CN110078865B - High-temperature-resistant foaming agent and preparation method thereof - Google Patents
High-temperature-resistant foaming agent and preparation method thereof Download PDFInfo
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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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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/92—Compositions for stimulating production by acting on the underground formation characterised by their form or by the form of their components, e.g. encapsulated material
- C09K8/94—Foams
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Abstract
A high temperature resistant foaming agent and a preparation method thereof relate to the technical field of tertiary oil recovery in oil fields. The high-temperature resistant foaming agent is generated by copolymerization reaction of 6-acrylamidocaproic acid, sodium methyl propylene sulfonate and 1-acryloyloxy-2-pyrrolidone. The preparation method of the high-temperature resistant foaming agent comprises the following steps: adding sodium methallyl sulfonate and an initiator persulfate into a flask, stirring by magnetic force, mixing 6-acrylamidocaproic acid and 1-acryloyloxy-2-pyrrolidone, and adding into a drip pump; and (3) after the temperature is raised to 30 ℃, injecting a mixture of 6-acrylamidocaproic acid and 1-acryloyloxy-2-pyrrolidone into a flask, raising the temperature to 70 ℃, keeping the temperature, adding a quinone polymerization inhibitor to terminate the polymerization reaction, continuing for 20-60 min, cooling to room temperature, separating and purifying to obtain the high-temperature resistant foaming agent. Can improve the recovery ratio of the oil field in the environment of hot water, steam and high-temperature flue gas.
Description
Technical Field
The invention relates to the technical field of tertiary oil recovery in oil fields, in particular to a high-temperature-resistant foaming agent capable of improving the recovery ratio of an oil field in hot water, steam and high-temperature flue gas environments and a preparation method thereof.
Technical Field
Modern industry is rapidly developing, energy consumption is continuously increasing, and oil, one of main energy sources, is exploited in the later stage of development. In order to recover more mineral oil and improve the recovery ratio of the oil, the research of tertiary oil recovery technology is very important. At present, a large amount of manpower and material resources are invested in China to carry out relevant research on tertiary oil recovery technology, and in oil fields in China, because of high thick oil proportion, the application of thermal oil recovery technology in tertiary oil recovery, such as steam flooding, steam huff and puff, high-temperature flue gas flooding and the like, is increasingly wide.
Because steam, flue gas and other hot fluids have low density and strong fluidity, the gas channeling phenomenon of the steam, the flue gas and other hot fluids in the gaps of the stratum is serious, the loss ratio is large, and the application of steam flooding and flue gas flooding is limited. The foaming agent is used as an important technical means for tertiary oil recovery, can form foam in formation gaps, effectively blocks an oil-free area with high formation permeability, forces steam and flue gas to directly act on an oil reservoir, increases the swept area of the steam and the flue gas, and improves recovery. The foaming agent is simultaneously used as a surfactant, and has low oil/water phase interfacial tension and certain oil washing capacity. Although the foaming agent is widely applied to oil field development as a general technology, in the field of thermal oil recovery, the general foaming agent cannot meet the technical requirement because the foaming agent needs to resist the high temperature of 300 ℃ and maintain good foaming performance.
In order to avoid flue gas pollution and simultaneously realize secondary utilization of flue gas, the method for improving the recovery rate by directly injecting the flue gas of the boiler in the oil field as hot fluid into a reservoir is remarkably developed. The high-temperature flue gas is adopted as the hot fluid, so that the heat efficiency can be obviously improved, for example, the average heat efficiency of a steam injection boiler in a victory oil field is 85 percent, wherein the exhaust gas temperature is 240 ℃, the heat loss is 9.8 percent, if the generated steam and the flue gas are injected into an oil layer together, no flue gas is discharged, and the heat efficiency is improved to 95 to 99 percent. In addition, the emission of carbon dioxide can be reduced, and the current trend of emission reduction and environmental protection is met. The main components of the high-temperature flue gas are nitrogen, carbon dioxide, oxygen and high-temperature water vapor, but the foaming capacity of the common foaming agent applied to the oil field at present is greatly influenced by temperature, oxygen and carbon dioxide, so that the foaming performance is greatly reduced, the plugging and profile control effects of an ideal foam liquid film cannot be achieved, and the recovery ratio is not obviously improved.
Therefore, the high-temperature-resistant foaming agent has wide prospect, is applied to the technical field of thermal oil recovery of oil fields, and can improve the oil field recovery ratio in the environments of hot water, steam and high-temperature flue gas.
