CN111272612B - Primary screening method of demulsifier - Google Patents
Primary screening method of demulsifier Download PDFInfo
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- CN111272612B CN111272612B CN202010138864.5A CN202010138864A CN111272612B CN 111272612 B CN111272612 B CN 111272612B CN 202010138864 A CN202010138864 A CN 202010138864A CN 111272612 B CN111272612 B CN 111272612B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
Abstract
The invention discloses a primary screening method of a demulsifier, and relates to the technical field of oilfield chemistry. The invention comprises the following steps: placing a solution containing a certain reagent and an oil-in-water emulsion droplet in a sample cell, and placing the sample cell in a sample cell clamping groove; acquiring the interaction force between two emulsion drops in the sample cell; and (3) selecting a system in which the interaction force of the emulsion drops in the solution is not only repulsive force, removing the two optical traps to observe whether the two emulsion drops are polymerized, and if the polymerization is carried out, obtaining the attractive force caused by vacancy force except Van der Waals force, and if the maximum value of the attractive force is greater than a limit value, using the system as a demulsifier. The invention provides a method for optimizing demulsifier through interaction force between emulsion drops, which adopts an optical tweezers technology to measure the interaction force between the emulsion drops and obtains attraction force caused by vacancy force through calculation.
Description
Technical Field
The invention belongs to the technical field of oilfield chemistry, and relates to a method for determining emulsion stability and primarily screening a demulsifier, in particular to a method for primarily screening a demulsifier.
Background
The efficient demulsification of petroleum emulsion is always an important production link for oil field exploitation and refinery desalination and dehydration. Researchers have studied the stability of oil-in-water (O/W) emulsions over the years in terms of emulsifier type, droplet size in the emulsion, interfacial tension, interfacial film strength, and interfacial charge to select suitable demulsifiers. The methods for researching the stability of the emulsion mainly comprise a colorimetric method, a turbidity method, an electric conductivity method, an interfacial tension method, an interfacial shear viscosity method and the like. The current more uniform understanding of stable emulsions is that emulsifiers adsorb on phase interfaces to reduce interfacial tension and the potential energy of the dispersed system is reduced; the toughness or high-viscosity interface film is formed on the interface, namely, the strength of the interface film is improved, so that the coalescence of liquid drops caused by collision can be prevented; when the emulsifier molecules are charged, the surfaces of the liquid drops are charged to form an electric double layer, and the probability of coalescence caused by approach and collision of the liquid drops is reduced. These are mainly based on the geometry and physical properties of the interface layer to consider the stability of the emulsion, and can not reveal the nature of the stability of the O/W emulsion from the interaction force among oil drops, meanwhile, the screening time is different, sometimes even as long as 24 hours, because the nature of the reagent to be screened is different, in addition, the oil sample and the reagent are consumed in the experimental process.
Disclosure of Invention
The invention aims to provide a primary screening method of a demulsifier, aiming at the defects of the prior art, the method combines the interaction force between two emulsion drops and the attraction force caused by vacancy force to screen the demulsifier, wherein the interaction force is measured by adopting an optical tweezers technology, the attraction force caused by the vacancy force is calculated by adopting the optical tweezers technology and a related formula, and compared with the current universal method for optimizing the demulsifier, the primary screening method of the demulsifier has the advantages of less consumption of oil samples and medicaments and fast primary screening.
