CN112521927A - Preparation method and application of oil film volume expanding agent - Google Patents
Preparation method and application of oil film volume expanding agent Download PDFInfo
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- CN112521927A CN112521927A CN202011480332.6A CN202011480332A CN112521927A CN 112521927 A CN112521927 A CN 112521927A CN 202011480332 A CN202011480332 A CN 202011480332A CN 112521927 A CN112521927 A CN 112521927A
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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
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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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
- C09K8/602—Compositions for stimulating production by acting on the underground formation containing surfactants
Abstract
The invention discloses a preparation method and application of an oil film volume expanding agent, wherein the preparation method comprises the following steps: (1) the oil-phase W/O type surfactant is wrapped outside by utilizing an O/W type surfactant, and the Span-80 is wrapped by utilizing self-made tetradecyl citrate to form O/W type emulsion in a water phase so as to achieve the purpose of conveying the oil-phase W/O type surfactant into an oil reservoir. (2) After the oil deposit is fed, calcium and magnesium ions are utilized to enable the tetradecanoyl citrate to form a chelate, so that the tetradecanoyl citrate is inactivated, the wrapped Span-80 is released, and the Span-80, an oil film and water form a water-in-oil emulsion, so that the aim of thickening the oil film is fulfilled. The oil displacement device is applied to oil displacement, so that an oil film is thickened, the friction force is increased, and the whole oil film is flushed out by utilizing pressure so as to achieve the effect of oil extraction. The invention makes full use of the good chelating characteristic of the myristoyl citrate, and reduces the demulsification difficulty of the emulsion.
Description
Technical Field
The invention belongs to the field of crude oil displacement, and particularly relates to a preparation method and application of an oil film volume expanding agent.
Background
The existing oil displacement is mainly to add an O/W type surfactant into water, and after the surfactant is driven into an oil reservoir by water displacement, the oil encounters crude oil to form an O/W type emulsion so as to achieve the effect of reducing the viscosity of the crude oil, but the O/W type emulsion is difficult to break compared with the W/O type emulsion. Therefore, an oil film volume expanding agent is developed, so that an oil film on the surface of a rock forms a water-in-oil emulsion, the volume of the oil film is increased, the effect of thickening is achieved, the resistance is increased, and the oil film is flushed out by pressure, so that oil displacement is simpler.
Disclosure of Invention
Residual oil in the stratum is exploited in an oil film thickening mode, so that the defect of difficult demulsification in the process of exploiting the original useful surfactant can be overcome; the invention provides a preparation method and application of an oil film volume expanding agent. The invention is applied to oil displacement, thickens an oil film, increases friction force, and utilizes pressure to flush out the whole oil film so as to achieve the effect of oil extraction. The invention makes full use of the good chelating characteristic of the myristoyl citrate, reduces the emulsion breaking difficulty of the emulsion, increases the volume and achieves the purpose of thickening the oil layer.
The technical scheme provided by the invention is as follows:
a preparation method of an oil film volume expanding agent comprises the following steps:
adding tetradecyl citrate into a water phase with a Span-80 surfactant as an oil phase to wrap the Span-80 to form an O/W type emulsion;
adding distilled water into O/W type emulsion, and stirring with magnetic stirring to obtain oil film volume expansion agent.
As a further improvement of the invention, the mass ratio of Span-80 to myristoyl citrate is (1:3) - (1: 5).
As a further improvement of the invention, the preparation method of the tetradecyl citrate comprises the following steps:
heating myristic acid to completely melt, adding PCl3Continuously reacting at 65-75 ℃, standing for layering after the reaction is finished, taking out supernatant, heating to evaporate excessive PCl3To obtain tetradecanoyl chloride;
adding acetone as a solvent into citric acid, heating to dissolve the citric acid, dropwise adding tetradecyl chloride in a reflux state, fully reacting, evaporating the acetone as the solvent, adding saturated saline solution for washing, removing excessive citric acid and other impurities, and drying the product under a reduced pressure condition to obtain tetradecyl citrate.
As a further improvement of the invention, myristic acid is used in combination with PCl3Is 1: 1.
As a further improvement of the invention, the molar ratio of the citric acid to the tetradecanoyl chloride is (1.2-1.3): 1.
As a further improvement of the invention, the adding amount of the distilled water is 1.5-3 times of the total mass of the Span-80 and the myristoyl citrate.
The oil film volume expanding agent prepared by the preparation method is applied to crude oil displacement.