Chinese patent CN201010260748.7 discloses a foaming agent composition and application thereof, mainly solving the problems that the foaming agent in the existing foam flooding enhanced oil recovery technology has poor thermal stability, precipitates when meeting divalent ions and cannot meet the requirements of foam flooding of high-temperature and high-salinity stratum.
Chinese patent application CN201711219887.3 discloses a high temperature resistant foaming agent for assisting steam flooding, which comprises the following components in parts by weight: 5-10 parts of foaming agent, 10-30 parts of foam stabilizer and 60-85 parts of water; the foaming agent is polyether sulfonate containing imino. The foaming agent is high temperature resistant, but the foaming performance under the conditions of carbon dioxide, oxygen and the like is not seen.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant foaming agent which is applied to the field of tertiary oil recovery in oil fields, can keep excellent foaming performance under the conditions of high temperature, carbon dioxide, oxygen and the like, and can resist the complex environment of high-temperature flue gas.
The invention also aims to provide a preparation method of the high-temperature-resistant foaming agent.
The high-temperature resistant foaming agent is generated by copolymerization reaction of 6-acrylamidocaproic acid, sodium methyl acrylate sulfonate and 1-acryloyloxy-2-pyrrolidone.
The molecular structural formula of the high-temperature-resistant foaming agent is as follows:
wherein x, y and z represent polymerization degree, x is 200-500, y is 100-300 and z is 100-400.
The mass ratio of the 6-acrylamidohexanoic acid to the sodium methallyl sulfonate to the 1-acryloyloxy-2-pyrrolidone is (40-60): 10-20): 20-50.
The molecular weight of the copolymer obtained by the copolymerization reaction is 4 × 104～10×104。
When in use, the high-temperature resistant foaming agent is prepared into an aqueous solution, and the mass concentration of the aqueous solution is 20-60%.
The preparation method of the high-temperature-resistant foaming agent comprises the following steps:
1) adding sodium methallyl sulfonate and an initiator persulfate into a flask, turning on a magnetic stirrer to heat a stirring switch, and simultaneously mixing 6-acrylamidocaproic acid and 1-acryloyloxy-2-pyrrolidone in advance and adding the mixture into a drip pump;
2) after the temperature rises to 30-50 ℃, opening a dropping liquid pump switch to inject the mixture of the 6-acrylamido caproic acid and the 1-acryloyloxy-2-pyrrolidone into the flask for 10-50 min;
3) and after the injection is finished, raising the temperature to 60-80 ℃, keeping the temperature for 1-3 h, adding 0.05-0.2% of quinone polymerization inhibitor to terminate the polymerization reaction, continuing for 20-60 min, cooling to room temperature, separating and purifying to obtain the high-temperature-resistant foaming agent.
The quinone polymerization inhibitor can be one of p-benzoquinone, tetrachlorobenzoquinone, naphthoquinone and the like.
The high-temperature resistant foaming agent prepared by the invention is compounded with water to obtain an aqueous solution, and the aqueous solution can be applied to tertiary oil recovery. The mass percentage concentration of the aqueous solution can be 0.1-5%.
Under the conditions of high temperature, carbon dioxide, oxygen and the like, the performance stability of the common foaming agent is poor, and the foaming agent prepared by the invention can still keep excellent foaming performance and can resist the complex environment of high-temperature flue gas.
