CN116120908B - Preparation method of ultra-thick oil emulsified viscosity-reducing microemulsion - Google Patents
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Abstract
The invention relates to the technical field of viscous oil emulsification viscosity reduction, and discloses a preparation method of an ultra-viscous oil emulsification viscosity reduction microemulsion, which comprises the following steps: (1) Firstly, mixing diesel oil and super heavy oil (0.3-1.5): 1, keeping the temperature in a water bath at 55 ℃, standing for 15min, and stirring for 20min under the condition of 1200-1500 r/min by using a stirrer; (2) Preparing 0.5% of octyl phenol polyoxyethylene ether-10 solution by mass, uniformly stirring at 20-30 ℃ and stirring speed of 400-800 r/min, and standing for 5 hours until the surfactant is completely dissolved in water; (3) Adding the prepared 0.5% octyl phenol polyoxyethylene ether-10 solution into a mixed system of diesel oil and super heavy oil, and stirring for 20min at the constant temperature of 55 ℃ and the stirring rotation speed of 1200-1500 r/min to obtain the emulsified viscosity-reducing oil-in-water microemulsion, wherein the particle size range of emulsion liquid drops is 100-150 mu m. The microemulsion has the advantages of low consumption of surfactant, easily available raw materials, simple preparation process, high viscosity reduction rate up to 99.81%, and capability of improving recovery ratio.
Description
Technical Field
The invention relates to the technical field of viscosity reduction of thickened oil, in particular to a preparation method of an ultra-thickened oil emulsifying viscosity-reducing microemulsion.
Background
The thickened oil resources are quite abundant as one of four large thickened oil production countries in the world. However, due to the characteristics of deep burial of the super heavy oil reservoir, high formation temperature, high pressure, high viscosity of the super heavy oil, high condensation point, poor fluidity and the like, the exploitation difficulty of the super heavy oil is high, and the recovery ratio of an oil field is low. For example, crude oil of Tahe oil field and Liaohe oil field in China belongs to a typical super heavy oil reservoir, and the viscosity of the crude oil is as high as 5 multiplied by 10 4 ~3×10 6 mPas. Because the flow resistance of the super-thick oil is large, the super-thick oil can flow into a shaft from an oil layer or can be lifted to the ground from the shaft to face heavy difficulties, so that the current super-thick oil exploitation has a plurality of difficulties. Among the numerous super-thick oil exploitation methods, the emulsification viscosity-reducing method is valued by more and more scientific researchers by virtue of the advantages of greenness, high efficiency, innocuity, stability and low carbon economy, and has important significance for improving the super-thick oil viscosity-reducing exploitation efficiency.
At present, the emulsification viscosity-reducing method is one of the most effective ways to produce super-thick oil. In order to realize efficient viscosity reduction of the ultra-thick oil emulsification, the method is firstly prepared and proper surfactant types, injection methods and injection amounts are selected according to parameters such as the component structure, the physicochemical properties, the stratum conditions and the like of the ultra-thick oil. The super heavy oil has the characteristics of few straight-run fractions, extremely high viscosity, high asphaltene colloid content and large heavy components, and has the characteristics similar to those of atmospheric residuum and even vacuum residuum, and the viscosity is mainly determined by the colloid and asphaltene content of the heavy components, so that the viscosity reducing effect of the conventional emulsification viscosity reducing method is not obvious. With the continuous deep exploitation, the formation condition is worsened, the pressure and temperature of the formation water are increased, and the microemulsion prepared by the conventional emulsification viscosity-reducing method cannot bear the severe formation environment for a long time, so that the viscosity-reducing effect of the super-heavy oil is poor, and the exploitation efficiency is low. In summary, the invention provides a preparation method of an ultra-thick oil emulsifying viscosity-reducing microemulsion.
Disclosure of Invention
Aiming at the problems of high exploitation difficulty of the super heavy oil in China and the like at present, the invention provides a preparation method of the super heavy oil emulsification viscosity-reducing microemulsion. The emulsion viscosity-reducing microemulsion prepared by the invention has the advantages of easily available raw materials, simple preparation process, no byproducts, safety, environmental protection, high emulsion viscosity-reducing rate and the like.