Compared with the prior art, the invention has the advantages that:
the invention forms an oil-in-water emulsion outside, wherein the oil phase is Span-80, the Span-80 is sent into a high-salt oil reservoir by water, calcium and magnesium ions in the oil reservoir are chelated with an O/W type surfactant wrapping the Span-80 to cause inactivation, the Span-80 is released, the Span-80, an oil layer and water form a water-in-oil emulsion, so as to achieve the purpose of volume expansion of the oil layer, and the whole oil layer is driven out by increasing the pressure. The W/O surfactant is Span-80, Span-80 is a water-insoluble oil phase substance, when Span-80 is conveyed into an oil reservoir, only one O/W surfactant can be used for emulsifying the oil phase substance, and the O/W surfactant must be inactivated in the oil reservoir through a certain way. The oil displacement agent is simple in use method, can be prepared by uniformly mixing the two raw materials and water according to the proportion at normal temperature, is simple to prepare, provides possibility for production under various environments, and can be prepared into the oil displacement agent convenient to use by simple operation as long as the simplest container is provided. Provides a new idea for the oil displacement technology.
The oil displacement agent is applied to oil displacement, so that an oil film is thickened, the friction force is increased, and the whole oil film is flushed out by utilizing pressure so as to achieve the effect of oil extraction. The invention makes full use of the good chelating characteristic of the myristoyl citrate, and reduces the demulsification difficulty of the emulsion.
Drawings
FIG. 1 is a diagram showing the reaction mechanism of the present invention.
Detailed Description
The invention relates to an oil film volume expanding agent, which is prepared by the following specific steps:
the first step is as follows: the reaction equation for myristoyl citrate ester:
the principle is that a Span-80 surfactant is used as an oil phase, the Span-80 is wrapped in a water phase by using the prepared tetradecyl citrate to form O/W type emulsion, the emulsion is sent into a high-salt oil reservoir, the tetradecyl citrate is triggered by calcium and magnesium ions to form a chelate so as to inactivate, and the wrapped Span-80 is released. The released Span-80 can form W/O emulsion with water and an oil layer, so that the aim of thickening the oil layer is fulfilled, and the mechanism is shown in figure 1.
According to the above reaction mechanism, as shown in fig. 1, the method comprises the steps of:
(1) placing myristic acid into completely dried three-neck flask, heating to completely melt, controlling temperature at 70 deg.C, and slowly dropping PCl under stirring3The dropping time is 2.5h, and the myristic acid and PCl3The molar ratio of (1: 1), continuously reacting at 65-75 ℃ for 4h, standing for 1h after the reaction is finished, layering, taking out supernatant, and distilling at 100 DEG CExcess PCl3To obtain tetradecanoyl chloride, and bottling for use.
(2) Putting citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding tetradecyl chloride at a speed of 4g/min under a reflux state, wherein the molar ratio of the citric acid to the tetradecyl chloride is (1.2-1.3): 1, reacting for 3 hours, evaporating the solvent acetone, adding a certain amount of saturated saline solution at 60 ℃ for washing for 3 times, removing excessive citric acid and other impurities, and drying the product under a reduced pressure condition to obtain the tetradecyl citrate.
The second step is that: placing Span-80 and tetradecyl citrate into a beaker, wherein the mass ratio of Span-80 to tetradecyl citrate is 1 (3-5), adding distilled water which is 1.5-3 times of the total mass of Span-80 and tetradecyl citrate, and magnetically stirring until a uniform O/W emulsion is formed.
The third step: the resulting O/W emulsion was added to the core and the percent volume increase was measured.
The following are specific examples to illustrate the invention:
example 1
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 70 ℃ and 70g of PCl was slowly added dropwise with stirring3Dropwise adding for 2.5h, reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride.
Putting 56g of citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding 60g of tetradecyl chloride at the speed of 4g/min under the reflux state, reacting for 3h, evaporating the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃, washing for 3 times, removing excessive citric acid and other impurities, and drying under the reduced pressure condition to obtain the tetradecyl citrate.
15g of Span-80 and 45g of tetradecanoyl citrate are added into a beaker, 120g of distilled water is added, magnetons are added, and the mixture is magnetically stirred for 15min to form uniform O/W emulsion.
The resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 2
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 70 ℃ and 70g of PCl was slowly added dropwise with stirring3Dropwise adding for 2.5h, reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride.
Putting 61g of citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding 60g of tetradecyl chloride at the speed of 4g/min under the reflux state, reacting for 3h, evaporating the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃, washing for 3 times, removing excessive citric acid and other impurities, and drying under the reduced pressure condition to obtain the tetradecyl citrate.
