CN111303855A - Nano emulsion miscible oil displacement agent and preparation method thereof - Google Patents
Nano emulsion miscible oil displacement agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano emulsion mixed phase oil displacement agent and a manufacturing method thereof, wherein the oil displacement agent comprises the following components in percentage by weight: 20-30% of gemini surfactant, 10-25% of solubilizer, 15-20% of mutual solvent and 25-55% of water phase; the gemini surfactant is dialkyl phenol ketone polyoxyethylene ether; the manufacturing method comprises the following steps: adding a gemini surfactant, a solubilizer and a mutual solvent into a reactor; mixing uniformly, heating to keep the temperature in the reactor within 60-70 ℃, and then adding water; and reacting for 1-2 hours under stirring to obtain the nano emulsion miscible phase oil displacement agent. The nano emulsion miscible phase oil displacement agent has good mutual solubility, diffusion and emulsification performance, can strip residual oil adsorbed on a rock core, can obviously reduce the oil-water interfacial tension, and improves the oil displacement efficiency.
Description
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a nano emulsion miscible phase oil displacement agent and a manufacturing method thereof.
Background
The main problems faced by oil fields in the middle and later stages of water injection development are that the efficiency of the measures for increasing production and injection, which are widely applied under the original water injection condition, is lower and lower, the technical difficulty is higher and higher, the oil production of production wells is reduced, the water content is greatly increased, and the economic benefit is poorer and poorer. The main oil fields in China all enter the middle and high water-cut period, and the technology for improving the water injection recovery ratio becomes the key of the middle and later periods of water injection development of old oil fields.
Chemical oil displacement is one of effective methods for improving recovery efficiency, and mainly comprises polymer flooding, surfactant flooding, alkali flooding and the like. The surfactant flooding can reduce the oil-water interfacial tension, has good emulsifying capacity, can drive residual oil of a stratum to improve the oil washing efficiency, and has great potential. The nano emulsion miscible oil displacement agent is a new mode of adding a displacement fluid prepared by adding a low-concentration nano emulsion miscible oil displacement agent into injection water, injecting the displacement fluid into a reservoir, and spontaneously emulsifying and eroding formation crude oil, particularly residual oil to realize oil displacement.
In addition, the proportion of unconventional energy oil gas in the energy pattern is increased year by year. The development of unconventional energy oil and gas in China is also in progress as well as fierce. Shale oil gas reserves in China are huge, and fracturing modification is a necessary link for development and production of shale oil gas wells. However, a large amount of fracturing fluid is introduced into a shale stratum during fracturing modification, due to the characteristic of low porosity and low permeability of the shale stratum, the problem of liquid phase retention of the fracturing fluid is serious, and the liquid retained in pores, clefts and cracks of coal and rock can block desorption of shale oil gas and migration of gas, so that the relative permeability of the oil gas is reduced, and the fractured and modified well even has a production reduction phenomenon. At present, the problem of flowback is solved mainly by reducing the interfacial tension by a surfactant, but the flowback rate is low and is basically below 50%.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a nano emulsion miscible oil displacement agent and a manufacturing method thereof, which can strip residual oil adsorbed on a core by using the oil displacement agent, and can significantly reduce the oil-water interfacial tension, improve the oil displacement efficiency and improve the flowback rate.
The technical scheme of the invention is as follows:
on the one hand, a nano emulsion mixed phase oil displacement agent is provided, and the oil displacement agent comprises the following components in percentage by weight: 20-30% of gemini surfactant, 10-25% of solubilizer, 15-20% of mutual solvent and 25-55% of water phase; the gemini surfactant is dialkyl phenol ketone polyoxyethylene ether.
Preferably, the structural formula of the dialkyl phenol ketone polyoxyethylene ether is as follows:
in the formula: m is 4,6,8,10, 12; n is 2, 4.
Preferably, the solubilizer is an alcohol.
Preferably, the alcohol is of the formula: CH (CH)3(CH2)iOH; wherein i is any natural number from 0 to 4.
Preferably, the mutual solvent is one or more of dihydrojasmone, limonene, dipentadiene and ethylene glycol monobutyl ether.
Preferably, the emulsion peak particle size of the oil displacement agent is within the range of 20-100 nm.
On the other hand, the preparation method of the nano emulsion mixed phase oil displacement agent comprises the following steps: adding a gemini surfactant, a solubilizer and a mutual solvent into a reactor; mixing uniformly, heating to keep the temperature in the reactor within 60-70 ℃, and then adding water; and reacting for 1-2 hours under stirring to obtain the nano emulsion miscible phase oil displacement agent.
