CN113248665B - Sewage-resistant polymer for oil extraction and preparation method thereof - Google Patents
Sewage-resistant polymer for oil extraction 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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention relates to a sewage-resistant polymer for oil extraction and a preparation method thereof, which relate to the technical field of oil extraction and comprise components such as acrylamide, acrylic acid, grafted sulfonated starch, sulfonate, an initiator and the like. The polymer has the characteristics of temperature resistance, salt resistance, bacteria resistance, high viscosity retention rate and capability of preparing produced sewage by using an oil field, can keep good solubility and tackifying effect under the sewage condition, and can improve the petroleum recovery ratio in a higher range.
Description
Technical field:
the invention relates to the technical field of petroleum exploitation, in particular to a sewage-resistant polymer for oil extraction, and especially relates to a preparation method of the sewage-resistant polymer for oil extraction.
The background technology is as follows:
with the rapid development of the economy in China and the continuous progress of society, petroleum is an important industrial energy and chemical raw material, and the demand of the petroleum is growing at a daily and monthly speed. The stable supply of petroleum resources is indispensible to the stable development of social economy and the guarantee of the production life quality of people. And the oil field is taken as the most main unit of oil exploitation and gathering, and the quality of exploitation technology directly influences the yield and quality of oil.
Polymer flooding has achieved great success since the beginning of industrial popularization and application in 1996. Polymer flooding has become an important support for continuous stable production in large oil fields in China. Along with the gradual expansion of the tertiary oil recovery scale, a development object is changed from a first-class oil layer, a second-class oil layer, a third-class oil layer, the physical property of the oil layer is poor, the matching difficulty is increased, and the oil displacement effect is poor; meanwhile, in order to meet the environment-friendly requirement, sewage cannot be discharged, the preparation mode of part of polymer flooding blocks is changed from clear water preparation to clean water dilution (clear water preparation and sewage dilution), the dry powder consumption is greatly increased, and the recovery ratio is reduced by 1-3 percent compared with the clear water preparation. In order to explore the technology of reducing the dry powder consumption and further improving the recovery ratio under the condition of a polymer sewage system, and combining with the analysis of the actual situation of an oil field, the adoption of a novel sewage-resistant polymer is one of effective ways for solving the problem that the consumption of the polymer diluted by sewage is large.
The invention comprises the following steps:
the invention aims to provide a sewage-resistant polymer for oil extraction, which has the characteristics of temperature resistance, salt resistance, antibacterial property, high viscosity retention rate and capability of being prepared by using oilfield produced sewage, and can keep good solubility and tackifying effect under the sewage condition, so that the petroleum recovery rate is improved to a higher extent. The invention also provides a preparation method of the sewage-resistant polymer for oil extraction.
The invention is realized by the following technical scheme:
the sewage-resistant polymer for oil extraction is prepared from the following components in parts by weight:
as a further improvement of the invention, the sewage-resistant polymer for oil extraction is prepared from the following components in parts by weight:
as a further improvement of the invention, the No. 1 initiator is ammonium persulfate, potassium persulfate or sodium persulfate.
As a further improvement of the invention, the initiator # 2 is sodium bisulphite, sodium thiosulfate or triethanolamine.
As a further improvement of the invention, the 3# initiator is azobisisobutyronitrile, azobisisoheptonitrile or azobisisobutylamidine hydrochloride.
As a further improvement of the invention, the preparation method of the grafted sulfonated starch comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: the starch was prepared as 35% starch milk with distilled water. 100 parts of 35% starch milk are taken in a three-necked round bottom flask, the pH is adjusted to 8.0 by 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser pipe and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
As a further improvement of the invention, the starch is one or more than one of corn starch, tapioca starch, sweet potato starch, yam bean starch, soybean starch, pea starch and glutinous rice starch in any proportion.
As a further improvement of the present invention, the sulfonate has the structural formula:
wherein R is 4-8.
The preparation method of the sewage-resistant polymer for oil extraction comprises the following specific operation steps:
(1) Mixing acrylamide, acrylic acid, grafted sulfonated starch, sulfonate and water, stirring uniformly, and regulating the pH to 7-8 by using 10% sodium hydroxide solution;
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 8-10 ℃, introducing nitrogen for 30min to remove oxygen, adding a 1# initiator into the polymerization kettle, adding a 2# initiator after 5min, adding a 3# initiator after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cook for 2h after the reaction is completed until the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The beneficial effects of the invention are as follows: the polymer has the characteristics of temperature resistance, salt resistance, antibiosis, high viscosity retention rate and capability of being prepared by using oilfield produced sewage, can keep good solubility and tackifying effect under the sewage condition, and can improve the petroleum recovery ratio in a relatively high range.