Compared with the prior art, the high-temperature-resistant foaming agent for tertiary oil recovery has the following outstanding advantages:
1) the carboxyl with low cost and easy acquisition is adopted as the active and hydrophilic groups, so that the foaming agent is ensured to have good foaming performance (the foaming volume at 50 ℃ under normal pressure is more than 500ml) and low interfacial activity tension (the interfacial tension with Shengli crude oil can reach 10)- 3mN/m)；
2) The sodium methallyl sulfonate can play a good role in stabilizing foam, and effectively improve the stability and temperature resistance of the foam;
3) the 6-acrylamidohexanoic acid and the sodium methallyl sulfonate are both strong hydrophilic structures, and pyrrolidone structures which are easy to obtain, moderate in polarity and strong in thermal stability are additionally added to adjust the polarity and the spatial structure;
4) the polymerization reaction of the three monomers of 6-acrylamidohexanoic acid, sodium methallyl sulfonate and 1-acryloyloxy-2-pyrrolidone is easy to occur, the reaction condition is mild, and the reaction process is easy to controlAnd containing a stable long-chain alkyl radical- (CH)2-CH2)nThe structure ensures that the foaming agent has outstanding advantages in temperature resistance and better stability (the half-life period can reach 140 min);
5) the main functional groups of the three monomers are difficult to generate chemical reaction with carbon dioxide and oxygen, and can maintain stable foam performance in a high-temperature flue gas environment.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1: testing of temperature resistance of foaming agent
1.5g of sodium methallyl sulfonate is prepared into a solution and poured into a four-neck flask, the four-neck flask is fixed on an iron support, the distance between the flask and a constant-temperature magnetic stirrer is noticed, the bottom of the flask is ensured to just contact the bottom of an oil bath pot, a spherical condenser pipe is connected, and a condensate switch is turned on. 5g of 6-acrylamidocaproic acid and 3.5g of 1-acryloyloxy-2-pyrrolidone are dissolved in water to prepare a solution, the solution is transferred to a dropping pump, and the rate of the dropping pump is adjusted for standby. 0.4g K2S2O8Preparing a solution, adding the solution into a flask containing a sodium methallyl sulfonate solution, opening a dropping pump switch containing a mixed solution of 6-acrylamidocaproic acid and 1-allenyloxy-2-pyrrolidone when a magnetic stirrer is heated to 30 ℃, dropwise adding the mixed solution into the flask containing the sodium methallyl sulfonate solution for 30min, continuously reacting at 70 ℃ for 2h after dropwise adding, adding 0.1g of p-benzoquinone, continuously preserving heat for 40min, cooling, separating and purifying to obtain a finished foam agent.
Preparing a foaming agent into a solution with the mass concentration of 0.4%, dividing the solution into three parts, testing the foaming performance of one part in a foaming instrument at the temperature of 50 ℃ under normal pressure, testing the foaming performance of the other part at the temperature of 300 ℃, aging the other part in a high-temperature high-pressure reaction kettle at the temperature of 300 ℃ for 72 hours, and then testing the foaming performance in the foaming instrument. The test results are shown in table 1.
Example 2: testing of temperature resistance of foaming agent
1.75g of sodium methallyl sulfonate prepared into a solution is poured into the containerIn the mouth flask, fix four-mouth flask on the iron stand platform, notice flask and constant temperature magnetic stirrers's distance, guarantee that the flask bottom just contacts oil bath bottom of a boiler portion, connect spherical condenser pipe, open the condensate switch. 5.5g of 6-acrylamidocaproic acid and 4g of 1-acryloyloxy-2-pyrrolidone were dissolved in water to prepare a solution, which was transferred to a dropping pump, and the rate of the dropping pump was adjusted for use. 0.4g K2S2O8Preparing a solution, adding the solution into a flask containing a sodium methallyl sulfonate solution, opening a dropping pump switch containing a mixed solution of 6-acrylamidocaproic acid and 1-acryloyloxy-2-pyrrolidone when a magnetic stirrer is heated to 30 ℃, dropwise adding the mixed solution into the flask containing the sodium methallyl sulfonate solution for 30min, continuously reacting for 2h at 70 ℃ after dropwise adding is finished, adding 0.1g of p-benzoquinone, continuously preserving heat for 40min, cooling, separating and purifying to obtain a finished foam agent.
Preparing a foaming agent into a solution with the mass concentration of 0.4%, dividing the solution into 3 parts, testing the foaming performance of 1 part in a foaming instrument at 50 ℃ and normal pressure, testing the foaming performance of 1 part at 300 ℃ and high pressure, placing 1 part in a high-temperature high-pressure reaction kettle, carrying out aging treatment at 300 ℃ for 72 hours, and then testing the foaming performance in the foaming instrument. The results of the foam temperature resistance test are shown in table 1:
TABLE 1
As can be seen from Table 1, after the foaming agent synthesized by using different monomer mass ratios is aged for 72 hours at 300 ℃, the foaming volume and half-life period of the foam are changed very little, the attenuation amplitude is controlled within 5%, the foaming agent can resist the high temperature of 300 ℃, the foaming volume and half-life period are not changed very much in the high-pressure environment of 300 ℃, and the high-temperature resistance of the foaming agent is good.
Example 3: foaming agent CO resistance2Testing
A synthetic foaming agent was prepared in the same manner as in example 1, tetrachlorobenzoquinone was used as the quinone polymerization inhibitor, and the foaming agent was prepared as a 0.4% solution by mass concentration and divided into twoOne part was subjected to a foam performance test in a foam tester at 50 ℃ under normal pressure, and the other part was additionally charged with 100% volume fraction CO under the same temperature and pressure2The gas was subjected to foam performance testing. The test results are shown in table 2.