The invention is realized by the following technical scheme:
a nonionic surfactant used in the preparation method of the ultra-thick oil emulsified viscosity-reducing microemulsion is octyl phenol polyoxyethylene ether-10, and the molecular structural formula of the nonionic surfactant is shown in figure 1.
The nonionic surfactant has high stability, good solubility in various solvents, no strong adsorption on the solid surface, and good use effect.
The invention aims to disclose a preparation method of an ultra-thick oil emulsified viscosity-reducing microemulsion, which comprises the following specific steps:
(1) Adding quantitative diesel oil and super-thick oil into a beaker, standing for 15min at a temperature of 55 ℃ under the condition of controlling the temperature, and stirring for 20min under the condition of 1200-1500 r/min by using a stirrer to obtain the mixed thin thick oil;
(2) Adding deionized water and a certain amount of octyl phenol polyoxyethylene ether-10 into another beaker, uniformly stirring at the temperature of 20-30 ℃ and the stirring speed of 400-800 r/min, and standing for 5 hours until the surfactant is completely dissolved in water to obtain an octyl phenol polyoxyethylene ether-10 aqueous solution;
(3) And adding the prepared octyl phenol polyoxyethylene ether-10 solution into a mixed system of diesel oil and super heavy oil, and stirring for 20min at the constant temperature of 55 ℃ and the stirring rotation speed of 1200-1500 r/min to obtain the emulsified viscosity-reducing microemulsion.
According to the invention, in the step (1), the mass ratio of diesel oil to super heavy oil is 1.5:1.
Further preferably, in the step (1), the mass ratio of the diesel oil to the super heavy oil is (0.3-0.5): 1.
Experiments show that the monomer selection, the monomer proportioning and the monomer adding method have good effect on reducing the viscosity of the super-thick oil, the viscosity reduction rate of the super-thick oil is 95-97% when the mass ratio of the diesel oil to the super-thick oil is 1.5:1, and the viscosity reduction efficiency of the super-thick oil is best and can reach 98-99.5% when the mass ratio of the diesel oil to the super-thick oil is (0.3-0.5): 1. However, when the mass ratio of the diesel oil to the super-thick oil is smaller than 0.3:1, the viscosity reducing rate of the super-thick oil is reduced to 88-91%, and compared with the mass ratio of the diesel oil to the super-thick oil (0.3-0.5): 1, the viscosity reducing effect is lower.
According to the invention, in the step (2), the mass fraction of the solution of the octyl phenol polyoxyethylene ether-10 is 0.5%.
According to the invention, the oil-water ratio of the diesel oil and super heavy oil mixed system and the octyl phenol polyoxyethylene ether-10 in the step (3) is 3:7.
The invention has the technical characteristics and advantages that:
the preparation method of the ultra-thick oil emulsified viscosity-reducing microemulsion has the advantages of easily available raw materials, simple preparation process, small addition amount of surfactant and good viscosity-reducing effect. Because of the existence of a large amount of asphaltene and colloid in the ultra-thick oil, the asphaltene contains functional groups such as carboxyl, pyrrolyl, pyridyl, thienyl, sulfite and the like which are composed of heteroatoms such as N, O, S and the like, hydrogen bonds are formed among the functional group atoms, aromatic condensed ring planes are piled up, and the polar interaction force of the functional groups jointly acts to cause the high viscosity state of the ultra-thick oil, so that the ultra-thick oil is more difficult to reduce viscosity than conventional crude oil and common thick oil, and mining is difficult. According to the invention, the nonionic surfactant octyl phenol polyoxyethylene ether-10 is used as a monomer, and is uniformly mixed with the diesel oil super-thick oil mixing system to prepare the emulsified viscosity-reducing microemulsion, so that the viscosity of the super-thick oil can be effectively reduced, and the recovery ratio is improved.
Drawings
The purpose of the attached drawings is as follows: in order to more clearly illustrate the embodiments and technical solutions of the present invention, the drawings that are required for the embodiments will be simply labeled and described below.
FIG. 1 is a molecular structural formula diagram of a nonionic surfactant, namely octyl phenol polyoxyethylene ether-10.
