CN112250791A - Retarder with water loss reducing function and preparation method thereof - Google Patents
Retarder with water loss reducing function and preparation method thereof Download PDFInfo
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- CN112250791A CN112250791A CN202011131414.XA CN202011131414A CN112250791A CN 112250791 A CN112250791 A CN 112250791A CN 202011131414 A CN202011131414 A CN 202011131414A CN 112250791 A CN112250791 A CN 112250791A
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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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- C—CHEMISTRY; METALLURGY
- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
Abstract
The invention discloses a retarder with a water loss reducing function, which comprises AMPS, AA and an initiator, wherein the monomer molar ratio of AMPS to AA is (30-80): (20-70); the initiator is redox initiator, the initiator is redox protogen of ammonium persulfate-sodium bisulfite, and the addition amount of the initiator is 0.5-2.5% of the mass of the monomer. In addition, the invention also discloses a preparation method of the retarder with the water loss reducing function; according to the invention, through researches on monomer ratio, reaction PH value, reaction temperature, initiator addition and reaction time, various parameters in the preparation of the retarder are accurately controlled, and the prepared retarder can play a role in prolonging thickening time of cement paste and simultaneously does not influence water loss of the cement paste.
Description
Technical Field
The invention relates to the technical field of oil field well cementation additives, in particular to a retarder with a water loss reducing function; in addition, the invention also relates to a preparation method of the retarder with the water loss reducing function.
Background
In the process of exploration and development of oil and gas fields, the well cementation engineering is an important link of well drilling and completion engineering, and the quality of well cementation is not only a premise that engineering operations such as subsequent exploitation, enhanced reservoir transformation and the like are normally implemented, but also an important guarantee that the normal production life of the oil and gas wells is prolonged, the productivity is found and fully improved, and the exploration and development benefits of the oil and gas fields are improved. The retarder for well cementation plays an important role in the current well cementation construction, and is important for the construction safety and the well cementation quality. However, the retarder has a certain effect on controlling the water loss of the cement paste. The water loss of the cement paste can cause damage to the stratum, thicken the cement paste, increase the pumping pressure and cause the risk of early solidification, and meanwhile, the large water loss is also one of the main reasons for causing gas channeling. Thus, various additives and cement slurry systems have been developed for preventing water loss in cement slurries at home and abroad.
The application numbers are: CN201510717589.1, publication no: the invention patent of CN106632842B discloses a preparation and application method of an oil well cement retarder. The preparation method comprises the steps of dissolving the alkene monomer with the anionic sulfonic acid group, the alkene monomer with the ammonium cation and the unsaturated monomer containing the carboxylic acid group in deionized water, adjusting the pH value of the system, adding the initiator under the condition of introducing nitrogen, and continuously reacting in a constant-temperature water bath to obtain the oil well cement retarder. The application method is that the micro-silicon, the glass micro-beads, the fluid loss additive, the dispersing agent, the obtained oil well cement retarder and the cement are mixed according to the proportion, and water is added to prepare a cement paste system. The invention has the following beneficial effects: (1) the stability is good, the degradation resistance and the high-temperature resistance are good under the high-temperature environment; (2) the applicable temperature difference range is large and can reach 50-150 ℃; (3) the cement can achieve ideal retarding effect in a cement system, has no super retarding phenomenon, has fast strength development of the cement stone at the top, and meets the requirement of large temperature difference well cementation.
However, for controlling water loss of cement paste, the existing method is single, so that a retarder which can prolong thickening time of the cement paste, does not influence water loss of the cement paste and even has a certain water loss reducing function is needed.
Disclosure of Invention
The invention aims to provide a retarder with a water loss reducing function, which has the function of prolonging thickening time of cement paste and does not influence water loss of the cement paste. In addition, the invention also discloses a preparation method of the retarder.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a retarder with a water loss reducing function comprises AMPS, AA and an initiator, wherein the monomer molar ratio of AMPS to AA is (30-80): (20-70); the initiator is redox initiator, the initiator is redox protogen of ammonium persulfate-sodium bisulfite, and the addition amount of the initiator is 0.5-2.5% of the mass of the monomer.
