dimethylaminopropyl acrylamide and N-vinyl pyrrolidone according to the mass ratio, and placing the weighed materials in water to be dissolved into a mixed solution;
(2) adjusting the pH value of the mixed solution in the step (1) to 4-7;
(3) heating the solution in water bath;
(4) and (4) gradually dropwise adding an initiator into the solution obtained in the step (3), and continuously reacting for 2-4 hours to obtain the retarder.
3. The method for preparing the high temperature resistant oil well cement retarder according to claim 2, characterized in that: the mass of the water in the step (1) is 230% of the total mass of the 2-methyl-2-acrylamidopropanesulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropylacrylamide and the N-vinylpyrrolidone.
4. The method for preparing the high temperature resistant oil well cement retarder according to claim 2, characterized in that: the pH value is adjusted in the step (2) by dropwise adding a NaOH solution with the concentration of 20%.
5. The method for preparing the high temperature resistant oil well cement retarder according to claim 2, characterized in that: the heating temperature of the water bath in the step (3) is 50-80 ℃.
6. The method for preparing the high temperature resistant oil well cement retarder according to claim 2, characterized in that: in the step (4), the initiator is ammonium persulfate-sodium bisulfite, and the mass of the initiator is 0.4-2.0% of the total mass of the 2-methyl-2-acrylamide-propanesulfonic acid, the itaconic acid, the acrylic acid, the N, N-dimethylaminopropyl acrylamide and the N-vinyl pyrrolidone.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662409A (en) * | 2020-06-30 | 2020-09-15 | 天津大学 | High-temperature oil well cement retarder capable of inhibiting abnormal gelation and preparation method thereof |
| CN115893900A (en) * | 2021-09-30 | 2023-04-04 | 中石化石油工程技术服务有限公司 | Phosphoaluminate cement multi-copolymerization retarder suitable for deep shale gas well cementation and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967371A (en) * | 2010-08-18 | 2011-02-09 | 成都欧美科石油科技股份有限公司 | High temperature resistant oil well cement retarder and preparation method thereof |
| CN105061661A (en) * | 2015-08-06 | 2015-11-18 | 中国石油集团渤海钻探工程有限公司 | Medium-high temperature delayed coagulant used for oil well cement and preparation method thereof |
| CN106188395A (en) * | 2016-07-14 | 2016-12-07 | 石家庄市长安育才建材有限公司 | A kind of preparation method of micro-cross-linked structure high temperature resistant salt tolerant cementing slurry fluid loss agent |
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2020
- 2020-03-11 CN CN202010167148.XA patent/CN111253519A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967371A (en) * | 2010-08-18 | 2011-02-09 | 成都欧美科石油科技股份有限公司 | High temperature resistant oil well cement retarder and preparation method thereof |
| CN105061661A (en) * | 2015-08-06 | 2015-11-18 | 中国石油集团渤海钻探工程有限公司 | Medium-high temperature delayed coagulant used for oil well cement and preparation method thereof |
| CN106188395A (en) * | 2016-07-14 | 2016-12-07 | 石家庄市长安育才建材有限公司 | A kind of preparation method of micro-cross-linked structure high temperature resistant salt tolerant cementing slurry fluid loss agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662409A (en) * | 2020-06-30 | 2020-09-15 | 天津大学 | High-temperature oil well cement retarder capable of inhibiting abnormal gelation and preparation method thereof |
| CN115893900A (en) * | 2021-09-30 | 2023-04-04 | 中石化石油工程技术服务有限公司 | Phosphoaluminate cement multi-copolymerization retarder suitable for deep shale gas well cementation and preparation method and application thereof |
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