FIG. 2 is a graph showing experimental data for evaluating the viscosity-reducing effect of the emulsion viscosity-reducing microemulsion according to each embodiment.
Fig. 3 is a schematic structural diagram of a flat-plate rotor system of an Anton Par MCR302 rheometer and a viscosity-temperature curve chart of ultra-thick oil.
Fig. 4 is a schematic structural diagram of an Anton Par MCR302 rheometer coaxial cylinder system and a viscosity shear graph of super heavy oil.
Fig. 5 is a view of the observation result of an emulsified viscosity-reducing microemulsion drop microscope.
FIG. 6 is a graph showing the comparison of the effects of the emulsion viscosity-reducing microemulsion of the super heavy oil.
Description of the embodiments
In order to make the technical solution in the present specification better understood, the technical solution in one or more embodiments of the present specification will be clearly and completely described in the following description with reference to the drawings in one or more embodiments of the present specification, and it is apparent that the described embodiments are only some embodiments of the specification, but not all embodiments, and other embodiments obtained by those skilled in the art without making creative efforts based on the one or more embodiments of the specification should fall within the scope of protection of the embodiments of the present specification.
Example 1: pure diesel oil, super heavy oil and surfactant are mixed simultaneously
(1) Introducing 2.5ml of octyl phenol polyoxyethylene ether-10 into deionized water, stirring at 20-30 ℃ at the stirring speed of 500r/min, uniformly stirring for 10min, and standing for 5h until the surfactant is completely dissolved in water;
(2) Setting the mass ratio of diesel oil to super heavy oil to be 1.5:1, taking 45ml of pure diesel oil and 30ml of super heavy oil, 175ml of octyl phenol polyoxyethylene ether-10 solution, setting the oil-water ratio to be 3:7, simultaneously placing the mixture into a 500ml beaker, and standing the mixture in a water bath constant temperature tank for 15min, and then starting stirring. Stirring the mixture by using an HJ-5 multifunctional stirrer at a stirring speed of 1500r/min for 20min at a constant temperature of 55 ℃.
Example 2: pure diesel oil and super heavy oil are mixed with a surfactant after being diluted (1.5:1)
(1) Introducing 2.5ml of octyl phenol polyoxyethylene ether-10 into deionized water, stirring at 20-30 ℃ at the stirring speed of 500r/min, uniformly stirring for 10min, and standing for 5h until the surfactant is completely dissolved in water;
(2) Setting the mass ratio of diesel oil to super-thick oil to be 1.5:1, taking 45ml of pure diesel oil and 30ml of super-thick oil, placing the two in a 500ml beaker, standing for 15min in a water bath constant temperature tank, and stirring a diesel oil super-thick oil mixed system by using an HJ-5 multifunctional stirrer at the stirring speed of 1500r/min for 10min at the constant temperature of 55 ℃;
(3) 175ml of 0.5% octyl phenol polyoxyethylene ether-10 solution is added into a mixed system of diesel oil and super thick oil, the oil-water ratio is 3:7, the mixture is kept stand for 10min at the constant temperature of 55 ℃, and is stirred by an HJ-5 multifunctional stirrer at the stirring rotating speed of 1500r/min for 20min.
Example 3: mixing polymer diesel oil and super heavy oil with surfactant after mixing with thin (0.5:1)
(1) Introducing 2.5ml of octyl phenol polyoxyethylene ether-10 into deionized water, stirring at 20-30 ℃ at the stirring speed of 500r/min, uniformly stirring for 10min, and standing for 5h until the surfactant is completely dissolved in water;
(2) Setting the mass ratio of diesel oil to super heavy oil to be 0.5:1, taking a polymer which is oil-soluble poly alpha olefin, preparing a polymer diesel oil solution with the concentration range of 60-1000 ppm, standing for 3 days, taking 30ml after the polymer is completely dissolved in pure diesel oil, taking 60ml of super heavy oil, placing the two in a 500ml beaker, standing in a water bath constant temperature tank for 15min, stirring a diesel oil super heavy oil mixed system by using an HJ-5 multifunctional stirrer, wherein the stirring speed is 1500r/min, the stirring time is 10min, and the constant temperature is 55 ℃;
(3) 210ml of 0.5% octyl phenol polyoxyethylene ether-10 solution is added into a mixed system of polymer diesel oil and super heavy oil, the oil-water ratio is 3:7, the mixture is kept stand for 10min at the constant temperature of 55 ℃, and is stirred by an HJ-5 multifunctional stirrer, the stirring rotating speed is 1500r/min, and the stirring time is 20min.