Further optimizing, the monomer molar ratio of AMPS to AA is 70: 30.
further defined, the initiator is added in an amount of 1% by mass of the monomers.
The preparation method of the retarder disclosed by the invention comprises the following steps:
step 1: weighing AMPS, and dissolving the AMPS in deionized water to enable the monomer concentration to be 25%; weighing AA and dissolving AA in deionized water to ensure that the monomer concentration is 25 percent;
step 2: mixing the AMPS and AA solutions prepared in the step 1, and adjusting the pH value to 3-11 by using a sodium hydroxide solution with the concentration of 20%;
and step 3: adding the mixed solution obtained in the step 2 into a three-neck flask, uniformly mixing the solution through a stirrer, and introducing nitrogen into the solution for deoxygenation, wherein the nitrogen introducing time is as follows: 10 min;
and 4, step 4: after the oxygen removal step was completed, the three-necked flask was placed in a water bath to raise the temperature to 70 ℃, and then an initiator of 1% by mass of the monomer was added to the solution, and the temperature was kept constant at 70 ℃ and continuously stirred for 5 hours.
In step 2, PH is 5.
Further limiting, in step 4, the stirring speed is 150-200 r/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention can reach the same thickening time under the condition of small addition amount, and has low temperature and addition amount sensitivity.
2. The invention helps the cement slurry to lose water, and provides favorable support for the well cementation safety and the well cementation quality.
3. The invention has good compatibility with other well cementation additives, is easy to adjust and control and has stable system.
4. The invention has simple production process, low cost and stable product quality.
5. The invention has the functions of prolonging the thickening time of the cement paste and not influencing the water loss of the cement paste.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic flow diagram of the present invention for preparing a retarder.
FIG. 2 is a graph of the amount of water loss of the retarder prepared according to the present invention versus a conventional retarder in use.
FIG. 3 is a plot of monomer molar ratio of AMPS to AA versus thickening time for the present invention.
FIG. 4 is a graph of pH versus thickening time for retarders made according to the present invention.
FIG. 5 is a graph of reaction temperature versus thickening time for retarder preparations of the present invention.
FIG. 6 is a graph of initiator loading versus thickening time for a retarder of the present invention.
FIG. 7 is a graph of reaction time versus thickening time for retarder preparations of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Example one
The embodiment discloses a retarder with a water loss reducing function, which comprises AMPS, AA and an initiator, wherein the monomer molar ratio of AMPS to AA is (30-80): (20-70); the initiator is redox initiator, the initiator is redox protogen of ammonium persulfate-sodium bisulfite, and the addition amount of the initiator is 0.5-2.5% of the mass of the monomer.
In this example, the monomer molar ratio of AMPS to AA was 70:30, of a nitrogen-containing gas; the amount of initiator added is 1% of the mass of the monomers.
Example two
This example is substantially similar to the first example except that the monomer molar ratio of AMPS to AA is 80: 20; the initiator addition was 0.5% of the mass of the monomers.
EXAMPLE III
This example is substantially similar to the first example except that the monomer molar ratio of AMPS to AA is 73: 27; the initiator addition was 1.5% of the mass of the monomers.
Example four
This example is substantially similar to the first example except that the monomer molar ratio of AMPS to AA is 50: 50; the amount of initiator added is 1% of the mass of the monomers.
EXAMPLE five
This example is substantially similar to the first example except that the monomer molar ratio of AMPS to AA is 40: 60, adding a solvent to the mixture; the initiator is added in an amount of 2% by mass based on the mass of the monomers.
Example 6
This example is substantially similar to the first example except that the monomer molar ratio of AMPS to AA is 30: 70; the initiator addition was 2.5% of the monomer mass.
