CN112745454B - Thickener for high-temperature deep well acidification and preparation method thereof - Google Patents
Thickener for high-temperature deep well acidification and preparation method thereof Download PDFInfo
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- 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
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- C09K8/62—Compositions for forming crevices or fractures
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- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
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Abstract
The invention belongs to the technical field of oilfield chemical additives, relates to a thickening agent, and particularly relates to a thickening agent for acidification of a high-temperature deep well and a preparation method thereof. The preparation method of the thickener comprises the following steps: (1) mixing acrylamide and alkyl methyl diallyl ammonium chloride, dissolving in water, and stirring; (2) ventilating and deoxidizing the solution obtained in the step (1), and adding an initiator for reaction; (3) and (3) precipitating and drying the reactant obtained in the step (2) by using acetone to obtain the catalyst. The thickening agent has higher shear resistance, and the shear rate is 170s ‑1 Under the condition, the viscosity of the thickening acid system is as high as 42 mPa.s. In addition, the thickening agent can resist high temperature, the viscosity of a thickening acid system is still higher than 30 mPa.s at 160 ℃, and the use requirement under the condition of high-temperature deep well is met.
Description
Technical Field
The invention belongs to the technical field of oilfield chemical additives, relates to a thickening agent, and particularly relates to a thickening agent for acidification of a high-temperature deep well and a preparation method thereof.
Background
The main principle of acidification is that acid liquor is pumped into stratum to react with rock, so as to erode minerals and inorganic plugs in near-wellbore area, enlarge communication pores and recover and improve stratum permeability. In the process of acidification, the acid liquor reacts with formation rock more rapidly, and particularly in a high-temperature deep well, the acid liquor is easily consumed near a shaft, and the formation far away from the well cannot be sufficiently acidified. Therefore, the method delays the reaction speed of the acid rock, improves the effective penetration distance of the acid liquor, is one of the directions for further improving the acidification effect of the reservoir, and is particularly important for acidification of a high-temperature deep well.
A thickening acid (also called gelled acid) and its process are developed from abroad, and it is characterized by that a thickening agent is added in the conventional acid liquor to raise viscosity of acid liquid phase and delay H in the acid liquor + The mass transfer speed to the solid-liquid interface, thereby playing an acid liquor system with a deep retarded acidification effect. Compared with a common acid liquid system, the thickening acid system has higher viscosity, good retarding performance, filtration loss reduction, drag reduction performance and the like, and has small secondary damage to an acidified stratum, so that the acidification period of validity of the thickening acid is longer than that of a conventional acidification system. With the gradual increase of the development depth of oil and gas fields, the facing formation temperature is higher and higher, and a thickening acid system with a retarding effect is rapidly developed. The biopolymer thickening agent is generally only suitable for the condition of lower formation temperature (below 40 ℃) due to poor temperature resistance.
The performance of the viscosifying acid is determined by the viscosifying agent used, and the molecular weight and structure of the viscosifying agent affect the acid viscosity. The thickener forms a spatial network structure after being dissolved in an acid liquor system, so that the apparent viscosity of the system can be greatly improved, and the diffusion rate of hydrogen ions in active acid is effectively reduced, thereby delaying the reaction speed of the acid liquor and rocks, reducing the consumption rate of the acid liquor and effectively increasing the action distance of the acid liquor. Therefore, the key for improving the performance of the thickening acid system is to develop a thickening acid system with strong tackifying capability, good solubility, stable performance and good chemical compatibility.
The most studied and widely used synthetic polymers are still mainly based on acrylamide modification. Compared with natural polymer thickeners, the thickeners have obvious advantages in aspects of thickening, temperature resistance and shear resistance, bacterial sensitivity, formation damage and the like. The acid thickener synthesized at home and abroad is mainly obtained by copolymerizing acrylamide or dilute monomers and some monomers containing temperature-resistant and salt-resistant group structures. For example, the patent CN101864031A proposes a method for preparing a gelling agent for temperature-controlled variable viscosity acid, which uses an amphoteric copolymer obtained by copolymerizing acrylamide, 2-acrylamide-2-methylpropanesulfonate and methacryloyloxyethyl R-dimethyl ammonium chloride (R is an alkyl group of C1 to C32). The invention patent CN102993358A discloses an acid liquid thickener preparation process based on initiator control, which is obtained by copolymerizing acrylamide with AMPS, MA and AM. The invention patent CN102994070A uses polyvinyl, pyrrolidone and dihydric alcohol to carry out polymerization reaction to prepare the polymer acid thickener. The total performance of the thickeners can meet the use requirement, the viscosity is between 10 and 40 mPas, but in order to improve the system viscosity, the three substances are copolymerized usually, the production process is complex, and the raw material cost is high. In addition, there are some documents reporting thickeners used in acid pressure of crosslinking acids, such as patent nos. CN103805158A, CN104403658A, etc., and these polymer thickeners are generally higher in viscosity than ordinary crosslinking acids, but need to be used in combination with a metal crosslinking agent.