The specific embodiment is as follows:
the present invention is further described in terms of the following examples, which are given by way of illustration only, and not by way of limitation, of the present invention, and any person skilled in the art may make any alterations or modifications to the equivalent examples using the teachings disclosed above. Any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention fall within the protection scope of the present invention.
Example 1
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) 100 parts of acrylamide, 10 parts of acrylic acid, 10 parts of sulfonate, 10 parts of grafted sulfonated starch and 300 parts of water are mixed and stirred uniformly, and the pH is regulated to 7.5 by 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 8 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.05 part of sodium persulfate into the polymerization kettle, adding 0.05 part of sodium bisulfite after 5min, adding 0.1 part of azobisisobutyronitrile after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed until the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 15 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: corn starch was prepared as 35% starch milk with distilled water. 100 parts of 35% starch milk is taken in a three-neck round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
Example 2
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) Mixing and stirring 120 parts of acrylamide, 10 parts of acrylic acid, 20 parts of sulfonate, 10 parts of grafted sulfonated starch and 350 parts of water uniformly, and regulating the pH to 7.5 by using a 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 8 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.1 part of potassium persulfate into the polymerization kettle, adding 0.1 part of triethanolamine after 5min, adding 0.2 part of azodiisobutylamidine hydrochloride after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed and the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 20 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: the soybean starch was prepared as 35% starch milk with distilled water. 100 parts of 35% starch milk is taken in a three-neck round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four:and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
Example 3
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) Mixing and stirring 120 parts of acrylamide, 10 parts of acrylic acid, 20 parts of sulfonate, 20 parts of grafted sulfonated starch and 400 parts of water uniformly, and adjusting the pH to 7.5 by using a 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 8 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.1 part of potassium persulfate into the polymerization kettle, adding 0.1 part of triethanolamine after 5min, adding 0.2 part of azodiisobutylamidine hydrochloride after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed and the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 20 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: the tapioca starch was prepared with distilled water to 35% starch milk. 100 parts of 35% starch milk is taken in a three-neck round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
Example 4
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) Mixing and stirring 150 parts of acrylamide, 20 parts of acrylic acid, 40 parts of sulfonate, 15 parts of grafted sulfonated starch and 500 parts of water uniformly, and regulating the pH to 7.5 by using 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 10 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.2 part of ammonium persulfate into the polymerization kettle, adding 0.2 part of sodium thiosulfate after 5min, adding 0.3 part of azodiisoheptonitrile after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed and the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 25 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: pea starch was prepared as 35% starch milk with distilled water. 100 parts of 35% starch milk is taken in a three-neck round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
Example 5
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) Mixing and stirring 150 parts of acrylamide, 20 parts of acrylic acid, 40 parts of sulfonate, 15 parts of grafted sulfonated starch and 500 parts of water uniformly, and regulating the pH to 7.5 by using 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 10 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.2 part of ammonium persulfate into the polymerization kettle, adding 0.2 part of sodium thiosulfate after 5min, adding 0.3 part of azodiisoheptonitrile after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed and the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 25 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: the glutinous rice starch was prepared into 35% starch milk with distilled water. 100 parts of 35% starch milk is taken in a three-neck round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: taking 50 parts of the intermediate obtained in the step three into a three-neck round-bottom flask, and respectively arranging an air duct and cold air ducts on the three-neck round-bottom flaskThe coagulation tube and the electric stirrer are arranged in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
Example 6
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) 200 parts of acrylamide, 10 parts of acrylic acid, 10 parts of sulfonate, 10 parts of grafted sulfonated starch and 500 parts of water are mixed and stirred uniformly, and the pH is regulated to 7.5 by 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 10 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.05 part of sodium persulfate into the polymerization kettle, adding 0.05 part of sodium bisulfite after 5min, adding 0.1 part of azobisisobutyronitrile after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed until the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 35 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: sweet potato, potato and yam bean starch (starch is a mixture of sweet potato and potato in the mass ratio of 1:1:1) are prepared into starch milk with distilled water in an amount of 35%. 100 parts of 35% starch milk are taken in a three-necked round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser pipe and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass.