The specific scheme of the invention is as follows:
the primary screening method of the demulsifier comprises the following steps:
a1, injecting a solution containing a reagent and an oil-in-water emulsion into a sample cell, and placing the sample cell in a sample cell clamping groove;
a2, capturing two emulsion drops in a sample cell by using a double optical trap, adjusting the distance of the two emulsion drops to gradually approach each other, and measuring the interaction force of the two emulsion drops in the reagent solution under the condition of different distances;
the difference of the sizes of the two emulsion drops is not more than 0.02 micrometer, and the double optical traps are respectively a point optical trap and a line optical trap;
a3, if the interaction forces measured in step A2 are repulsive forces, the agent cannot act as a demulsifier, otherwise, the two optical traps are removed to observe whether the two emulsion droplets are polymerized. If two emulsion drops can exist independently and stably, the agent cannot be used as a demulsifier, otherwise, the attraction force caused by vacancy force except Van der Waals force between the two emulsion drops is calculated, if the maximum value of the attraction force exceeds a limit value, the agent is used as an optional emulsifier, otherwise, the agent cannot be used as the demulsifier;
the step of finding the attractive force between two emulsion droplets caused by the vacancy force is as follows:
b1, fixing the two emulsion drops obtained in the step A2 by using a double optical trap, replacing substances except the two fixed emulsion drops in the sample cell by using water, and then repeating the step A2 to measure the interaction force of the two emulsion drops in the water under different distance conditions;
b2, calculating the difference of the interaction forces of the two emulsion drops in the reagent solution and the water to obtain the interaction force induced by the unadsorbed chemical substances between the two emulsion drops; (ii) a
B3, calculating the attraction force between the two emulsion droplets caused by the vacancy force by the interaction force induced by the unadsorbed chemicals between the two emulsion droplets.
Preferably, the step of calculating the attraction force between two emulsion droplets caused by the vacancy force in the step B3 is as follows:
c1, correcting the optical trap to obtain optical trap rigidity k, and measuring the surface distance between the two emulsion drops and the radius of the two emulsion drops by using an optical trap technology; measuring the Zeta potential by a Zeta potentiometer;
c2, calculating the attraction force between two emulsion droplets caused by the vacancy force: the interaction force induced by unadsorbed chemical substances between the two emulsion drops is the resultant force of electric double layer repulsion force, van der waals attraction force and attraction force caused by vacancy force, wherein the electric double layer repulsion force and van der waals attraction force between the two emulsion drops are calculated by known variables and formulas, and the calculation formula of the attraction force caused by vacancy force is as follows:
Fdep＝Ftol-Fel-FVDW
wherein, FdepThe attraction between two emulsion droplets caused by the vacancy forces, FtolInteraction force induced by unadsorbed chemicals between two emulsion droplets, FelIs the electric double layer repulsive force between two emulsion droplets, FVDWIs composed of two milksVan der waals attraction between drops;
the calculation formula of the electric double layer repulsive force between two emulsion droplets is as follows:
Z＝(eξ/kBT)(R/λb)(1+κR)
λb＝e2/4πε0εrkBT
where ξ is the Zeta potential, e is the elementary charge, ε0Is a vacuum dielectric constant of ∈rIs the relative dielectric constant of the solution, R is the radius of the emulsion droplet, κ is the reciprocal of the Debye length, and x is the surface distance between two emulsion droplets; k is a radical ofBBoltzmann constant, T is temperature;
the calculation formula of van der waals attraction between two emulsion droplets is as follows:
wherein A is a Hammarsk constant;
c3, controlling the two emulsion drops to approach continuously by the optical trap technology, repeating the steps C1-C2, and calculating the attraction force of the two emulsion drops caused by the vacancy force under different distances;
or
Repeating the steps C1-C2, calculating the attractive force of the two emulsion drops caused by the vacancy force under the condition of two or more different distances, fitting the attractive force into a fitting calculation formula of the attractive force caused by the vacancy force to obtain the osmotic pressure between micelles in the solution and the action range of the attractive force caused by the vacancy force, and calculating the attractive force caused by the vacancy force under the condition of different distances according to the fitting calculation formula of the attractive force caused by the vacancy force, wherein the fitting calculation formula of the attractive force caused by the vacancy force is as follows:
wherein pi is the osmotic pressure between micelles in the solution, and 2 delta is the action range of the attraction force caused by the vacancy force.
Preferably, the limit value in step a3 is 1 pN.