Compared with the prior art, the invention has the following advantages:
the nano emulsion miscible phase oil displacement agent has good mutual solubility, diffusion and emulsification performance, can strip residual oil adsorbed on a rock core, can obviously reduce the oil-water interfacial tension, and improves the oil displacement efficiency. In addition, a gravity drive flowback experiment shows that the nanoemulsion miscible phase oil displacement agent has flowback efficiency improved by more than 40% compared with the formation water, and is improved by more than 30% compared with the conventional surfactant; the nano emulsion has good compatibility with a slickwater system; core damage tests show that the core damage rate of the nano emulsion is less than 5%, is reduced by about 40% compared with formation water, and is lower.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a pre-XY-1 well intervention production curve from example 5;
FIG. 2 is a production curve after the XY-1 well procedure of example 5.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. It should be noted that, in the present application, the embodiments and the technical features of the embodiments may be combined with each other without conflict. Unless defined otherwise, technical or scientific terms used in the present disclosure should have the ordinary meaning as understood by those of ordinary skill in the art to which the present disclosure belongs. The use of the terms "comprising" or "including" and the like in the disclosure of the present invention means that the element or item appearing before the term covers the element or item listed after the term and its equivalents, without excluding other elements or items. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
[ example 1 ]
Preparing the dialkyl phenol ketone polyoxyethylene ether: adding a certain amount of reaction raw materials (bisphenol ketone) into a high-pressure reaction kettle; and then grinding potassium hydroxide serving as a catalyst, and adding the ground potassium hydroxide into the high-pressure reaction kettle, wherein the dosage of the potassium hydroxide is 3-4 per mill of the output of the discharged product. The autoclave is sealed, fixed, mounted on a heating device, optionally open heated with an oil bath. The metering tank was charged with ethylene oxide to a prescribed amount, the feed rate during the reaction was based on the rate of decrease of the liquid level in the metering tank, and the feed amount was calculated from the lattice number difference of the liquid level in the metering tank before and after the reaction. Replacing three times by using nitrogen, heating to raise the temperature to initiate reaction, after the temperature reaches the initiation temperature, adding ethylene oxide to the pressure of 0.4-0.5 MPa, stopping adding the ethylene oxide, continuing raising the temperature, reducing the pressure to about 0.1MPa, and controlling the temperature to be 120-140 ℃ until the ethylene oxide is completely added. After the addition of ethylene oxide, the mixture was aged to a pressure of 0MPa and slowly cooled to room temperature. Discharging, and neutralizing potassium hydroxide with glacial acetic acid until the pH value is about 7 to obtain the dialkyl phenol ketone polyoxyethylene ether product.
[ example 2 ]
Preparing the nano emulsion mixed phase oil displacement agent: adding 30% of dialkyl phenol ketone polyoxyethylene ether (m is 8, n is 2), 15% of solubilizer isopropanol and 20% of mutual solvent ethylene glycol monobutyl ether into a reactor; mixing uniformly, heating to keep the temperature in the reactor at 60-70 ℃, and then adding 35% of distilled water; the reaction was carried out for 1 to 2 hours with stirring to obtain a pale yellow transparent liquid sample 1. The sample 1 was subjected to the performance test, and the results are shown in table 1:
table 1 sample 1 performance test results
| Item | Index (I) |
| Density (20 ℃ +/-1 ℃) and g/cm3 | 1.02 |
| pH value | 7.0 |
| Surface tension (0.1% add), mN/m | 24.3 |
| Interfacial tension (0.1% addition with kerosene) mN/m | 0.0046 |
| The degree of emulsification,%) | 89.1 |
| Static imbibition displacement rate,% | 15.6 |
| Dynamic oil displacement rate% | 24.8 |
| Core damage rate% | 4.87 |
[ example 3 ]
Preparing the nano emulsion mixed phase oil displacement agent: adding 30% of dialkyl phenol ketone polyoxyethylene ether (m is 10, n is 2), 10% of n-butyl alcohol serving as a solubilizer and 20% of limonene serving as a mutual solvent into a reactor; mixing evenly, heating to keep the temperature in the reactor at 60-70 ℃, then adding 50% of distilled water, and reacting for 1-2 hours under stirring to obtain a light yellow transparent liquid sample 2. The sample 2 was subjected to the performance test, and the results are shown in table 2:
table 2 sample 2 performance test results
| Item | Index (I) |
| Density (20 ℃ +/-1 ℃) and g/cm3 | 1.03 |
| pH value | 7.0 |
| Surface tension (0.1% add), mN/m | 23.8 |
| Interfacial tension (0.1% addition, with kerosene) mN/m | 0.0018 |
| The degree of emulsification,%) | 93.1 |
| Static imbibition displacement rate,% | 16.9 |
| Dynamic oil displacement rate% | 25.4 |
| Core damage rate% | 4.21 |
[ example 4 ]
Trial production is carried out on the nano emulsion mixed phase oil displacement agent in 2017, pilot tests are carried out on the site, and the site implementation specifically comprises the following steps: injecting the nano emulsion miscible phase oil displacement agent aqueous solution (with the concentration of 0.2%) into a well at 3 mouths of an M28-1 block from 1 month in 2017 to 11 months in 2017, and recovering water injection at 12 months and 16 days in 2018. The oil increasing and water reducing effects during the test are obvious: the cumulative oil increase 21364t shows that the actual recovery ratio is improved by 4.73 percent, the water content reaches 71.7 percent in the peak time with effect, the water content is reduced by 22.6 percent compared with that before the test, the average daily oil reaches 58t in the peak time with effect, the average daily oil level is 47.9t, the water content is increased by 29.8t compared with that before the test, and the cumulative oil increase 21364t and the average single-well oil increase 4670t are carried out in 12 months in 2019. The input-output ratio reaches 1: 3.