In general, acid viscosifiers have undergone a continuous progression from natural polymers to synthetic polymers, but due to the lack of breakthrough progress in raw material selection in recent years, acid viscosifiers have gradually become stable in category focusing on the improvement of the properties of existing products. At present, although the common thickening acid systems (natural polymers and other thickening acids) used at home and abroad have better acidification effect than a simple acid system, the comprehensive performance of the thickening agent can not meet the construction requirements of on-site increasingly strict engraving, and the thickening agent often has the defects of poor thickening property, temperature resistance, salt resistance, shear stability and the like, so that the development of the acid thickening agent with stronger temperature resistance and shear resistance is needed.
Disclosure of Invention
The invention mainly aims to overcome the defects of the prior art and provide a thickening agent and a preparation method thereof.
In order to realize the purpose, the invention adopts the following technical scheme:
an object of the present invention is to provide a compound having the following structural formula:
wherein R is alkyl, the number of carbon atoms is 8-18, preferably, the number of carbon atoms is 12-18; n is 100-500, preferably, n is 200-300; m is 10 to 50, preferably, m is 20 to 40.
The second object of the present invention is to provide the use of the above-mentioned compounds in the preparation of thickeners.
The third object of the invention is to provide a thickening agent, which comprises the compound shown as the formula I.
The fourth object of the present invention is to provide a method for preparing the above thickener, which comprises:
(1) mixing acrylamide and alkyl methyl diallyl ammonium chloride, dissolving in water, and stirring;
(2) ventilating and deoxidizing the solution in the step (1), and adding an initiator to react;
(3) and (3) precipitating and drying the reactant obtained in the step (2) by using acetone to obtain the catalyst.
The fifth object of the invention is to provide the use of the thickener in high temperature deep well acidification.
Compared with the prior art, the invention has the following beneficial effects:
the thickening agent of the invention is prepared from acrylamide and alkyl methylThe diallyl ammonium chloride is copolymerized under the condition of an initiator, has the characteristics of simple synthesis process, wide raw material source and the like, and is convenient for realizing large-scale production and application. The thickening agent has higher shear resistance, and the shear rate is 170s -1 Under the condition, the viscosity of the thickening acid system is as high as 42 mPas. In addition, the thickening agent can resist high temperature, the viscosity of a thickening acid system is still higher than 30mPa & s at 160 ℃, and the use requirement under the condition of high-temperature deep wells is met.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
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 exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise, and it should also be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the features, steps, operations and/or combinations thereof.
In view of the problems involved in the background art, the present invention provides, in a first aspect, a compound having a structural formula as shown below:
wherein R is alkyl, the number of carbon atoms is 8-18, preferably, the number of carbon atoms is 12-18; n is 100-500, preferably, n is 200-300; m is 10 to 50, preferably, m is 20 to 40.
In a second aspect of the invention, there is provided the use of a compound as hereinbefore described in the preparation of a thickener.
In a third aspect of the present invention, there is provided a thickener comprising a compound of formula I above.
The molecular structure of the compound of the formula I contains a five-membered ring structure, and the rigid structure can effectively improve the shear resistance of the thickening agent; two C ═ C in alkyl methyl diallyl ammonium chloride molecules are opened, one end of the alkyl methyl diallyl ammonium chloride is combined with acrylamide, and the other end of the alkyl methyl diallyl ammonium chloride generates intramolecular reaction to form a stable long-chain structure with good temperature resistance, so that the alkyl methyl diallyl ammonium chloride has good high-temperature resistance stability. The length of the R-group carbon chain is 8-18, and the compound shown in the formula I can be ensured to have a good tackifying effect and good solubility in the length range. If the number of carbon atoms of the R group is less than 8, the formed carbon chain is short and the thickening effect cannot be exerted; if the carbon number of the R group is more than 18, the solubility of the alkyl methyl diallyl ammonium chloride is poor, and meanwhile, the solubility of the formed product is low, so that effective tackifying cannot be realized.
In a fourth aspect of the present invention, there is provided a method for producing the thickener as described above, comprising:
(1) mixing acrylamide and alkyl methyl diallyl ammonium chloride, dissolving in water, and stirring;
(2) ventilating and deoxidizing the solution in the step (1), and adding an initiator to react;
(3) and (3) precipitating and drying the reactant obtained in the step (2) by using acetone to obtain the catalyst.
