CN110229654B - High-molecular surfactant type thick oil viscosity reducer and preparation method thereof - Google Patents
High-molecular surfactant type thick oil viscosity reducer 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
- C08F220/56—Acrylamide; Methacrylamide
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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
- C09K8/584—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 surfactants
Abstract
The invention discloses a high-molecular surfactant type thick oil viscosity reducer and a preparation method thereof, and mainly solves the problem that the viscosity reducing effect of the conventional thick oil viscosity reducer is poor. The preparation method comprises the steps of firstly reacting maleic anhydride with nonylphenol polyoxyethylene ether to obtain an intermediate product, and then reacting the intermediate product with a certain amount of acrylamide to prepare the high-molecular surfactant. The surfactant has the advantages of reliable preparation process, low cost, low use concentration and capability of remarkably reducing the viscosity of the thickened oil.
Description
Technical Field
The invention belongs to the field of oil field oil extraction auxiliaries, and particularly relates to a high-molecular surfactant type thick oil viscosity reducer and a preparation method thereof.
Background
With the continuous development of society, the consumption of fossil energy is also increasing. While the heavy oil resources account for the majority of the oil resources that have been explored. The thickened oil is the crude oil with viscosity of more than 100 mPas of the degassed crude oil at the oil layer temperature. The viscous oil contains more waxy substances, colloid substances, asphaltene substances and other substances, so that the viscosity of the viscous oil is higher than that of the conventional crude oil, the fluidity is poor, and the exploitation difficulty is high. In order to solve the series of problems, a large amount of researches on viscosity reduction of the thick oil are carried out at home and abroad, and certain achievements are obtained. These achievements have been continuously improved and perfected in field application for many years, and a relatively complete viscosity reduction technical system for thick oil has been gradually formed.
In the process of thick oil exploitation, the viscosity reduction methods commonly used at home and abroad at present comprise a heating method, a thin oil mixing method, thick oil catalytic modification viscosity reduction, chemical viscosity reduction and the like. In chemical viscosity reduction, the types of crude oil flow modifiers are more, and the research on the viscosity reducer at home and abroad is integrated, the flow modifier has sharp selectivity and adaptability to crude oil, often, a certain flow modifier only has a good viscosity reduction effect on one crude oil, but has a poor or even no effect on other crude oils, and the main reasons for the phenomenon are mainly caused by the fact that the crude oil components are relatively complex, the molecular structure of the viscosity reducer is different from the viscosity reduction mechanism, and the like, so the deep research on the action relationship between the molecular structure of the viscosity reducer and the crude oil components is very important. Due to the difference of the components and the compositions of the crude oil, the viscosity reducer is continuously improved and improved on the original structure, and a plurality of new types appear, so that the viscosity reducer can better adapt to the target crude oil and obtain better flow modification effect.
The surfactant can reduce the surface tension and the interfacial tension between oil and water and promote the emulsification and dispersion of crude oil, so that the surfactant has an important position in oil field chemicals, particularly has a wide application prospect as a viscosity reducer in the exploitation of thick oil, is particularly suitable for thick oil with large water content, and can be used for demulsifying a water-in-oil type emulsion with high viscosity or inverting the water-in-oil type emulsion with low viscosity by adding a small amount of surfactant into the thick oil with water content, thereby effectively reducing the viscosity of the thick oil.
Therefore, in the field of thickened oil recovery, a novel surfactant type thickened oil viscosity reducer which has the characteristics of high viscosity reduction rate, stable performance, high natural dehydration rate, good compatibility with formation water and the like on the basis of the traditional surfactant is urgently needed to be researched.
Disclosure of Invention
The invention aims to solve the technical problem that the viscosity reducing effect of the conventional thick oil viscosity reducer is poor, and provides a high-molecular surfactant type thick oil viscosity reducer and a preparation method thereof.
In order to solve the technical problems, the technical scheme of the invention provides a thick oil viscosity reducer, and the preparation raw materials of the viscosity reducer comprise the following components:
maleic anhydride, nonylphenol polyoxyethylene ether, acrylamide, deionized water, p-toluenesulfonic acid and potassium persulfate.
