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    • 专利摘要:
    The present invention discloses a method for preparing ultraf1ne nanoparticle used in tight reservoir for drying agent containing ionic metal carbide, including the steps of: (1) adding absolute alcohol and ionic metal carbide into a high temperature/high pressure reaction kettle; (2) injecting carbon dioxide from an injection port of the reaction kettle, and 10 allowing the temperature and pressure of the reaction kettle to reach and/or exceed supercritical state of carbon dioxide; and (3) emitting materials dissolved in supercritical carbon dioxide through an ultrasonic atomizer, reducing pressure to condense nanoparticles, and collecting the nanoparticles on a collector plate through gravitational sedimentation. Drying agent nanoparticles made by the present invention contemplates the effect of a 15 micropore structure of a water-lock tight gas reservoir, solves a difficulty in injecting a drying agent into micropores, improves capacity of injection of a ionic metal carbide-based drying agent into a water-bearing tight gas reservoir, and provides a new method for preparing an ultrafine ionic metal carbide nanoparticle.
    公开号:NL2026222A
    申请号:NL2026222
    申请日:2020-08-05
    公开日:2021-02-16
    发明作者:Xiong Yu；Fu Xitong；Zhang Liehui
    申请人:Univ Southwest Petroleum；
    IPC主号:
    专利说明:

    METHOD OF PREPARING ULTRAFINE NANOPARTICAL USED IN TIGHTRESERVOIR FOR DRYING AGENT CONTAINING IONIC METAL CARBIDE
    TECHNICAL FIELD The present invention relates to the technical field of ultrafine nanopartical preparation, and in particular to a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide.
    BACKGROUND Tight gas reservoir resources are enormous in China, with geological reserves of approximately 22.88 * 10 m*. As an important mainstay of sustainable growth of natural gas in China, tight gas reservoir resources will be a successor for conventional oil and gas resources and one of the leading roles in securing a supply of oil and gas resources to China. However, a tight gas reservoir usually has high original water saturation and causes water-lock damage very easily, leading to low gas phase permeability and high mining costs. Experiments have found that permeability of dry tight gas reservoir core is at least 10 times that of original water-cut core. Therefore, provided that a drying agent is injected into a tight gas reservoir and chemically reacts with formation water to produce gases and heat and thus deplete the water, the water saturation of the tight gas reservoir will be minimized and the water-lock damage to the tight gas reservoir will be relieved to improve the gas seepage capacity. Currently, China Patent No. CN107459981A (DRYING AGENT FOR REDUCING TIGHT RESERVOIR WATER BLOCKING EFFECT) provides a drying agent composed of aluminum carbide (Al4Cs) and sodium acetylide (C2HNa) for drying tight reservoir. However, the tight gas reservoir has small pores and throats, main body of reservoir space thereof is a nanoscale pore-throat system, and pore size distribution ranges from 40 to 700 nm. Therefore, it is necessary to use extremely small Al4C3 and CoHNa nanoparticals to inject into tight reservoir pores, however, under present conditions, ionic metal carbide drying agent AlsCs has a micron-grade particle size, which cannot be effectively injected into nano-pores of the tight reservoir due to excessively large particle size; moreover, drying agent nanoparticals cannot be made by the prior art. Therefore, it is particularly necessary to develop a method for preparing drying agent nanoparticals.SUMMARY
    Particles of ionic metal carbides (as a main drying agent) and drying agents remain micron-sized and cannot be injected into tight reservoir micropores effectively.
    To solve the defect in the prior art, the present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide.
    The method can achieve the following objectives: to obtain nano-sized ionic metal carbides and nano-sized drying agents; to solve a current problem that drying agents cannot be injected into tight reservoir micropores; to improve capacity of injection of a ionic metal carbide-based drying agent into a water-bearing tight gas reservoir; and to expand a broader application scope of ionic metal carbides.