15g of Span-80 and 45g of tetradecanoyl citrate are added into a beaker, 120g of distilled water is added, magnetons are added, and the mixture is magnetically stirred for 15min to form uniform O/W emulsion.
The resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 3
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 70 ℃ and 70g of PCl was slowly added dropwise with stirring3Dropwise adding for 2.5h, reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride.
Putting 56g of citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding 60g of tetradecyl chloride at the speed of 4g/min under the reflux state, reacting for 3h, evaporating the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃, washing for 3 times, removing excessive citric acid and other impurities, and drying under the reduced pressure condition to obtain the tetradecyl citrate.
12g of Span-80 and 48g of tetradecanoyl citrate are added into a beaker, 120g of distilled water is added, magnetons are added, and the mixture is magnetically stirred for 15min to form a uniform O/W emulsion.
The resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 4
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 70 ℃ and 70g of PCl was slowly added dropwise with stirring3Dropwise adding for 2.5h, reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride.
Putting 61g of citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding 60g of tetradecyl chloride at the speed of 4g/min under the reflux state, reacting for 3h, evaporating the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃, washing for 3 times, removing excessive citric acid and other impurities, and drying under the reduced pressure condition to obtain the tetradecyl citrate.
12g of Span-80 and 48g of tetradecanoyl citrate are added into a beaker, 120g of distilled water is added, magnetons are added, and the mixture is magnetically stirred for 15min to form a uniform O/W emulsion.
The resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 5
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 70 ℃ and 70g of PCl was slowly added dropwise with stirring3Dropwise adding for 2.5h, reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride.
Putting 56g of citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding 60g of tetradecyl chloride at the speed of 4g/min under the reflux state, reacting for 3h, evaporating the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃, washing for 3 times, removing excessive citric acid and other impurities, and drying under the reduced pressure condition to obtain the tetradecyl citrate.
10g of Span-80 and 50g of tetradecanoyl citrate are added into a beaker, 120g of distilled water is added, magnetons are added, and the mixture is magnetically stirred for 15min to form uniform O/W emulsion.
The resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 6
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 70 ℃ and 70g of PCl was slowly added dropwise with stirring3Dropwise adding for 2.5h, reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride.
Putting 61g of citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding 60g of tetradecyl chloride at the speed of 4g/min under the reflux state, reacting for 3h, evaporating the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃, washing for 3 times, removing excessive citric acid and other impurities, and drying under the reduced pressure condition to obtain the tetradecyl citrate.
10g of Span-80 and 50g of tetradecanoyl citrate are added into a beaker, 120g of distilled water is added, magnetons are added, and the mixture is magnetically stirred for 15min to form uniform O/W emulsion.
The resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 7
114g of myristic acid was placed in a completely dry three-neck flask, heated to completely melt, controlled at 65 ℃, and under full stirring, 70g of PCl was slowly dropped3The dropping time is 2.0h, and the myristic acid and PCl3The molar ratio of (1: 1), continuously reacting at 65 deg.C for 5h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 110 deg.C3To obtain tetradecanoyl chloride, and bottling for use.
(2) Putting citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding tetradecyl chloride at a speed of 4g/min under a reflux state, wherein the molar ratio of the citric acid to the tetradecyl chloride is 1.2:1, reacting for 3h, evaporating out the solvent acetone, adding a certain amount of saturated saline solution at 60 ℃ for washing for 3 times, removing excessive citric acid and other impurities, and drying the product under a reduced pressure condition to obtain the tetradecyl citrate.
The second step is that: placing the Span-80 and the tetradecyl citrate into a beaker, wherein the mass ratio of the Span-80 to the tetradecyl citrate is 1:3, adding distilled water which is 1.5 times of the total mass of the Span-80 and the tetradecyl citrate, and magnetically stirring until a uniform O/W emulsion is formed.
The third step: the resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 8
Placing myristic acid into completely dried three-neck flask, heating to completely melt, controlling temperature at 75 deg.C, and slowly dropping PCl under stirring3The dropping time is 3h, and the myristic acid and PCl3The molar ratio of (1: 1) is continuously reacted for 3h at 75 ℃, the reaction is kept still for 1h after the reaction is finished, the mixture is layered, the supernatant is taken out, and excessive PCl is distilled off at the temperature of 100 DEG C3To obtain tetradecanoyl chloride, and bottling for use.