The synthesis principle of the macromolecular surfactant type viscosity reducer is as follows:
(1) synthesis of monoester intermediates
In a three-neck flask provided with a stirring device, a condensation reflux device and a thermometer, taking p-toluenesulfonic acid accounting for 3 percent of the total mass of reactants as a catalyst, and reacting maleic anhydride and nonylphenol polyoxyethylene ether at 100 ℃ for 3.5h to obtain a monoester intermediate, wherein the reaction chemical formula is as follows:
(2) preparation of the target product
And (2) reacting the monoester intermediate obtained in the step (1) with acrylamide and deionized water in a three-neck flask provided with a stirring device, a condensation reflux device and a thermometer in a nitrogen atmosphere at 40 ℃ for 7h by using potassium persulfate as a catalyst to obtain a viscous product, carrying out reduced pressure distillation on the obtained product, washing and precipitating the product in acetone for multiple times to remove unreacted monomers, and drying the purified product at 80 ℃ for 3h to obtain the high-molecular surfactant. The reaction formula is as follows:
the invention has the beneficial effects that:
(1) the invention provides a preparation method of a high-molecular surfactant type thick oil viscosity reducer, which has the advantages of relatively easy acquisition of raw materials, simple production flow and high yield.
(2) The high-molecular viscosity reducer provided by the invention is a water-soluble emulsification viscosity reducer, and is mixed with thick oil according to a certain mass ratio after being dissolved in water, so that the original water-in-oil type is converted into an oil-in-water type emulsion, the intermolecular friction force and the oil-water interfacial tension are reduced, the crude oil viscosity is effectively reduced, and the flowability of the crude oil is increased.
(3) The high-molecular viscosity reducer provided by the invention has the characteristics of relatively small dosage, high viscosity reduction rate and high natural dehydration rate, and is suitable for the exploitation application of thick oil.
Description of the attached tables
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the attached tables needed to be used in the description of the embodiments or the prior art will be briefly introduced below.
TABLE 1 viscosity reduction Effect of different examples on Tarim oil field thickened oil
TABLE 2 viscosity reduction Effect of the five viscosity reducers of examples with different concentrations on Tarim heavy oil
TABLE 3 viscosity reduction Effect of viscosity reducers of the same concentration on different thickened oils
Detailed Description
The first embodiment is as follows:
(1) synthesis of monoester intermediates
Adding maleic anhydride and nonylphenol polyoxyethylene ether into a three-neck flask with a stirring device, a condensation reflux device and a thermometer according to the mol ratio of 1:1, heating the reaction temperature to 100 ℃, adding p-toluenesulfonic acid accounting for 3% of the total mass of reactants as a catalyst, and carrying out magnetic stirring reaction for 3.5 hours to obtain an intermediate.
(2) Preparation of the target product
Adding the obtained intermediate and acrylamide into a three-neck flask according to the molar ratio of 1:1, adding a proper amount of deionized water, fully and uniformly stirring, adding potassium persulfate accounting for 5% of the total mass of reactants as an initiator, raising the reaction temperature to 45 ℃, introducing nitrogen for 20min, removing the air in the flask, and reacting for 7h in a nitrogen atmosphere to obtain a viscous product. And (3) carrying out reduced pressure distillation on the obtained product, washing and precipitating the product in acetone for multiple times to remove unreacted monomers, and then drying the purified product at 80 ℃ for 3h to obtain the high-molecular surfactant.
Preparing the prepared viscosity reducer into an aqueous solution with the concentration of 0.5 wt%, and mixing the aqueous solution of the viscosity reducer with Tarim thick oil in a ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The results are shown in Table 1.
Example two:
(1) synthesis of monoester intermediates
Adding maleic anhydride and nonylphenol polyoxyethylene ether into a three-neck flask with a stirring device, a condensation reflux device and a thermometer according to the mol ratio of 1:2, heating the reaction temperature to 100 ℃, adding p-toluenesulfonic acid accounting for 3% of the total mass of reactants as a catalyst, and carrying out magnetic stirring reaction for 3.5 hours to obtain an intermediate.
(2) Preparation of the target product
The specific preparation method is the same as the step (2) in the first example.
Preparing the prepared viscosity reducer into an aqueous solution with the concentration of 0.5 wt%, and mixing the aqueous solution of the viscosity reducer with Tarim thick oil in a ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The results are shown in Table 1.