    To achieve the above purpose, the present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide, where the method includes the following steps of: (1) Adding absolute alcohol and ionic metal carbide into a high temperature/high pressure reaction kettle; (2) After sealing the reaction kettle tightly, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and/or exceed supercritical state of carbon dioxide; (3) Opening an outlet connecting to an ultrasonic atomizer of the reaction kettle, emitting materials dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and reducing pressure to condense nanoparticals; settling and collecting nanoparticals on a collector plate arranged below through gravitational differentiation.
    Further, a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) is 1:30. Further, step (1) further includes a drying agent accelerator used in combination with the ionic metal carbide, and a molar ratio of the drying agent accelerator to the ionic metal carbide is (1-2):(1-2). Further, the 1onic metal carbide is aluminum carbide, calcium carbide, lithium carbide, or sodium acetylide.
    Further, the drying agent accelerator in step (1) is sodium ethoxide.
    Further, step (2) specifically includes the following steps: injecting carbon dioxide from the injection port of the reaction kettle, pressurizing the carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide injected to exceed a critical pressure of the carbon dioxide of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and closing the injection port of the reaction kettle; turning on a heater of the reaction kettle while injecting carbon dioxide, and adjusting the temperature above the critical pressure of the carbon dioxide, i.e, up to 60°C; starting stirring with a balancing rotor placed in the reaction kettle to make materials mutually soluble with supercritical carbon dioxide better until the pressure and temperature meet desirable requirements. Further, step (3) specifically includes the following steps: heating to 90°C, opening the outlet of the reaction kettle, where the ultrasonic atomizer emits nanoparticals condensed from the supercritical carbon dioxide; settling the nanoparticals on a particle collector plate; closing the outlet and stopping emitting when the pressure decreases to the critical pressure of the carbon dioxide (7 MPa) in the reaction kettle. The present invention adopts the above technical solution, and includes the following beneficial effects: drying agent nanoparticals made by the present invention contemplates the effect of a micropore structure of a water-lock tight gas reservoir, solves a difficulty in injecting a drying agent into micropores, improves capacity of injection of a ionic metal carbide-based drying agent into a water-bearing tight gas reservoir, and further provides a new method for preparing an ultrafine ionic metal carbide nanopartical.
    BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 schematically illustrates equipment used in the method of the present invention; FIG. 2 illustrates a characterization test for final nanoparticals obtained by the present invention using scanning electron microscopy (SEM); FIG. 3 illustrates a characterization test for nanoparticals obtained by the present invention using transmission electron microscopy (TEM); FIG. 4 shows an energy dispersive spectrum (EDS) of nanoparticals obtained by the present invention; FIG. 5 illustrates a characterization test for nanoparticals obtained by the present invention using X-ray diffraction (XRD).DETAILED DESCRIPTION
    The present invention will be described in detail below with reference to the examples.
    Example 1: The present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide. For example, the ionic metal carbide is aluminum carbide, and the method includes the following steps: (1) Adding absolute alcohol and aluminum carbide into a high temperature/high pressure reaction kettle; (2) After sealing the reaction kettle tightly, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and/or exceed supercritical state of carbon dioxide; (3) Opening an outlet connecting to an ultrasonic atomizer of the reaction kettle, emitting the aluminum carbide dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and reducing pressure to condense aluminum carbide nanoparticals; settling and collecting aluminum carbide nanoparticals on a collector plate arranged below through gravitational differentiation.
    Further, a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) 1s 1:30.
    What the example finally obtains is nano-sized aluminum carbide, which usually serves as a principal component of a drying agent used in tight reservoir, such that the component and other accelerator can be injected into the tight reservoir; because the principal component is nano-sized, it can be injected into tight reservoir micropores better and thus chemically reacts with formation water to produce gases and heat to deplete the water; in this way, the water saturation of the tight gas reservoir will be minimized and the water-lock damage to the tight gas reservoir will be relieved to improve the gas seepage capacity and gas phase permeability and reduce natural gas exploitation costs.