Example 4: foaming agent CO resistance2Testing
A synthetic foaming agent was prepared as in example 2, naphthoquinone was used as the quinone type polymerization inhibitor, the foaming agent was prepared as a 0.4% solution by mass, divided into two portions, one portion was subjected to a foam performance test in a foam instrument at 50 ℃ under normal pressure, and the other portion was additionally charged with 100% by volume of CO at the same temperature and pressure2The gas was subjected to foam performance testing. Foaming agent CO resistance2The results of the sexual tests are shown in table 2:
TABLE 2
As can be seen from Table 2, the foam compositions synthesized with different monomer mass ratios were additionally charged with 100% volume fraction CO2Later, the foam had little change in both lather volume and half-life, and was considered within normal error, indicating CO tolerance of the foam formulation2The performance is good.
Example 5: foaming agent O resistance2Testing
A synthetic foam was prepared as in example 1 by formulating the foam into a 0.4% strength by mass solution and dividing into two portions, one portion being tested for foam properties in a foam tester at 50 ℃ and atmospheric pressure and the other portion being additionally charged with 100% volume fraction of O at the same temperature and pressure2The gas was subjected to foam performance testing. The test results are shown in table 3.
Example 6: foaming agent O resistance2Testing
A synthetic foam was prepared as in example 2, by formulating the foam into a 0.4% strength by mass solution and dividing into two portions, one portion being tested for foam properties in a foam tester at 50 ℃ and atmospheric pressure, and the other portion being additionally charged with 100% volume fraction of O at the same temperature and pressure2Gas (es)Foam performance testing was performed. Foaming agent O resistance2The results of the sexual tests are shown in table 3:
TABLE 3
As can be seen from Table 3, the foam compositions synthesized with different monomer mass ratios were additionally charged with 100% volume fraction O2Thereafter, both the lather volume and half-life of the lather remained nearly constant, indicating that the lather was O resistant2The performance is good.
Experiments prove that the foaming agent prepared by the invention solves the problem that the current common foaming agent can not keep stable foaming performance in a high-temperature flue gas environment, and can effectively resist the high temperature of 300 ℃ and CO2And O2The foam material still keeps stable foam performance under the condition of high-temperature flue gas, has good plugging and profile control capacity, and improves the recovery ratio of crude oil.
Claims (6)
1. The high temperature resistant foaming agent is characterized in that 6-acrylamido caproic acid, sodium methyl propylene sulfonate and 1-acryloyloxy-2-pyrrolidone are subjected to copolymerization reaction to generate the high temperature resistant foaming agent.
2. The high temperature resistant foaming agent of claim 1, wherein the molecular structural formula of the high temperature resistant foaming agent is as follows:
wherein x, y and z represent polymerization degree, x is 200-500, y is 100-300 and z is 100-400.
3. The high-temperature-resistant foaming agent according to claim 1, wherein the mass ratio of the 6-acrylamidohexanoic acid, the sodium methallyl sulfonate and the 1-acryloyloxy-2-pyrrolidone is (40-60): 10-20): 20-50.
4. The high temperature resistant foamable composition of claim 1, wherein the copolymer obtained by said copolymerization has a molecular weight of 4 × 104～10×104。
5. The method for preparing the high-temperature-resistant foaming agent according to claim 1, characterized by comprising the following steps:
1) adding sodium methallyl sulfonate and an initiator persulfate into a flask, turning on a magnetic stirrer to heat a stirring switch, and simultaneously mixing 6-acrylamidocaproic acid and 1-acryloyloxy-2-pyrrolidone in advance and adding the mixture into a drip pump;
2) after the temperature rises to 30-50 ℃, opening a dropping liquid pump switch to inject the mixture of the 6-acrylamido caproic acid and the 1-acryloyloxy-2-pyrrolidone into the flask for 10-50 min;
3) and after the injection is finished, raising the temperature to 60-80 ℃, keeping the temperature for 1-3 h, adding 0.05-0.2% of quinone polymerization inhibitor to terminate the polymerization reaction, continuing for 20-60 min, cooling to room temperature, separating and purifying to obtain the high-temperature-resistant foaming agent.
6. The method of claim 5, wherein in step 3), the quinone type polymerization inhibitor is selected from one of p-benzoquinone, chloranil, and naphthoquinone.
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| CN102504788B (en) * | 2011-10-25 | 2013-10-30 | 中国石油天然气股份有限公司 | Foaming agent suitable for oil-field development |
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