the oil displacement principle of the nano emulsion miscible phase oil displacement agent is as follows:
1) the method reduces the oil-water interfacial tension mechanism, reduces the interfacial tension between the displacement fluid and the formation crude oil, leads to easy deformation and displacement of residual oil films and oil droplets, reduces the work WE required for stripping the residual oil from rocks in the form of oil droplets, and reduces the work required for interfacial deformation when the oil droplets pass through throats of porous media, according to the thermodynamic principle, WE is 2 бo/w(бo/wOil-water interfacial tension) of бo/wIs 35mJ/m2Then, the peeling area is 1m2The energy required to emulsify the oil is 70mJ, which is a large value. If the nano emulsion mixed phase oil displacement agent is used, the oil-water interfacial tension is reduced to 0.0025mJ/m2WE is 0.005mJ, which is reduced to 1/10000, so that the residual oil is easy to emulsify and peel, and oil drops are easy to deform and enrich, which is different from the traditional concept WA б related to work of adhesion in the process of extracting residual oilo/w(1-cos θ), θ is the wetting angle, and is also different from the concept in oil recovery theory regarding the relationship of residual oil to capillary force.
2) The mechanism of mutual solubility diffusion. The nano emulsion miscible phase oil displacement agent has stronger capability of diffusing to the crude oil phase, thereby leading the oil and water to form a miscible phase. Under the action of the emulsifier, emulsion is formed spontaneously, and residual oil adsorbed on the rock core is stripped continuously, so that the oil washing efficiency is improved. The experimental study shows that: the microstructure of the nano emulsion miscible phase oil displacement agent is important for an interfacial tension value, a solubilization degree, fluidity, adsorption and the like, the strength of the diffusion capacity of the nano emulsion miscible phase oil displacement agent to a crude oil phase is determined by the molecular structure and the crude oil composition, the diffusion capacity of the nano emulsion miscible phase oil displacement agent is greater than that of a conventional surfactant, the concentration of the nano emulsion miscible phase oil displacement agent is higher, more spontaneous emulsion is formed, the coalescence of the formed emulsion is faster, and a continuous crude oil enrichment zone is formed. And the combination of the crude oil enrichment zones forms an oil wall, and because the oil wall exists in a lower active agent concentration environment, the viscosity and the resistance of a flowing system are reduced, so that the continuity of the oil wall is maintained and the oil wall is not broken and trapped again, the extraction of crude oil is facilitated, and the recovery ratio is improved.
3) The spontaneous emulsification mechanism. In the much lower range of σ c, the residual oil can be driven. During flooding, the formation of residual oil lumps depends on the pressure gradient, the oil-water interfacial tension, the pore geometry, and also on the properties of the interfacial film. When water invades the porous rock, a transition zone of oil-water is formed, wherein the increase of oil saturation causes the fracture of continuous oil line, the action of low interfacial tension on the movement of a trapped oil drop through a narrow orifice neck is beneficial to the oil drop combination to form the form of oil wall, and the advancement of the oil wall and the surfactant concentration as low as possible keep the continuity of the oil line without being broken and trapped again.
After the nano emulsion miscible phase oil displacement agent disclosed by the invention is used for displacing oil, the physical properties of the crude oil are changed, the viscosity, the initial boiling point and the heavy component content in the four components of the crude oil are increased, and the fraction at 300 ℃ is reduced. The viscosity of the crude oil rises from 1972mPa.s to 3293mPa.s, and the heavy component is increased by 7.14 percent; the initial boiling point was increased from 187 ℃ to 234 ℃ before the test, and the 300 ℃ fraction was decreased by 1% from that before the test. The theory is consistent with the oil displacement theory of the nano emulsion miscible oil displacement agent, and shows that the nano emulsion miscible oil displacement agent can strip and drive residual oil with high surface viscosity of rocks in the oil displacement process, and has a strong oil washing effect.