    Example 2: The present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide. For example, the ionic metal carbide 1s aluminum carbide, sodium ethoxide is used as a drying agent additive and a molar ratio of aluminum carbide to sodium ethoxide is 1:2. The method includes the following steps: (1) Adding absolute alcohol, aluminum carbide, and sodium ethoxide into a high
    5 temperature/high pressure reaction kettle, where the aluminum carbide may be micron-sized; (2) After sealing the reaction kettle tightly, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and/or exceed supercritical state of carbon dioxide; (3) Opening an outlet connecting to an ultrasonic atomizer of the reaction kettle, emitting materials dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and reducing pressure to condense nanoparticals; settling and collecting nanoparticals on a collector plate arranged below through gravitational differentiation.
    Specifically, a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) is 1:30.
    Specifically, step (2) includes the following steps: injecting carbon dioxide from the injection port of the reaction kettle, pressurizing the carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide injected to exceed a critical pressure of the carbon dioxide of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and closing the injection port of the reaction kettle; turning on a heater of the reaction kettle while injecting carbon dioxide, and adjusting the temperature above the critical pressure of CO; (e.g., 60°C); starting stirring with a balancing rotor placed in the reaction kettle to make the ionic metal carbide mutually soluble with supercritical carbon dioxide better until the pressure and temperature meet desirable requirements.
    Specifically, step (3) includes the following steps: opening the outlet of the reaction kettle; at the outlet, instantaneously emitting ultrafine particles condensed during depressurization after dissolving aluminum carbide in supercritical carbon dioxide through the ultrasonic atomizer connected via a high pressure resistant pipeline; instantaneously evaporating excess ethanol in a high temperature oven, allowing oven temperature to rise to 90°C, emitting particles condensed from the supercritical carbon dioxide from the ultrasonic atomizer, and settling the particles on a particle collector plate; closing the outlet and stopping emitting after the pressure in the reaction kettle declines to the critical pressure of the carbon dioxide (7 MPa).
    In the present invention, a nano-sized drying agent is made from principal component aluminum carbide and accelerator using the method of the present invention; the particles collected are characterized by SEM, TEM, EDS, and XRD. FIG. 1 illustrates equipment used in the method of the present invention; FIG. 2 illustrates a characterization test for final nanoparticals obtained by the present invention using SEM; FIG. 3 illustrates a characterization test for nanoparticals obtained by the present invention using TEM; FIG. 4 shows an energy dispersive spectrum of nanoparticals obtained by the present invention; FIG. 5 illustrates a characterization test for nanoparticals obtained by the present invention using XRD. The ultrafine particles obtained are determined as a nano-sized drying agent; the material is composed of aluminum, carbon, sodium, and oxygen, and the principal component 1s Al4C3.
    Example 3: The present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide. For example, the ionic metal carbide is calcium carbide, sodium ethoxide is used as a drying agent additive and a molar ratio of calcium carbide to sodium ethoxide is 1:1. The method includes the following steps: (1) Adding absolute alcohol, calcium carbide, and sodium ethoxide into a high temperature/high pressure reaction kettle, where, the calcium carbide may be micron-sized, (2) After sealing the reaction kettle tightly, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and/or exceed supercritical state of carbon dioxide; (3) Opening an outlet connecting to an ultrasonic atomizer of the reaction kettle, emitting materials dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and reducing pressure to condense nanoparticals; settling and collecting nanoparticals on a collector plate arranged below through gravitational differentiation.
    Specifically, a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) is 1:30.
    Specifically, step (2) includes the following steps: injecting carbon dioxide from the injection port of the reaction kettle, pressurizing the carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide injected to exceed a critical pressure of the carbon dioxide of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and closing the injection port of the reaction kettle; turning on a heater of the reaction kettle while injecting carbon dioxide, and adjusting the temperature above the critical pressure of CO: (e.g., 60°C); starting stirring with a balancing rotor placed in the reaction kettle to make the ionic metal carbide mutually soluble with supercritical carbon dioxide better until the pressure and temperature meet desirable requirements.