Preferably, the volume of the sample cell is 200-600 microliters; the laser intensity of the double optical traps is 0.15W; the sizes of the two emulsion drops are 3.4-3.8 micrometers; the distance between the spherical centers of the two emulsion drops is set to be 6.5-7.2 microns.
The method for measuring the interaction force between two emulsion drops by using the optical tweezers technology in the scheme is a known technology, specifically, one emulsion drop is controlled to approach to an emulsion drop controlled by a point optical trap at a certain speed through the line optical trap, and the interaction force between the two emulsion drops is obtained by optical tweezers software according to the position of the center of the emulsion drop deviating from the optical trap and the rigidity of the optical trap; meanwhile, the experiment result is influenced by the disturbance caused by the liquid flow due to the fact that the speed is too high, the experiment time is prolonged due to the fact that the speed is too low, the speed is determined to be 40nm/s, and the disturbance caused by the liquid flow can be avoided at the speed.
Meanwhile, the invention improves a sample cell in the conventional optical tweezers technology, so as to be convenient for replacing a medium in the sample cell, the sample cell is a two-way quantitative sample cell and comprises an upper layer glass slide, a lower layer cover glass and a middle layer which are fixed by glue, and the middle layer is an annular rubber pad with two through holes correspondingly arranged on the peripheral side.
Has the advantages that: the invention provides a method for optimizing demulsifier and emulsifier by interaction force between emulsion droplets, which adopts optical tweezers technology to measure the interaction force, adopts the optical tweezers technology and a related formula to calculate out attraction force caused by vacancy force, and has the advantages of small sample pool volume, low consumption of required oil sample (emulsion droplets), low consumption of medicament (volume to be selected), fast primary screening and no influence of the property of the reagent to be screened on screening time.
Drawings
FIG. 1 shows the interaction force of two emulsion droplets in 5.0cmc SDBS and water, respectively;
FIG. 2 is a graph of the pure vacancy force induced attraction of two emulsion droplets in a 5.0cmc SDBS;
FIG. 3 shows the interaction force of two emulsion droplets in water at 10.0cmc SDBS;
FIG. 4 is a graph of the pure vacancy force induced attraction of two emulsion droplets in a 10.0cmc SDBS;
FIG. 5 shows the interaction force of two emulsion droplets in 5.0cmc CTAB and water, respectively;
FIG. 6 is a pure vacancy force induced attraction force with two emulsion droplets in 5.0cmc CTAB;
FIG. 7 shows the interaction force of two emulsion droplets in water at 10.0cmc CTAB;
FIG. 8 is a pure vacancy force induced attraction force with two emulsion droplets in 10.0cmc CTAB;
FIG. 9 shows the interaction force of two emulsion droplets in water at 5.0cmc OP-10;
in fig. 2, 4, 6, and 8, the legend fit represents the curve after fitting.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The oil-in-water emulsion in the following examples 1-6 is prepared by putting oil (toluene) and water in a mass ratio of 5:95 into a high-speed shearing machine and emulsifying for 5min at 14000 r/min.
The solvents to be selected were different surfactants with the following critical micelle concentrations (cmc):
SDBS，2.9×10-3M；
CTAB，9.2×10-4M；
OP-10，2.1×10-4M。
example 1
1. 600 microliters of an oil-in-water emulsion containing 5.0cmc SDBS was injected into a quantification cuvette and placed in a Nikon microscope cuvette card slot.
2. A pair of emulsion droplets with the diameter of 3.40 mu m in an oil-in-water emulsion are respectively captured by using double optical traps (one is a point optical trap, the other is a line optical trap, the laser intensity is 0.15W), a camera and the optical traps are corrected, then the two optical traps are set to be 6.90 mu m, the distance between the two optical traps is adjusted to be gradually close to each other (the line optical trap controls the captured emulsion droplets to be gradually close to the emulsion droplets controlled by the point optical trap at a certain speed (40 nm/s)), and the interaction force of the two emulsion droplets under different surface distances is measured.