Further, in the step (1), acrylamide and alkyl methyl diallyl ammonium chloride are mixed according to the mass ratio of 1: 0.1-1. In the experimental process, the temperature resistance of the thickening agent is increased along with the increase of the concentration of the alkyl methyl diallyl ammonium chloride in the initial reaction liquid, when the mass ratio of the acrylamide to the alkyl methyl diallyl ammonium chloride is within the range of 1:0.1-1, the high temperature stability is good, and the viscosity of a thickening acid system can reach more than 30mPa & s under the high temperature condition of 160 ℃.
Further, the stirring speed in the step (1) is 100-200 rpm. The dissolving of reactants can be promoted in the rotating speed range, the uniformity of the obtained product is ensured, and the thickening effect of the product cannot be damaged due to overlarge shearing force. If the rotating speed is lower than 100 revolutions per minute, the reactants are slowly dissolved, and agglomeration and other phenomena occur, so that the uniformity of the product is influenced; rotation speeds above 200 rpm can cause shear damage to the product viscosity, affecting the final viscosity.
Further, nitrogen is introduced into the step (2) for 30-45 min.
Further, in the step (2), the initiator is any one of azobisisobutyronitrile, dibenzoyl peroxide and potassium persulfate; preferably, the initiator is potassium persulfate.
Further, the reaction temperature in the step (2) is 40-60 ℃, and the reaction time is 4-6 h; the drying time in the step (3) is 8-12 h. A higher reaction rate can be ensured in this temperature range. If the reaction temperature is lower than 40 ℃, the reaction yield is lower; the reaction temperature is higher than 60 ℃, and the effect of improving the reaction yield is not obvious.
In a fifth aspect of the invention, there is provided the use of a thickener as described above in high temperature deep well acidizing.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
Example 1
100g of acrylamide and 100g of dodecyl methyl diallyl ammonium chloride are respectively weighed and fully dissolved by 400ml of deionized water, and then the solution is added into a three-mouth reaction bottle which is arranged in a thermostatic water bath and is provided with an electromagnetic stirrer, and the stirring speed is 100 r/min. At 60 ℃, introducing N 2 After deoxygenation for 30min, 0.1g of potassium persulfate was added and the reaction was carried out for 4 h. After the reaction is finished, the reactant is precipitated by acetone and is dried for 10 hours in vacuum at the temperature of 40 ℃ to obtain a white solid sample for later use.
Example 2:
100g of acrylamide and 10g of cetylmethyldiallylammonium chloride were weighed out separately and charged with 400ml of deionized waterAfter dissolution, the solution was put into a three-necked reaction flask equipped with an electromagnetic stirrer in a constant temperature water bath and stirred at 100 rpm. Introducing N at 50 DEG C 2 After deoxygenation for 30min, 0.15g of potassium persulfate was added and the reaction was carried out for 4 h. After the reaction is finished, the reactant is precipitated by acetone and dried in vacuum for 8 hours at the temperature of 40 ℃ to obtain a white solid sample for later use.
Example 3:
100g of acrylamide and 50g of octadecyl methyl diallyl ammonium chloride were weighed, respectively, and after fully dissolving them in 400ml of deionized water, the solutions were put into a three-neck reaction flask equipped with an electromagnetic stirrer in a thermostatic water bath, and stirred at a speed of 100 rpm. Introducing N at 60 DEG C 2 After deoxygenation for 30min, 0.2g of potassium persulfate was added and the reaction was carried out for 4 h. After the reaction is finished, the reactant is precipitated by acetone and is dried for 10 hours in vacuum at the temperature of 40 ℃ to obtain a white solid sample for later use.
Example 4:
100g of acrylamide and 100g of dodecyl methyl diallyl ammonium chloride are respectively weighed, and after being fully dissolved by 400ml of deionized water, the solution is added into a three-port reaction bottle which is arranged in a thermostatic water bath and is provided with an electromagnetic stirrer, and the stirring speed is 200 r/min. At 40 ℃, introducing N 2 After deoxygenation for 30min, 0.1g of potassium persulfate was added and the reaction was carried out for 6 h. After the reaction is finished, the reactant is precipitated by acetone and is dried in vacuum at 40 ℃ for 12 hours to obtain a white solid sample for later use.
Comparative example 1:
100g of acrylamide and 100g of eicosyl methyldiallylammonium chloride are respectively weighed, and after being fully dissolved by 400ml of deionized water, the solution is added into a three-port reaction bottle which is arranged in a thermostatic water bath and is provided with an electromagnetic stirrer, and the stirring speed is 100 r/min. At 60 ℃, introducing N 2 After deoxygenation for 30min, 0.1g of potassium persulfate was added and the reaction was carried out for 4 h. After the reaction is finished, the reactant is precipitated by acetone and is dried for 10 hours in vacuum at the temperature of 40 ℃ to obtain a white solid sample for later use.