Example three:
(1) synthesis of monoester intermediates
Adding maleic anhydride and nonylphenol polyoxyethylene ether into a three-neck flask with a stirring device, a condensation reflux device and a thermometer according to the mol ratio of 2:1, heating the reaction temperature to 100 ℃, adding p-toluenesulfonic acid accounting for 3% of the total mass of reactants as a catalyst, and carrying out magnetic stirring reaction for 3.5 hours to obtain an intermediate.
(2) Preparation of the target product
The specific preparation method is the same as the step (2) in the first example.
Preparing the prepared viscosity reducer into an aqueous solution with the concentration of 0.5 wt%, and mixing the aqueous solution of the viscosity reducer with Tarim thick oil in a ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The results are shown in Table 1.
Example four:
(1) synthesis of monoester intermediates
The specific preparation method is the same as the step (1) in the first example.
(2) Preparation of the target product
Adding the obtained intermediate and acrylamide into a three-neck flask according to the molar ratio of 1:4, adding a proper amount of deionized water, fully and uniformly stirring, adding potassium persulfate accounting for 5% of the total mass of reactants as an initiator, raising the reaction temperature to 45 ℃, introducing nitrogen for 20min, removing the air in the flask, and reacting for 7h in a nitrogen atmosphere to obtain a viscous product. And (3) carrying out reduced pressure distillation on the obtained product, washing and precipitating the product in acetone for multiple times to remove unreacted monomers, and then drying the purified product at 80 ℃ for 3h to obtain the high-molecular surfactant.
Preparing the prepared viscosity reducer into an aqueous solution with the concentration of 0.5 wt%, and mixing the aqueous solution of the viscosity reducer with Tarim thick oil in a ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The results are shown in Table 1.
Example five:
(1) synthesis of monoester intermediates
The specific preparation method is the same as the step (1) in the first example.
(2) Preparation of the target product
Adding the obtained intermediate and acrylamide into a three-neck flask according to the molar ratio of 1:8, adding a proper amount of deionized water, fully and uniformly stirring, adding potassium persulfate accounting for 5% of the total mass of reactants as an initiator, raising the reaction temperature to 45 ℃, introducing nitrogen for 20min, removing the air in the flask, and reacting for 7h in a nitrogen atmosphere to obtain a viscous product. And (3) carrying out reduced pressure distillation on the obtained product, washing and precipitating the product in acetone for multiple times to remove unreacted monomers, and then drying the purified product at 80 ℃ for 3h to obtain the high-molecular surfactant.
Preparing the prepared viscosity reducer into an aqueous solution with the concentration of 0.5 wt%, and mixing the aqueous solution of the viscosity reducer with Tarim thick oil in a ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The results are shown in Table 1.
Example six:
(1) synthesis of monoester intermediates
The specific preparation method is the same as the step (1) in the first example.
(2) Preparation of the target product
Adding the obtained intermediate and acrylamide into a three-neck flask according to the molar ratio of 1:10, adding a proper amount of deionized water, fully and uniformly stirring, adding potassium persulfate accounting for 5% of the total mass of reactants as an initiator, raising the reaction temperature to 45 ℃, introducing nitrogen for 20min, removing the air in the flask, and reacting for 7h in a nitrogen atmosphere to obtain a viscous product. And (3) carrying out reduced pressure distillation on the obtained product, washing and precipitating the product in acetone for multiple times to remove unreacted monomers, and then drying the purified product at 80 ℃ for 3h to obtain the high-molecular surfactant.
Preparing the prepared viscosity reducer into an aqueous solution with the concentration of 0.5 wt%, and mixing the aqueous solution of the viscosity reducer with Tarim thick oil in a ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The results are shown in Table 1.
TABLE 1 viscosity reduction Effect of different examples on Tarim oil field thickened oil
As can be seen from Table 1, the viscosity reducer prepared in the first to sixth examples is prepared into an aqueous solution with a concentration of 0.5 wt% at 50 ℃, and the viscosity reduction effect test is performed on thick oil in a Tarim oil field, and the product obtained in the fifth example has the best viscosity reduction effect, and the viscosity reduction rate can reach 92.7%, so that the best molar ratio of maleic anhydride to nonylphenol polyoxyethylene ether to acrylamide is 1:1: 8.