    Specifically, step (3) includes the following steps: opening the outlet of the reaction kettle; at the outlet, instantaneously emitting ultrafine particles condensed during depressurization after dissolving aluminum carbide in supercritical carbon dioxide from the ultrasonic atomizer connected via a high pressure resistant pipeline; instantaneously evaporating excess ethanol in a high temperature oven, allowing oven temperature to rise to 90°C, emitting particles condensed from the supercritical carbon dioxide from the ultrasonic atomizer, and settling the particles on a particle collector plate; closing the outlet and stopping emitting after the pressure in the reaction kettle declines to the critical pressure of the carbon dioxide (7 MPa).
    Example 4: The present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide. For example, the ionic metal carbide is lithium carbide, sodium ethoxide is used as a drying agent additive and a molar ratio of lithium carbide to sodium ethoxide is 2:1. The method includes the following steps: (1) Adding absolute alcohol, lithium carbide, and sodium ethoxide into a high temperature/high pressure reaction kettle, where the calcium carbide may be micron-sized, (2) After sealing the reaction kettle tightly, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and/or exceed supercritical state of carbon dioxide; (3) Opening an outlet connecting to an ultrasonic atomizer of the reaction kettle, emitting materials dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and reducing pressure to condense nanoparticals; settling and collecting nanoparticals on a collector plate arranged below through gravitational differentiation.
    Specifically, a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) is 1:30.
    Specifically, step (2) includes the following steps: injecting carbon dioxide from the injection port of the reaction kettle, pressurizing the carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide injected to exceed a critical pressure of the carbon dioxide of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and closing the injection port of the reaction kettle, turning on a heater of the reaction kettle while injecting carbon dioxide, and adjusting the temperature above the critical pressure of CO: (e.g., 60°C); starting stirring with a balancing rotor placed in the reaction kettle to make the ionic metal carbide mutually soluble with supercritical carbon dioxide better until the pressure and temperature meet desirable requirements.
    Specifically, step (3) includes the following steps: opening the outlet of the reaction kettle; at the outlet, instantaneously emitting ultrafine particles condensed during depressurization after dissolving aluminum carbide in supercritical carbon dioxide through the ultrasonic atomizer connected via a high pressure resistant pipeline; instantaneously evaporating excess ethanol in a high temperature oven, allowing oven temperature to rise to 90°C, emitting particles condensed from the supercritical carbon dioxide from the ultrasonic atomizer, and settling the particles on a particle collector plate; closing the outlet and stopping emitting after the pressure in the reaction kettle declines to the critical pressure of the carbon dioxide (7 MPa).
    Example 5: The present invention provides a method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide. For example, the ionic metal carbide is sodium acetylide, sodium ethoxide 1s used as a drying agent additive and a molar ratio of sodium acetylide to sodium ethoxide is 1:1. The method includes the following steps: (1) Adding absolute alcohol, sodium acetylide, and sodium ethoxide into a high temperature/high pressure reaction kettle, where the calcium carbide may be micron-sized,; (2) After sealing the reaction kettle tightly, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and/or exceed supercritical state of carbon dioxide; (3) Opening an outlet connecting to an ultrasonic atomizer of the reaction kettle, emitting materials dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and reducing pressure to condense nanoparticals; settling and collecting nanoparticals on a collector plate arranged below through gravitational differentiation.
    Specifically, a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) is 1:30.
    Specifically, step (2) includes the following steps: injecting carbon dioxide from the injection port of the reaction kettle, pressurizing the carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide injected to exceed a critical pressure of the carbon dioxide of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and closing the injection port of the reaction kettle, turning on a heater of the reaction kettle while injecting carbon dioxide, and adjusting the temperature above the critical pressure of CO: (e.g., 60°C); starting stirring with a balancing rotor placed in the reaction kettle to make the ionic metal carbide mutually soluble with supercritical carbon dioxide better until the pressure and temperature meet desirable requirements.