Example 7
The embodiment discloses a preparation method of the retarder in the first embodiment, referring to the attached figure 1 of the specification, comprising the following steps:
step 1: weighing AMPS, and dissolving the AMPS in deionized water to enable the monomer concentration to be 25%; weighing AA and dissolving AA in deionized water to ensure that the monomer concentration is 25 percent;
step 2: mixing the AMPS and AA solutions prepared in the step 1, and adjusting the pH value to 3-11 by using a sodium hydroxide solution with the concentration of 20%;
and step 3: adding the mixed solution obtained in the step 2 into a three-neck flask, uniformly mixing the solution through a stirrer, and introducing nitrogen into the solution for deoxygenation, wherein the nitrogen introducing time is as follows: 10 min;
and 4, step 4: after the oxygen removal step was completed, the three-necked flask was placed in a water bath to raise the temperature to 70 ℃, and then an initiator of 1% by mass of the monomer was added to the solution, and the temperature was kept constant at 70 ℃ and continuously stirred for 5 hours.
Further preferably, in step 2 of this embodiment, PH is 5.
Further, in step 4 of this embodiment, the stirring speed is 150-.
The invention is further illustrated below with reference to specific preparation cases and procedures:
29.015g of AMPS were weighed out and dissolved in deionized water to give a monomer concentration of 25%. Weighing 4.32g of AA, dissolving in deionized water to enable the monomer concentration to be 25%, then uniformly mixing the two solutions, adjusting the pH value to be 5 by using a 20% sodium hydroxide solution, and pouring the mixed solution into a three-neck flask. The stirrer is started to uniformly mix the solution, and nitrogen is introduced for 10 minutes to remove oxygen. The water bath was opened and the temperature was raised to 70 ℃. Adding an initiator accounting for 1 percent of the mass of the monomer into the solution, and stirring for 5 hours at the constant temperature of 70 ℃. After 5h the reaction was complete and the product copolymer solution was taken out.
The monomer molar ratio of AMPS to AA, the reaction pH, the reaction temperature, the initiator charge and the reaction time have a considerable influence on the thickening time.
Therefore, in the production, each production requirement and parameters need to be strictly controlled.
Since the monomer ratio has a large influence on the product, as shown in the attached FIG. 3, the monomer ratio is different, and the number of the adsorption groups and the hydration groups in the product is different, the monomer molar ratio is selected to be 70:30(AMPS: AA) in this example.
Because the pH value of the reaction system has a large influence on the result, the retarder synthesized in an alkaline environment has a particularly poor retarding effect, as shown in the attached figure 4 of the specification. The retarder synthesized under the weakly acidic condition of pH 5 exhibited the best retardation effect, and therefore, in this example, the pH of the reaction system was 5.
When the temperature is too low, the number of free radicals is small, the activity is low, the polymerization reaction speed is slow, and the conversion rate is low; at too high a temperature, a large amount of initiator thermally decomposes to rapidly generate a large amount of free radicals to initiate polymerization, which results in too rapid or even violent polymerization. The proper temperature can improve the polymerization activity of the monomer, thereby changing the performance of the copolymer and enhancing the retardation effect; as shown in FIG. 5, the properties of the copolymer product were the best when the temperature for the continuous reaction was 70 ℃ and, therefore, 70 ℃ was used as the temperature for the copolymerization reaction in this example.
As shown in the attached figure 6 of the specification, when the amount of the initiator is less, the molecular chain of the product is longer, the molecular chain is curled, partial carboxyl and hydroxyl groups playing a retarding role are wrapped at the inner side, the retarding effect is weakened, and meanwhile, the initiator is completely consumed before the induction period is finished, so that the monomer cannot be completely polymerized, and the product conversion rate is lower. When the initiator dosage is more than 1%, the synthesized polymer molecules are in an extended state, active groups are arranged on the side surfaces of the molecules and are exposed outside, the retarding performance of the polymer is fully exerted, and the retarding effect reaches the maximum value. Meanwhile, the concentration of the initiator is too high, and the concentration of free radicals of the system is too high in the polymerization process, so that the polymerization rate of the system is increased, the heat release is more, the temperature is increased quickly, the decomposition rate of the initiator is increased, the chain termination reaction is increased, the polymerization degree is reduced, the molecular weight is reduced, and the retardation is weakened; thus, in this example, the redox initiator ammonium persulfate-sodium bisulfite was used in an amount of 1% by mass of the monomers.