Example 7
A sewage-resistant polymer for oil extraction and a preparation method thereof are provided:
(1) Mixing and stirring 130 parts of acrylamide, 10 parts of acrylic acid, 10 parts of sulfonate, 20 parts of grafted sulfonated starch and 400 parts of water uniformly, and adjusting the pH to 7.5 by using a 10% sodium hydroxide solution;
wherein, the structure of the sulfonate is as follows:
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 8 ℃, introducing nitrogen for 30min to remove oxygen, adding 0.05 part of ammonium persulfate into the polymerization kettle, adding 0.05 part of sodium thiosulfate after 5min, adding 0.1 part of azodiisoheptonitrile after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed until the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding 20 parts of solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
The preparation method of the grafted sulfonated starch in the step (1) comprises the following steps:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water, the distilled water is added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath. 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that the esterification agent is obtained, wherein the mass fractions are.
Step two: and (3) regulating the PH of the esterifying agent obtained in the step (I) to 8.0 by using 10% sodium hydroxide for later use.
Step three: the tapioca starch was prepared with distilled water to 35% starch milk. 100 parts of 35% starch milk is taken in a three-neck round-bottomed flask, the pH is adjusted to 8.0 with 10% sodium hydroxide, and alkalization is carried out for 20min. And (3) respectively mounting a constant-pressure funnel, a condenser and an electric stirrer on the three-neck round-bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on the starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process. After the end of the ultrasound, the reaction was continued for 6h at 35 ℃. After the reaction, the pH of the emulsion was adjusted to 6.5 with 1mol/L hydrochloric acid solution to give an intermediate for use. The above components are all in parts by mass.
Step four: and (3) taking 50 parts of the intermediate obtained in the step (III) in a three-neck round-bottom flask, respectively arranging an air duct, a condenser and an electric stirrer on the three-neck round-bottom flask, and placing the whole device in a water bath. The temperature was controlled at 48℃and nitrogen was introduced under stirring, after 30 minutes of holding, 0.07 part of sodium persulfate was added, after 10 minutes, 3.5 parts of acrylic acid was added, the reaction was continued for 120 minutes, and the mixture was cooled to room temperature. Adding ethanol to precipitate, separating, vacuum filtering, washing filter cake with distilled water and ethanol, and repeating
And (3) repeating the steps, combining the precipitates, drying, crushing and sieving to obtain grafted sulfonated starch. The above components are all in parts by mass. The following is a description of the performance evaluation of the oil recovery sewage-resistant polymer of the present invention
Seven types of sewage-resistant polymers for oil extraction prepared by the formula have the characteristics of temperature resistance, salt resistance, high viscosity retention rate and capability of being prepared by using oilfield produced sewage, and can keep good solubility and tackifying effect under the conditions of high temperature and high mineralization, so that the petroleum recovery rate is improved greatly. Six types of sewage-resistant polymers for oil recovery are tested in terms of salt resistance, viscosity stability, molecular weight, oil displacement performance and the like:
1. evaluation of salt resistance
The salt resistance of the sewage-resistant polymer for oil recovery example 1, example 2, example 3, example 4, example 5, example 6, example 7 and the common polymer were compared. The common polymer is conventional polyacrylamide with molecular weight of 1600 ten thousand, the concentration of the polymer is 1000mg/L, the detection temperature is 45 ℃, a Brookfield viscometer is used for detecting the viscosity of aqueous solutions under the condition of sodium chloride with different concentrations, and the viscosity of the aqueous solutions is shown in the following table I:
table-viscosity of aqueous solutions under the conditions of different concentrations of sodium chloride
| NaCl concentration (mg/L) | 1000 | 5000 | 10000 | 15000 | 20000 |
| Example 1 viscosity (mpa.s) | 119.7 | 115.4 | 109.8 | 106.8 | 103.7 |
| Example 2 viscosity (mpa.s) | 120.1 | 115.7 | 109.3 | 108.1 | 105.2 |
| Example 3 viscosity (mpa.s) | 116.3 | 111.9 | 105.4 | 104.6 | 101.8 |
| Example 4 viscosity (mpa.s) | 112.6 | 108.1 | 102.0 | 100.3 | 97.6 |
| Example 5 viscosity (mpa.s) | 111.9 | 107.3 | 101.6 | 99.8 | 97.1 |
| Example 6 viscosity (mpa.s) | 111.5 | 107.4 | 101.7 | 98.5 | 96.9 |
| Example 6 viscosity (mpa.s) | 118.3 | 115.6 | 110.8 | 108.3 | 104.7 |
| Ordinary Polymer viscosity (mpa.s) | 47.2 | 20.5 | 11.3 | 2.6 | 0 |
The products obtained in each example have higher viscosity under the condition of sodium chloride with different concentrations, and the viscosity of the common polymer is greatly reduced, which proves that the invention has salt resistance.