(2) Putting citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding tetradecyl chloride at the speed of 3.5g/min under the reflux state, wherein the molar ratio of the citric acid to the tetradecyl chloride is 1.25:1, reacting for 3h, evaporating out the solvent acetone, adding a certain amount of saturated saline solution at the temperature of 60 ℃ to wash for 3 times, removing excessive citric acid and other impurities, and drying the product under the reduced pressure condition to obtain the tetradecyl citrate.
The second step is that: placing the Span-80 and the tetradecyl citrate into a beaker, wherein the mass ratio of the Span-80 to the tetradecyl citrate is 1:5, adding distilled water which is 3 times of the total mass of the Span-80 and the tetradecyl citrate, and magnetically stirring until a uniform O/W emulsion is formed.
The third step: the resulting O/W emulsion was added to the core and the percent volume increase was measured.
Example 9
Placing myristic acid into completely dried three-neck flask, heating to completely melt, controlling temperature at 70 deg.C, and slowly dropping PCl under stirring3The dropping time is 2.5h, and the myristic acid and PCl3The molar ratio of (1: 1), continuously reacting at 70 deg.C for 4h, standing for 1h after reaction, layering, taking out supernatant, and evaporating excessive PCl at 100 deg.C3To obtain tetradecanoyl chloride, and bottling for use.
(2) Putting citric acid into a three-neck flask, adding acetone as a solvent, heating to dissolve the citric acid, dropwise adding tetradecyl chloride at a speed of 4g/min under a reflux state, wherein the molar ratio of the citric acid to the tetradecyl chloride is 1.3:1, reacting for 3h, evaporating out the solvent acetone, adding a certain amount of saturated saline solution at 60 ℃ for washing for 3 times, removing excessive citric acid and other impurities, and drying the product under a reduced pressure condition to obtain the tetradecyl citrate.
The second step is that: placing Span-80 and tetradecyl citrate into a beaker, wherein the mass ratio of Span-80 to tetradecyl citrate is 1:4, adding distilled water with the mass of 2 times of the total mass of Span-80 and tetradecyl citrate, and magnetically stirring until a uniform O/W emulsion is formed.
The third step: the resulting O/W emulsion was added to the core and the percent volume increase was measured. The specific data are shown in Table 1.
Table 1 percentage volume increase in each example
As can be seen from Table 1, the percentage of volume increase in example 9 is the highest, indicating that the oil film volume expander produced by the process is more effective when the citric acid content is increased and the mass ratio of Span-80 to myristoyl citrate is 1: 4.
The foregoing is a more detailed description of the invention and it is not intended that the invention be limited to the specific embodiments described herein, but that various modifications, alterations, and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be construed to fall within the scope of the invention as defined by the appended claims.
Claims (7)
1. The preparation method of the oil film volume expanding agent is characterized by comprising the following steps:
adding tetradecyl citrate into a water phase with a Span-80 surfactant as an oil phase to wrap the Span-80 to form an O/W type emulsion;
adding distilled water into O/W type emulsion, and stirring with magnetic stirring to obtain oil film volume expansion agent.
2. The method for preparing the oil film volume expanding agent according to claim 1, wherein the mass ratio of Span-80 to myristoyl citrate is 1 (3-5).
3. The preparation method of the oil film volume expanding agent according to claim 1, wherein the preparation method of the tetradecanoyl citrate is as follows:
heating myristic acid to completely melt, adding PCl3Continuously reacting at 65-75 ℃, standing for layering after the reaction is finished, taking out supernatant, heating to evaporate excessive PCl3To obtain tetradecanoyl chloride;
adding acetone as a solvent into citric acid, heating to dissolve the citric acid, dropwise adding tetradecyl chloride in a reflux state, fully reacting, evaporating the acetone as the solvent, adding saturated saline solution for washing, removing excessive citric acid and other impurities, and drying the product under a reduced pressure condition to obtain tetradecyl citrate.
4. The method for preparing an oil film volume expander as claimed in claim 3, wherein the myristic acid is reacted with PCl3Is 1: 1.
5. The method for preparing the oil film volume expanding agent according to claim 3, wherein the molar ratio of citric acid to tetradecanoyl chloride is (1.2-1.3): 1.
6. The method for preparing an oil film volume expander according to claim 1, wherein the amount of distilled water added is 1.5-3 times of the total mass of Span-80 and tetradecyl citrate.
7. The use of the oil film volume expanding agent prepared by the preparation method of any one of claims 1 to 6 in oil displacement of crude oil.
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