Example 4: pure diesel oil and super heavy oil are mixed with a surfactant after being diluted (0.5:1)
(1) Introducing 2.5ml of octyl phenol polyoxyethylene ether-10 into deionized water, stirring at 20-30 ℃ at the stirring speed of 500r/min, uniformly stirring for 10min, and standing for 5h until the surfactant is completely dissolved in water;
(2) Setting the mass ratio of diesel oil to super-thick oil to be 0.5:1, taking 30ml of pure diesel oil and 60ml of super-thick oil, placing the two in a 500ml beaker, standing for 15min in a water bath constant temperature tank, and stirring a diesel oil super-thick oil mixed system by using an HJ-5 multifunctional stirrer at the stirring speed of 1500r/min for 10min at the constant temperature of 55 ℃;
(3) 210ml of 0.5% octyl phenol polyoxyethylene ether-10 solution by mass fraction is added into a mixed system of diesel oil and super heavy oil, and the mixture is kept stand for 10min at the constant temperature of 55 ℃, stirred by a HJ-5 multifunctional stirrer at the stirring rotating speed of 1500r/min for 20min.
Performance testing
For each of the above examples, the viscosity reducing effect of the emulsion viscosity reducing microemulsion prepared in each example was evaluated by using an Anton Par MCR302 rotational rheometer (coaxial cylinder system) manufactured by austria An Dongpa company, the experimental condition being temperatureT=40℃，γ=5s -1 . The viscosity-reducing effect of the prepared emulsion viscosity-reducing microemulsion can be evaluated by using the viscosity-reducing rate, and the calculation expression is as follows:R VR =((μ 0 -μ)/μ)×100%。
wherein:R VR for the viscosity reduction rate,%;μ o is viscosity of super thick oil at 40 ℃ and mPa ∙ s;μthe viscosity is measured for the ultra-thick oil emulsifying viscosity-reducing microemulsion at 40 ℃ and mPa ∙ s.
The evaluation data of the viscosity-reducing effect of the emulsion-reducing microemulsion of each example are shown in FIG. 2.
(1) The test and experiment results in the example 1 show that the good emulsified viscosity-reducing microemulsion cannot be formed, and the rest part of the super-thick oil is attached to the bottom of the beaker;
(2) The test and experiment result of the embodiment 2 shows that the emulsion viscosity-reducing microemulsion can be formed, and the viscosity of the super-thick oil obtained by the viscosity shearing experiment at 40 ℃ is 6040 mPa ∙ s, and the viscosity-reducing efficiency is 98.20%;
(3) The test and experiment result of the embodiment 3 shows that the emulsion viscosity-reducing microemulsion can be well formed, and the viscosity of the super-thick oil obtained by the viscosity-cutting experiment at 40 ℃ is 1015mPa ∙ s, the viscosity-reducing effect is good, and the viscosity-reducing efficiency is 99.71%;
(4) The test and experiment result in example 4 shows that the emulsion viscosity-reducing microemulsion can be well formed, and the viscosity of the super-thick oil obtained by the viscosity shearing experiment at 40 ℃ is 658mPa ∙ s, the viscosity-reducing efficiency is 99.81%, and the viscosity-reducing effect is good.
Product characterization
1. Macroscopic viscosity temperature test for super heavy oil
An Anton Par MCR302 rotational rheometer (flat plate rotor system, flat plate rotor radius) manufactured by austria An Dongpa companyR=12.50 mm), at shear rateγ=5s -1 Temperature (temperature)TTest the corresponding shear stress of super-thick oil at different temperatures under the condition of being in range of 40-100 ℃ (temperature rise) and 3 ℃/minτAnd shear viscosityη p (T) As shown in fig. 3.