2. Viscosity stability
The polymer was prepared and diluted to 1000mg/L with field sewage from a Daqing oil production plant, and the viscosity after standing for 0d, 3d, 15d, 30d, 60d, 90d at 45℃under anaerobic conditions was measured with a Brookfield viscometer. Wherein the common polymer is conventional polyacrylamide with a molecular weight of 1600 ten thousand. The test results are shown in Table II below:
table II viscosity after various times of standing
| Days (days) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Polymers in general |
| 0d | 66.8 | 78.1 | 74.6 | 70.3 | 69.8 | 68.5 | 75.2 | 11.9 |
| 3d | 65.3 | 76.4 | 73.4 | 69.5 | 68.6 | 67.4 | 73.6 | 4.3 |
| 7d | 63.1 | 74.5 | 72.6 | 67.9 | 67.4 | 65.8 | 71.2 | 0 |
| 15d | 71.9 | 81.6 | 80.3 | 75.6 | 75.6 | 73.9 | 75.8 | / |
| 30d | 79.6 | 87.4 | 87.7 | 83.8 | 83.7 | 81.0 | 85.6 | / |
| 60d | 86.4 | 95.1 | 94.8 | 90.5 | 91.3 | 89.8 | 90.3 | / |
| 90d | 86.8 | 95.5 | 92.9 | 91.2 | 90.2 | 90.0 | 95.4 | / |
| Viscosity retention | 129.9％ | 122.3％ | 124.5％ | 129.7％ | 129.2％ | 131.4％ | 126.9％ | / |
As can be seen from the data in the table, the average value of the viscosity retention rate of the oil recovery sewage-resistant polymer examples 1 to 7 provided by the invention exceeds 120% after being placed for 90 days at 45 ℃ under the anaerobic condition, and the average value of the viscosity retention rate of the oil recovery sewage-resistant polymer is 0, so that the oil recovery sewage-resistant polymer provided by the invention has excellent stability.
3. Molecular weight
Six types of sewage-resistant polymers for oil extraction were tested for molecular weight by using a Ubbelohde viscometer, and the molecular weight distribution is shown in the following Table III:
table three molecular weight distribution
| Temperature-resistant and salt-resistant polymer | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 6 |
| Molecular weight (. Times.10) 4 ) | 1753 | 1987 | 2257 | 1921 | 1340 | 2042 | 2524 |
As can be seen from the data in the table, the molecular weight distribution range of the sewage-resistant polymer for oil extraction example 1-7 is 1200-2500 ten thousand, and the distribution range is wide.
4. Oil displacement performance
The oil displacement scheme is as follows: the artificial rock core is 30-4.5 cm, and the water is driven to 98% of water content, and is converted into polymer, and the water is driven to 98% of water content subsequently. The displacement speed was 0.5ml/min, and the chemical flooding injection amount was 0.5pv.
Polymer flooding: the products obtained in examples 1 to 7 and the usual polymer concentration were 1000mg/L. Wherein the common polymer is conventional polyacrylamide with molecular weight of 1600 ten thousand. The recovery is shown in table four below:
table four recovery results
From Table IV, the average recovery of the polymer of the present invention is 18% higher, whereas the average polymer is about 11% higher, indicating that the present invention can be more improved than the average polymer.
Claims (8)
1. A sewage resistant polymer for oil recovery, which is characterized in that: the composite material is prepared from the following components in parts by mass:
the sulfonated starch is grafted sulfonated starch grafted with acrylic acid;
the sulfonate has the following structural formula:
wherein R is 4-8.
2. The wastewater resistant polymer for oil recovery according to claim 1, wherein: the composite material is prepared from the following components in parts by mass:
3. the sewage resistant polymer for oil recovery according to claim 1 or 2, wherein the initiator # 1 is ammonium persulfate, potassium persulfate or sodium persulfate.