As shown in the attached figure 7 of the specification, the retardation effect is increased when the monomer conversion rate is higher along with the increase of the reaction time, and when the reaction time reaches 5 hours, the retardation effect is not obviously changed any more, and the reaction is basically finished; therefore, the reaction time is set to 5h in this embodiment.
The retarder prepared by the preparation method disclosed by the invention is used with a conventional retarder, and the results are compared, wherein the water loss result is shown in the attached figure 2 in the specification. The coagulant synthesized by the invention has water loss smaller than that of the conventional retarder.
The invention can solve the technical problem that the retarder influences the water loss of cement paste; besides, the retarder and common additives can be prepared into a double-acting cement paste system.
According to the invention, through researches on monomer ratio, reaction PH value, reaction temperature, initiator addition and reaction time, various parameters in the preparation of the retarder are accurately controlled, and the prepared retarder can play a role in prolonging thickening time of cement paste and simultaneously does not influence water loss of the cement paste.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, it should be noted that any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A retarder with a water loss reducing function is characterized in that: the catalyst comprises AMPS, AA and an initiator, wherein the monomer molar ratio of AMPS to AA is (30-80): (20-70); the initiator is redox initiator, the initiator is redox protogen of ammonium persulfate-sodium bisulfite, and the addition amount of the initiator is 0.5-2.5% of the mass of the monomer.
2. The retarder with water loss reducing function according to claim 1, wherein: the monomer molar ratio of AMPS to AA is 70: 30.
3. the retarder with water loss reducing function according to claim 1, wherein: the amount of initiator added is 1% of the mass of the monomers.
4. A preparation method of a retarder with a water loss reducing function is characterized by comprising the following steps:
step 1: weighing AMPS, and dissolving the AMPS in deionized water to enable the monomer concentration to be 25%; weighing AA and dissolving AA in deionized water to ensure that the monomer concentration is 25 percent;
step 2: mixing the AMPS and AA solutions prepared in the step 1, and then adjusting the pH value by using a sodium hydroxide solution with the concentration of 20%;
and step 3: adding the mixed solution obtained in the step 2 into a three-neck flask, uniformly mixing the solution through a stirrer, and removing oxygen from the solution;
and 4, step 4: after the oxygen removal step was completed, the three-necked flask was placed in a water bath to raise the temperature to 70 ℃, and then an initiator of 1% by mass of the monomer was added to the solution, and the temperature was maintained and the stirring was continued.
5. The preparation method of the retarder with water loss reducing function according to claim 4, wherein the retarder comprises: in the step 4, the stirring speed is 150-.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011070323A1 (en) * | 2009-12-08 | 2011-06-16 | Halliburton Energy Services, Inc. | A biodegradable set retarder for a cement composition |
| CN102351986A (en) * | 2011-07-28 | 2012-02-15 | 中国石油集团川庆钻探工程有限公司 | Method for preparing binary copolymer retarder for oil and gas well cementing |
| WO2015141667A1 (en) * | 2014-03-18 | 2015-09-24 | 株式会社日本触媒 | Cement composition and cement curing retarder |
| CN109503760A (en) * | 2017-09-14 | 2019-03-22 | 中石化石油工程技术服务有限公司 | A kind of high temperature oil well cement retarder, preparation method and application |
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- 2020-10-21 CN CN202011131414.XA patent/CN112250791A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011070323A1 (en) * | 2009-12-08 | 2011-06-16 | Halliburton Energy Services, Inc. | A biodegradable set retarder for a cement composition |
| CN102351986A (en) * | 2011-07-28 | 2012-02-15 | 中国石油集团川庆钻探工程有限公司 | Method for preparing binary copolymer retarder for oil and gas well cementing |
| WO2015141667A1 (en) * | 2014-03-18 | 2015-09-24 | 株式会社日本触媒 | Cement composition and cement curing retarder |
| CN109503760A (en) * | 2017-09-14 | 2019-03-22 | 中石化石油工程技术服务有限公司 | A kind of high temperature oil well cement retarder, preparation method and application |
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