3. Fixing the two emulsion drops by using a double optical trap, injecting 4mL of water into a quantitative sample pool by using a micro-injection part to replace the aqueous solution containing 5.0cmc SDBS, and then measuring the interaction force between the two emulsion drops at different distances.
4. The experimental results are as follows: the interaction force of two emulsion drops in the solvent and water is shown in figure 1, and the two emulsion drops in the 5.0cmc SDBS solvent have repulsive force and attractive force; continued fitting to obtain its pure vacancy force induced attraction is shown in fig. 2, from which it can be derived that the maximum vacancy force induced attraction is 6.5pN, and the experiment results in the coalescence of the two droplets after the optical trap is removed. This indicates that the oil-in-water emulsion at this point is unstable due to attraction and therefore this concentration of the agent can act as a breaker.
Example 2
1. Injecting 600 microliters of SDBS oil-in-water emulsion containing 10.0cmc into a quantitative sample cell, and placing the emulsion in a sample cell clamping groove of a Nikon microscope;
2. a pair of emulsion droplets with the diameter of 3.40 mu m in an oil-in-water emulsion are respectively captured by using double optical traps (one is a point optical trap, the other is a line optical trap, the laser intensity is 0.15W), a camera and the optical traps are corrected, then the two optical traps are set to be 6.90 mu m and the distance between the two optical traps is adjusted to be gradually close to each other (the line optical trap controls the captured emulsion droplets to gradually close to the emulsion droplets controlled by the point optical trap at a certain speed (40 nm/s)), and the interaction force between the two emulsion droplets at different distances is measured.
3. The two emulsion droplets were fixed with a double optical trap, and 4mL of water was injected into the quantitative sample cell with a microinjection part to replace the aqueous solution containing 10.0cmc SDBS, and then the interaction force between the two emulsion droplets was measured.
4. The experimental results are as follows: the interaction force of two emulsion drops in the solvent and water is shown in figure 3, and the two emulsion drops in the 10.0cmc SDBS solvent have repulsive force and attractive force; continued fitting to obtain its pure vacancy force induced attraction is shown in fig. 4, from which it can be derived that the maximum vacancy force induced attraction is 38.6pN, and the experiment results in the coalescence of the two droplets after the optical trap is removed. This indicates that the oil-in-water emulsion at this point is unstable due to attraction and therefore this concentration of the agent can act as a breaker.
Example 3
1. Injecting 600 microliter of CTAB oil-in-water emulsion containing 5.0cmc into a quantitative sample cell, and placing the emulsion in a sample cell neck of a Nikon microscope;
2. a pair of emulsion droplets with the diameter of 3.45 mu m in an oil-in-water emulsion are respectively captured by using double optical traps (one is a point optical trap, the other is a line optical trap, the laser intensity is 0.15W), a camera and the optical traps are corrected, then the two optical traps are set to be 7.1 mu m and the distance between the two optical traps is adjusted to be gradually close to each other (the line optical trap controls the captured emulsion droplets to be gradually close to the emulsion droplets controlled by the point optical trap at a certain speed (40 nm/s)), and the interaction force between the two emulsion droplets at different distances is measured.
3. Fixing the two emulsion drops by using a double optical trap, injecting 4mL of water into a quantitative sample pool by using a micro-injection part to replace the water solution containing 5.0cmc CTAB, and then measuring the interaction force between the two emulsion drops.
4. The experimental results are as follows: the interaction force of two emulsion drops in the solvent and water is shown in figure 5, and in the 5.0cmc CTAB solvent, the two emulsion drops have both repulsive force and attractive force; continued fitting to obtain its pure vacancy force induced attraction is shown in fig. 6, from which it can be derived that the maximum vacancy force induced attraction is 11.4pN, and the experiment results in the coalescence of the two droplets after the optical trap is removed. This indicates that the oil-in-water emulsion at this point is unstable due to attraction and therefore this concentration of the agent can act as a breaker.