4. The polymer as claimed in claim 1 or 2, wherein the initiator # 2 is sodium bisulphite, sodium thiosulfate or triethanolamine.
5. The polymer as claimed in claim 1 or 2, wherein the initiator 3# is azobisisobutyronitrile, azobisisoheptonitrile or azobisisobutylamino hydrochloride.
6. The sewage resistant polymer for oil recovery according to claim 1 or 2, wherein the preparation method of the grafted sulfonated starch is as follows:
step one: 44.72 parts of sodium bisulphite is dissolved in 200 parts of distilled water and added into a three-neck round-bottom flask, a constant-pressure funnel, a condenser tube and an electric stirrer are respectively arranged on the three-neck round-bottom flask, and the whole device is placed in a water bath; 3.45 parts of sodium nitrite solution with the mass fraction of 20% is filled into a constant pressure funnel, under the stirring condition, the sodium nitrite solution with the mass fraction of 20% is dropwise added into a three-neck flask at a constant speed within 20min, the temperature is controlled at 90 ℃, and the reaction is continued for 70min, so that an esterifying agent is obtained, wherein the mass fractions are the same;
step two: regulating the PH of the esterifying agent obtained in the step one to 8.0 by using 10% sodium hydroxide for standby;
step three: preparing starch into 35% starch milk by using distilled water; 100 parts of 35% starch milk is taken in a three-neck round bottom flask, 10% sodium hydroxide is used for adjusting the PH value to 8.0, and alkalization is carried out for 20min; respectively mounting a constant-pressure funnel, a condenser pipe and an electric stirrer on the three-neck round bottom flask, mounting 2 parts of the esterifying agent obtained in the second step in the constant-pressure funnel, placing the three-neck flask under the ultrasonic condition of 500W, carrying out ultrasonic treatment on starch milk for 60min, and dripping the esterifying agent into the starch milk at a constant speed in the ultrasonic treatment process; after the ultrasonic treatment is finished, continuously reacting for 6 hours at the temperature of 35 ℃; after the reaction is finished, the PH of the emulsion is regulated to 6.5 by using 1mol/L hydrochloric acid solution to obtain an intermediate for later use; the components are all in parts by weight;
step four: taking 50 parts of the intermediate obtained in the step three, putting the intermediate into a three-neck round-bottom flask, respectively arranging an air duct, a condenser pipe and an electric stirrer on the three-neck round-bottom flask, and putting the whole device into a water bath; controlling the temperature at 48 ℃, introducing nitrogen under stirring, maintaining for 30min, adding 0.07 part of sodium persulfate, adding 3.5 parts of acrylic acid after 10min, continuing to react for 120min, and cooling to room temperature; adding ethanol to separate the precipitate, carrying out suction filtration, washing a filter cake with distilled water and ethanol, repeating for 4-6 times, combining the precipitate, drying, crushing and sieving to obtain grafted sulfonated starch; the above components are all in parts by mass.
7. The sewage resistant polymer for oil recovery according to claim 6, wherein the starch is one or more of corn starch, tapioca starch, sweet potato starch, yam bean starch, soybean starch, pea starch and glutinous rice starch.
8. The preparation method of the sewage-resistant polymer for oil recovery according to claim 1 or 2 comprises the following specific operation steps:
(1) Mixing acrylamide, acrylic acid, grafted sulfonated starch, sulfonate and water, stirring uniformly, and regulating the pH to 7-8 by using 10% sodium hydroxide solution;
(2) Transferring the solution prepared in the step (1) to an adiabatic polymerization kettle after the temperature is regulated to 8-10 ℃, introducing nitrogen for 30min to remove oxygen, adding a 1# initiator into the polymerization kettle, adding a 2# initiator after 5min, adding a 3# initiator after 5min, stopping introducing nitrogen after the temperature of the system in the kettle is raised, and continuing to cure for 2h after the reaction is completed until the temperature is not raised any more to obtain polymer colloid;
(3) Crushing the polymer colloid obtained in the step (2), adding solid sodium hydroxide, fully mixing, hydrolyzing for 6 hours at the temperature of 80 ℃, drying for 12 hours at the temperature of 45 ℃, crushing, and screening to obtain particles with the particle size of 200-1000 mu m, thus obtaining a finished product.
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