    Specifically, step (3) includes the following steps: opening the outlet of the reaction kettle; at the outlet, instantaneously emitting ultrafine particles condensed during depressurization after dissolving aluminum carbide in supercritical carbon dioxide through the ultrasonic atomizer connected via a high pressure resistant pipeline; instantaneously evaporating excess ethanol in a high temperature oven, allowing oven temperature to rise to 90°C, emitting particles condensed from the supereritical carbon dioxide from the ultrasonic atomizer, and settling the particles on a particle collector plate; closing the outlet and stopping emitting after the pressure in the reaction kettle declines to the critical pressure of the carbon dioxide (7 MPa).
    The above descriptions are merely preferred examples of the present invention, and are not intended to limit the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention. Any modification, equivalent substitution and improvement without departing from the spirit and principle of the present invention shall be included within the protection scope of the present invention.
    权利要求:
    Claims (7)
    [1]
    A method of preparing an ultra-fine nanoparticle to be used in a dense container for a desiccant containing ionic metal carbide, the method comprising the steps of: (1) adding absolute alcohol and ionic metal carbide in a high temperature reaction kettle and high pressure; (2) after tightly closing the reaction kettle, injecting carbon dioxide from an injection port of the reaction kettle, and closing the injection port of the reaction kettle until the temperature and pressure of the reaction kettle reach and / or exceed a supercritical carbon dioxide state; (3) opening an outlet communicating with an ultrasonic atomizer of the reaction kettle, sending materials dissolved in supercritical carbon dioxide through the ultrasonic atomizer, and lowering pressure to condense nanoparticles; arranging and collecting nanoparticles on a collection plate arranged beneath them by means of gravity differentiation.
    [2]
    A method of preparing an ultra-fine nanoparticle for use in a dense container for a desiccant containing ionic metal carbide according to claim 1, wherein a mass ratio of the absolute alcohol to the ionic metal carbide in step (1) is 1:30.
    [3]
    A method of preparing an ultra-fine nanoparticle to be used in a dense reservoir for a desiccant containing ionic metal carbide according to claim 1, wherein step (1) further comprises a desiccant accelerator used in combination with the ionic metal carbide, and a molar ratio from the desiccant accelerator to the ionic metal carbide (1 - 2) :( 1 - 2).
    [4]
    The method of preparing an ultra-fine nanoparticle for use in a dense container for a desiccant containing ionic metal carbide according to claim 1, wherein the ionic metal carbide is aluminum carbide,
    -11- NL2026222 is calcium carbide, lithium carbide or sodium acetylide.
    [5]
    The method of preparing an ultra-fine nanoparticle for use in a dense container for a desiccant containing ionic metal carbide according to claim 1, wherein the desiccant accelerator in step (1) is sodium ethoxide.
    [6]
    The method of preparing an ultrafine nanoparticle for use in a dense reservoir for a desiccant containing ionic metal carbide according to claim 1, wherein step (2) specifically comprises the steps of: injecting carbon dioxide from the injection port of the reaction kettle, pressurizing carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide being injected to exceed a carbon dioxide critical pressure of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and shutting off the injection port of the reaction kettle; turning on a heater of the reaction kettle during the injection of carbon dioxide, and adjusting the temperature above the critical pressure of the carbon dioxide, i.e., up to 60 ° C; starting to stir with a balancing rotor placed in the reaction kettle to make materials more mutually soluble with supercritical carbon dioxide until the pressure and temperature reach desired conditions.
    [7]
    A method of preparing an ultra-fine nanoparticle for use in a dense container for a desiccant containing ionic metal carbide according to claim 1, wherein step (3) specifically comprises the steps of: heating to 90 ° C, opening the reaction kettle outlet, the ultrasonic atomizer emitting nanoparticles condensed from the supercritical carbon dioxide; arranging the nanoparticles on a particle collection plate; shutting off the outlet and stopping emission when the pressure drops to the critical pressure of the carbon dioxide (7 MPa) in the reaction kettle.
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    法律状态:
    优先权:
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