Example 4
1. Injecting 600 microliter of CTAB oil-in-water emulsion containing 10.0cmc into a quantitative sample cell, and placing the emulsion in a sample cell neck of a Nikon microscope;
2. a pair of emulsion droplets with the diameter of 3.45 mu m in an oil-in-water emulsion are respectively captured by using double optical traps (one is a point optical trap, the other is a line optical trap, the laser intensity is 0.15W), a camera and the optical traps are corrected, then the two optical traps are set to be 7.1 mu m and the distance between the two optical traps is adjusted to be gradually close to each other (the line optical trap controls the captured emulsion droplets to be gradually close to the emulsion droplets controlled by the point optical trap at a certain speed (40 nm/s)), and the interaction force between the two emulsion droplets at different distances is measured.
3. Fixing the two emulsion drops by using a double-optical trap, injecting 4mL of water into a quantitative sample pool by using a micro-injection part to replace the aqueous solution containing 10.0cmc CTAB, and then measuring the interaction force between the two emulsion drops.
4. The experimental results are as follows: the interaction force of two emulsion drops in the solvent and water is shown in figure 7, and in the 10.0cmc CTAB solvent, the two emulsion drops have both repulsive force and attractive force; continued fitting to obtain its pure vacancy force induced attraction is shown in fig. 8, from which it can be derived that the maximum vacancy force induced attraction is 22.1pN, and the experiment results in the coalescence of the two droplets after the optical trap is removed. This indicates that the oil-in-water emulsion at this point is unstable due to attraction and therefore this concentration of the agent can act as a breaker.
Example 5
1. Injecting 600 microliters of oil-in-water emulsion containing 5.0cmc OP-10 into a quantitative sample cell, and placing the quantitative sample cell in a sample cell clamping groove of a Nikon microscope;
2. a pair of emulsion droplets with the diameter of 3.40 mu m in an oil-in-water emulsion are respectively captured by using double optical traps (one is a point optical trap, the other is a line optical trap, the laser intensity is 0.15W), a camera and the optical traps are corrected, then the two optical traps are set to be 6.90 mu m and the distance between the two optical traps is adjusted to be gradually close to each other (the line optical trap controls the captured emulsion droplets to gradually close to the emulsion droplets controlled by the point optical trap at a certain speed (40 nm/s)), and the interaction force between the two emulsion droplets at different distances is measured.
3. The two emulsion drops are fixed by a double optical trap, 4mL of water is injected into a quantitative sample pool by a micro-injection part to replace the aqueous solution containing 5.0cmc OP-10, and then the interaction force between the two emulsion drops is measured.
4. The experimental results are as follows: the interaction force of two emulsion drops in solvent and water is shown in figure 9, and in 5.0cmc OP-10, only repulsive force exists between the two emulsion drops, and the two emulsion drops are separated after the optical trap is removed. This indicates that the oil-in-water emulsion at this point is stable due to repulsion and that this concentration of agent does not act as a demulsifier.
The present invention has been disclosed in the foregoing in terms of preferred embodiments, but it will be understood by those skilled in the art that these embodiments are merely illustrative of the present invention and should not be construed as limiting the scope of the present invention. Further modifications are possible without departing from the principles of the invention and these modifications are to be considered as protection of the invention.