[ example 5 ]
And (3) field implementation: as shown in fig. 1-2, XY-1 well was put into production by fracturing in 2013 in 10 months, P2w (3513.5-3560.0m) was shot, and the shot thickness was 13.0 m; 8.3t of the initial daily liquid, 8.0t of the daily oil and 3.8 percent of water; production is started in 2015 9 months; and no production is shut in before the measure. The well geological reserve is 4.05 x 104t, cumulative oil 2516.4t, 6.2% recovery. The well P2w (3513.5-3560.0m) is repeatedly fractured by adopting a process of adding a pre-nano emulsion miscible phase oil displacement agent and slickwater in 2019, 6 months and 2 days, 1400 parts of the nanometer slickwater is injected, the formula is 0.2 percent of the nano emulsion miscible phase oil displacement agent, 0.1 percent of the drag reducer and the flowback fluid, and the yield-increasing effect after the fracturing is obvious. The oil production of the well before the measure is 0, the daily yield after the measure is 9.7 tons, and the oil is increased by 1269 tons cumulatively.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A nano emulsion mixed phase oil displacement agent is characterized by comprising the following components in percentage by weight: 20-30% of gemini surfactant, 10-25% of solubilizer, 15-20% of mutual solvent and 25-55% of water phase; the gemini surfactant is dialkyl phenol ketone polyoxyethylene ether.
2. The nanoemulsion miscible oil displacement agent according to claim 1, wherein the structural formula of the bisalkylphenol ketone polyoxyethylene ether is as follows:
in the formula: m is 4,6,8,10, 12; n is 2, 4.
3. The nanoemulsion miscible oil displacement agent according to claim 1, wherein the solubilizer is an alcohol.
4. The nanoemulsion miscible oil displacement agent according to claim 3, wherein the alcohol has the following structural formula: CH (CH)3(CH2)iOH; wherein i is any natural number from 0 to 4.
5. The nanoemulsion mixed-phase oil displacement agent according to claim 1, wherein the mutual solvent is one or more of dihydrojasmone, limonene, dipentadiene and ethylene glycol monobutyl ether.
6. The nano emulsion miscible oil displacement agent according to claim 1, wherein the oil displacement agent has an emulsion peak particle size within a range of 20 to 100 nm.
7. The preparation method of the nano-emulsion mixed-phase oil displacement agent as claimed in any one of claims 1 to 6, characterized by comprising the following steps: adding a gemini surfactant, a solubilizer and a mutual solvent into a reactor; mixing uniformly, heating to keep the temperature in the reactor within 60-70 ℃, and then adding water; and reacting for 1-2 hours under stirring to obtain the nano emulsion miscible phase oil displacement agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116589995A (en) * | 2022-12-28 | 2023-08-15 | 陕西邦达诺环保科技有限公司 | Multi-type-nonionic oil film stripping agent and preparation method thereof |
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| CN1352224A (en) * | 2001-09-19 | 2002-06-05 | 西安长奇通讯化工科技有限公司 | High efficiency oil-displacing agent |
| CN104830301A (en) * | 2015-04-13 | 2015-08-12 | 山东大学 | Vesicle oil displacement agent formed from gemini surfactant, and applications of vesicle oil displacement agent in crude oil recovery rate increase |
| CN107663449A (en) * | 2016-07-28 | 2018-02-06 | 安庆五宁精细化工有限责任公司 | A kind of efficient cleanup additive of nano emulsion type |
| CN110951473A (en) * | 2018-09-27 | 2020-04-03 | 北京市捷博特能源技术有限公司 | Nano-terpene composite oil displacement agent |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1352224A (en) * | 2001-09-19 | 2002-06-05 | 西安长奇通讯化工科技有限公司 | High efficiency oil-displacing agent |
| CN104830301A (en) * | 2015-04-13 | 2015-08-12 | 山东大学 | Vesicle oil displacement agent formed from gemini surfactant, and applications of vesicle oil displacement agent in crude oil recovery rate increase |
| CN107663449A (en) * | 2016-07-28 | 2018-02-06 | 安庆五宁精细化工有限责任公司 | A kind of efficient cleanup additive of nano emulsion type |
| CN110951473A (en) * | 2018-09-27 | 2020-04-03 | 北京市捷博特能源技术有限公司 | Nano-terpene composite oil displacement agent |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116589995A (en) * | 2022-12-28 | 2023-08-15 | 陕西邦达诺环保科技有限公司 | Multi-type-nonionic oil film stripping agent and preparation method thereof |
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Application publication date: 20200619 |