Comparative example 2:
100g of acrylamide and 120g of dodecylmethyldiallylammonium chloride were weighed out separately from each other, and 4 was usedAfter 00ml of deionized water was sufficiently dissolved, the solution was put into a three-necked reaction flask equipped with an electromagnetic stirrer in a constant temperature water bath and stirred at 100 rpm. Introducing N at 60 DEG C 2 After deoxygenation for 30min, 0.1g of potassium persulfate was added and the reaction was carried out for 4 h. After the reaction is finished, the reactant is precipitated by acetone and is dried for 10 hours in vacuum at the temperature of 40 ℃ to obtain a white solid sample for later use.
Comparative example 3:
conventional acidified thickeners cationic polymers dimethyldiallylammonium chloride (DMDAAC).
Test examples
The thickeners prepared in examples 1-4 and comparative examples 1-2, and thickener of comparative example 3 were mixed with acid solutions to produce corresponding thickened acid systems, respectively, each thickener being used at a concentration of 0.5%, acid solution being 15% HCl:
(1) high temperature resistance of each thickener
The experiment was carried out using a high temperature high pressure rheometer with a shear rate of 100s -1 The viscosity of each of the above gelled acid systems was measured at different temperatures, and the results are shown in table 1 below.
TABLE 1 viscosity of the synthesized thickeners at different temperatures
As can be seen from Table 1, in examples 1 to 4, the viscosity of each thickening acid system decreased with an increase in temperature, and the viscosity was 20 mPas or more at 160 ℃ and satisfied the use requirements. In contrast, the reaction product of comparative example 1, which used eicosylmethyl diallyl ammonium chloride, had poor solubility due to excessively high carbon chain length, and white insoluble substances appeared, which were not usable. Comparative example 2 used an excess of dodecylmethyldiallylammonium chloride, resulting in an insufficient reaction and a certain effect on performance. Comparative example 3 using the cationic polymer dimethyldiallylammonium chloride (DMDAAC), a conventional acidizing thickener, the viscosity decreased rapidly at high temperature and was only suitable for reservoir acidizing needs below 100 ℃.
(2) Shear resistance of each thickener
The experiment was carried out using a high temperature and high pressure rheometer, the experimental temperature being 100 ℃, and the viscosity of each of the above gelled acid systems under different shear forces was measured, and the results are shown in table 2 below.
TABLE 2 viscosity of the synthesized thickeners at different shear rates
As can be seen from the table, the viscosity of the thickening acid decreases with increasing shear rate, and examples 1-4 are at high shear rate (170 s) -1 ) Still has higher viscosity and better anti-shearing capability.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (3)
1. A thickener comprising a copolymer of the formula:
wherein R is alkyl, and the number of carbon atoms is 8-18; n is 200-300; m is 20 to 40;
the binary copolymer is prepared by the following steps:
(1) according to the formula of acrylamide: mixing alkyl methyl diallyl ammonium chloride in a mass ratio of 1:1, dissolving the mixture in water, and stirring at a rotation speed of 100-;
(2) introducing nitrogen into the solution in the step (1) for 30-45min to remove oxygen, adding an initiator of azobisisobutyronitrile or dibenzoyl peroxide or potassium persulfate to react, controlling the reaction temperature at 40-60 ℃ and the reaction time at 4-6 h;
(3) and (3) precipitating the reactant obtained in the step (2) by using acetone, and drying for 8-12h to obtain the product.
2. The thickener of claim 1, wherein the number of carbon atoms is from about 12 to about 18.
3. Use of the thickener of claim 1 in high temperature deep well acidizing.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103497288A (en) * | 2013-10-21 | 2014-01-08 | 西南石油大学 | AM/AA/HMDAAC/A-beta-CD copolymer and preparation method thereof |
| CN103819609A (en) * | 2014-03-05 | 2014-05-28 | 成都佰椿石油科技有限公司 | Low-friction-resistance high-temperature-resistant gelled acid and preparation method thereof |
| US9932517B1 (en) * | 2017-04-06 | 2018-04-03 | China University Of Petroleum (East China) | Polymer and preparation method thereof, and viscosified acid fluid |
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| CN103497288A (en) * | 2013-10-21 | 2014-01-08 | 西南石油大学 | AM/AA/HMDAAC/A-beta-CD copolymer and preparation method thereof |
| CN103819609A (en) * | 2014-03-05 | 2014-05-28 | 成都佰椿石油科技有限公司 | Low-friction-resistance high-temperature-resistant gelled acid and preparation method thereof |
| US9932517B1 (en) * | 2017-04-06 | 2018-04-03 | China University Of Petroleum (East China) | Polymer and preparation method thereof, and viscosified acid fluid |
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