Claims (3)
1. The primary screening method of the demulsifier comprises the following steps:
a1, injecting a solution containing a reagent and an oil-in-water emulsion into a sample cell, and placing the sample cell in a sample cell clamping groove;
a2, capturing two emulsion drops in a sample cell by using a double optical trap, adjusting the distance of the two emulsion drops to gradually approach each other, and measuring the interaction force of the two emulsion drops in the reagent solution under the condition of different distances;
the difference of the sizes of the two emulsion drops is not more than 0.02 micrometer, and the double optical traps are respectively a point optical trap and a line optical trap;
a3, if the interaction forces measured in the step A2 are repulsive forces, the reagent cannot be used as a demulsifier, otherwise, two optical traps are removed to observe whether two emulsion drops are polymerized, if the two emulsion drops can independently and stably exist, the reagent cannot be used as the demulsifier, otherwise, the attraction force caused by vacancy force between the two emulsion drops is solved, if the maximum value of the attraction force exceeds a limit value, the reagent is used as an optional emulsifier, otherwise, the reagent cannot be used as the demulsifier;
the step of finding the attractive force between two emulsion droplets caused by the vacancy force is as follows:
b1, fixing the two emulsion drops obtained in the step A2 by using a double optical trap, replacing substances except the two fixed emulsion drops in the sample cell by using water, and then repeating the step A2 to measure the interaction force of the two emulsion drops in the water under different distance conditions;
b2, calculating the difference of the interaction forces of the two emulsion drops in the reagent solution and the water to obtain the interaction force induced by the unadsorbed chemical substances between the two emulsion drops;
b3, calculating the attraction force caused by the vacancy force between the two emulsion drops through the interaction force induced by the unadsorbed chemical substances between the two emulsion drops, and specifically comprising the following steps:
c1, correcting the optical trap to obtain optical trap rigidity k, and measuring the surface distance between the two emulsion drops and the radius of the two emulsion drops by using an optical trap technology; measuring the Zeta potential by a Zeta potentiometer;
c2, calculating the attraction force between two emulsion droplets caused by the vacancy force: the interaction force induced by unadsorbed chemical substances between the two emulsion drops is the resultant force of electric double layer repulsion force, van der waals attraction force and attraction force caused by vacancy force, wherein the electric double layer repulsion force and van der waals attraction force between the two emulsion drops are calculated by known variables and formulas, and the calculation formula of the attraction force caused by vacancy force is as follows:
Fdep＝Ftol-Fel-FVDW
wherein, FdepThe attraction between two emulsion droplets caused by the vacancy forces, FtolInteraction force induced by unadsorbed chemicals between two emulsion droplets, FelIs the electric double layer repulsive force between two emulsion droplets, FVDWIs the van der waals attraction between two emulsion droplets;
the calculation formula of the electric double layer repulsive force between two emulsion droplets is as follows:
Z＝(eξ/kBT)(R/λb)(1+κR)
λb＝e2/4πε0εrkBT
where ξ is the Zeta potential, e is the elementary charge, ε0Is a vacuum dielectric constant of ∈rIs the relative dielectric constant of the solution, R is the radius of the emulsion droplet, κ is the reciprocal of the Debye length, and x is the surface distance between two emulsion droplets; k is a radical ofBBoltzmann constant, T is temperature;
the calculation formula of van der waals attraction between two emulsion droplets is as follows:
wherein A is a Hammarsk constant;
c3, controlling the two emulsion drops to approach continuously by the optical trap technology, repeating the steps C1-C2, and calculating the attraction force of the two emulsion drops caused by the vacancy force under different distances;
or
Repeating the steps C1-C2, calculating the attractive force of the two emulsion drops caused by the vacancy force under the condition of two or more different distances, fitting the attractive force into a fitting calculation formula of the attractive force caused by the vacancy force to obtain the osmotic pressure between micelles in the solution and the action range of the attractive force caused by the vacancy force, and calculating the attractive force caused by the vacancy force under the condition of different distances according to the fitting calculation formula of the attractive force caused by the vacancy force, wherein the fitting calculation formula of the attractive force caused by the vacancy force is as follows:
where Π is the osmotic pressure between micelles in solution, and 2 Δ is the attractive force range due to vacancy forces.
2. The method for prescreening the demulsifier of claim 1 wherein the limit of step a3 is 1 pN.
3. The primary screening method of the demulsifier of claim 1, wherein the volume of the sample cell is 200-600 microliters; the laser intensity of the double optical traps is 0.15W; the sizes of the two emulsion drops are 3.4-3.8 micrometers; the distance between the spherical centers of the two emulsion drops is set to be 6.5-7.2 microns.
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