2. Super viscous oil macroscopic viscosity shear test
An Anton Par MCR302 rotational rheometer (coaxial cylinder system, inside radiusr i = 13.327mm, rotary test die radiusr e Die height = 14.450mmI= 40.008 mm), as shown in fig. 4, at shear viscosity ofγ=0.1~800s -1 Temperature (temperature)TTest at 100 ℃ to obtain the shear stress corresponding to the super thick oilτAnd shear viscosityη s (γ) The viscosity-shear test temperature is 100 ℃ because the viscosity of the super-thick oil is extremely high at 40 ℃, 352000mPa ∙ s, and the test is not feasible by adopting a coaxial cylinder system, but the super-thick oil viscosity-shear curve at 100 ℃ can be obviously observed to show typical non-Newtonian fluid characteristics and has pseudoplasticity.
3. Microscopic observation test of emulsified viscosity-reducing microemulsion
Microscopic morphology observation was performed on the prepared emulsified viscosity-reduced microemulsion droplets by using a DM2700P polarized electron microscope (195 achromatic objective lens 4×, 10×, 20×, 40×, 100×, eyepiece 10×, LED light source automatically adjustable) from the company of the come instruments, germany, the magnification was 40 times, the microemulsion was observed to be an oil-in-water emulsion, and the microscopic observation result of the microemulsion was shown in fig. 5, and the particle size range of the microemulsion was 100 to 150 μm.
4. Evaluation of viscosity reduction of ultra-thick oil emulsification
An Anton Par MCR302 rotational rheometer (coaxial cylinder system, inside radiusr i = 13.327mm, rotary test die radiusr e Die height = 14.450mmI= 40.008 mm) at shear viscosity ofγ=0.1~1000s -1 Temperature (temperature)TTesting at the temperature of 40 ℃ to obtain the corresponding shear stress of the ultra-thick oil emulsified viscosity-reducing microemulsion at different shear ratesτAnd shear viscosityη e (γ) (as shown in FIG. 6), the viscosity-reducing effect can be evaluated by the viscosity-reducing rateR VR The experimental data results are shown in fig. 2.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (3)
1. The preparation method of the ultra-thick oil emulsified viscosity-reducing microemulsion is characterized by comprising the following specific steps of:
(1) Adding quantitative diesel oil and super-thick oil into a beaker, wherein the mass ratio of the diesel oil to the super-thick oil is (0.3-0.5): 1, standing for 15min at a temperature of 55 ℃ under a temperature control condition, and stirring for 20min under a condition of 1200-1500 r/min by using a stirrer to obtain diluted thick oil;
(2) Adding deionized water and quantitative octyl phenol polyoxyethylene ether-10 into another beaker, wherein the mass fraction of the octyl phenol polyoxyethylene ether-10 solution is 0.5%, uniformly stirring at 20-30 ℃ and stirring speed of 400-800 r/min, and standing for 5 hours until the surfactant is completely dissolved in water to obtain an octyl phenol polyoxyethylene ether-10 aqueous solution;
(3) Adding the prepared octyl phenol polyoxyethylene ether-10 solution into a mixed system of diesel and super-thick oil, wherein the mixed oil-water ratio of the mixed system of diesel and super-thick oil and the 0.5 percent octyl phenol polyoxyethylene ether-10 solution is 3:7, and stirring for 20min under the conditions of constant temperature 55 ℃ and stirring rotation speed of 1200-1500 r/min to obtain the emulsified viscosity-reducing microemulsion.
2. The method for preparing the ultra-thick oil emulsion viscosity-reducing microemulsion according to claim 1, wherein the particle size of the ultra-thick oil emulsion viscosity-reducing microemulsion is 100-150 μm.
3. The method for preparing the ultra-thick oil emulsified viscosity-reducing microemulsion according to claim 1, wherein the ultra-thick oil emulsified viscosity-reducing microemulsion is at a temperature ofT=40℃，γ=0.1~1000s -1 The viscosity is reduced to 658mPa ∙ s, and the viscosity reduction rate is as high as 99.81%.
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