Example seven:
since the viscosity reducer prepared according to the fifth mixture ratio in the embodiment has the best viscosity reduction effect, the viscosity reducer is prepared into aqueous solutions with different concentrations to test the viscosity reduction effect of the same heavy oil, and then the aqueous solutions with the same concentration are used to test the viscosity reduction effect of different heavy oils. The method comprises the following steps:
(1) viscosity reduction effect test of example five viscosity reducers with different concentrations on same crude oil
The crude oil sample is thick oil in a Xinjiang Tarim oil field, the viscosity of the thick oil is 15814mPa.s when the viscosity reducer is not added under the condition of 50 ℃ by using a rheometer, the viscosity reducer prepared in the fifth embodiment is prepared into aqueous solutions with different concentrations, and then the aqueous solution of the viscosity reducer and the crude oil are mixed according to the weight ratio of 7: 3, mixing the oil and the water according to the mass ratio, uniformly stirring, keeping the temperature for 1.5 hours at 50 ℃, and finally measuring the viscosity of the mixture at 50 ℃ and calculating the viscosity reduction rate. The viscosity and viscosity reduction rate of crude oil after the viscosity reducer with different concentrations is added are shown in Table 2.
TABLE 2 viscosity reduction Effect of the five viscosity reducers of examples with different concentrations on Tarim heavy oil
As can be seen from Table 2, the viscosity reducer prepared in the fifth example has an obvious viscosity reduction effect on thick oil in Tarim oil field at 50 ℃. When the concentration of the viscosity reducer is 0.6 wt%, the viscosity reduction rate is 92.8%.
(2) Viscosity reduction effect test of example five viscosity reducers with same concentration on different crude oils
The product obtained in example five was used to prepare an aqueous solution with a mass fraction of 0.3%. The aqueous viscosity reducer solution was then mixed with various types of highly viscous crude oil at a ratio of 7: 3, stirring uniformly, keeping the temperature at 50 ℃ for 1.5 hours, and finally measuring the viscosity at 50 ℃, wherein the measurement results are shown in table 3.
TABLE 3 viscosity reduction Effect of viscosity reducers of the same concentration on different thickened oils
As can be seen from Table 3, the viscosity reducer obtained in the fifth embodiment of the invention has better viscosity reducing effect on different types of thickened oil.
In conclusion, the viscosity reducer obtained in the fifth embodiment of the invention is prepared into an aqueous solution at 50 ℃ according to a mass ratio of 0.5%, and the using effect is best. Moreover, the viscosity reducer of the invention has better viscosity reducing effect on different types of high-viscosity crude oil. The viscosity reducer prepared by the method has low cost and obvious viscosity reduction effect, and provides reference and reference for exploitation of thick oil.
Claims (3)
1. A high molecular surfactant type viscosity reducer for thick oil comprises the following main components: maleic anhydride, nonylphenol polyoxyethylene ether and acrylamide, and the preparation method of the viscosity reducer comprises the following steps:
mixing maleic anhydride and nonylphenol polyoxyethylene ether according to the proportion of 1:1, adding the mixture into a three-neck flask provided with a stirring device, a condensation reflux device and a thermometer, raising the reaction temperature to 100 ℃, adding p-toluenesulfonic acid with a certain mass ratio as a catalyst, and carrying out magnetic stirring reaction for 3.5 hours to obtain an intermediate A; the intermediate A and acrylamide are prepared according to the following weight ratio of 1: adding the mixture into a three-neck flask according to a molar ratio of 8-10, adding a proper amount of deionized water, fully and uniformly stirring, adding a certain weight percentage of potassium persulfate serving as an initiator, raising the reaction temperature to 45 ℃, introducing nitrogen for 20min, removing air in the flask, reacting for 7h under the nitrogen atmosphere to obtain a viscous product, washing and precipitating the viscous product for multiple times by using acetone to remove unreacted monomers, and drying the purified product at 80 ℃ for 3h to obtain the high-molecular surfactant.
2. The viscosity reducer of thickened oil of high molecular surfactant type according to claim 1, characterized in that in the reaction of maleic anhydride and nonylphenol polyoxyethylene ether, the weight percentage of the added catalyst in the total mass of the reaction raw materials is 3%.
3. The high molecular surfactant type viscosity reducer for thick oil according to claim 1, wherein in the reaction of the intermediate A and acrylamide, the added initiator accounts for 5% by weight of the total mass of the reaction raw materials.
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