NL2026222B1 - Method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide - Google Patents

Method for preparing ultrafine nanopartical used in tight reservoir for drying agent containing ionic metal carbide Download PDF

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NL2026222B1
NL2026222B1 NL2026222A NL2026222A NL2026222B1 NL 2026222 B1 NL2026222 B1 NL 2026222B1 NL 2026222 A NL2026222 A NL 2026222A NL 2026222 A NL2026222 A NL 2026222A NL 2026222 B1 NL2026222 B1 NL 2026222B1
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carbon dioxide
metal carbide
ionic metal
pressure
reaction vessel
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Xiong Yu
Zhang Liehui
Fu Xitong
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Univ Southwest Petroleum
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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02—Well-drilling compositions
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
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    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

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 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 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 ultra?ne ionic metal carbide nanoparticle.

Description

METHOD OF PREPARING ULTRAFINE NANOPARTICLE USED IN TIGHT RESERVOIR FOR DRYING AGENT CONTAINING IONIC METAL CARBIDE
TECHNICAL FIELD The present invention relates to the technical field of ultrafine nanoparticle preparation, and in particular to a method for preparing ultrafine nanoparticle 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 nanoparticles 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 nanoparticles cannot be made by the prior art. Therefore, it is particularly necessary to develop a method for preparing drying agent nanoparticles.
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 nanoparticle 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 nanoparticle 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 nanoparticles; collecting the nanoparticles on a collector plate through gravitational sedimentation.
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 carbideis 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 nanoparticles condensed from the supercritical carbon dioxide; settling the nanoparticles 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 nanoparticles 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 nanoparticle.
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 nanoparticles obtained by the present invention using scanning electron microscopy (SEM); FIG. 3 illustrates a characterization test for nanoparticles obtained by the present invention using transmission electron microscopy (TEM); FIG. 4 shows an energy dispersive spectrum (EDS) of nanoparticles obtained by the present invention; FIG. 5 illustrates a characterization test for nanoparticles 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 nanoparticle 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 nanoparticles; settling and collecting aluminum carbide nanoparticles 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 nanoparticle 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 nanoparticles; collecting the nanoparticles on a collector plate through gravitational sedimentation.
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 nanoparticles obtained by the present invention using SEM; FIG. 3 illustrates a characterization test for nanoparticles obtained by the present invention using TEM; FIG. 4 shows an energy dispersive spectrum of nanoparticles obtained by the present invention; FIG. 5 illustrates a characterization test for nanoparticles 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 nanoparticle 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 nanoparticles; collecting the nanoparticles on a collector plate through gravitational sedimentation. .
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 nanoparticle 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 nanoparticles; collecting the nanoparticles on a collector plate through gravitational sedimentation.
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 nanoparticle 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 nanoparticles; collecting the nanoparticles on a collector plate through gravitational sedimentation.
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.

Claims (7)

- 10 - NL2026222 Conclusies- 10 - NL2026222 Conclusions 1. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat 1onisch metaalcarbide bevat, waarbij de werkwijze de volgende stappen omvat: (1) het toevoegen van absolute alcohol en ionisch metaalcarbide in een reactieketel met hoge temperatuur en hoge druk; (2) na het strak afsluiten van de reactieketel, het injecteren van koolstofdioxide vanuit een injectiepoort van de reactieketel, en het afsluiten van de injectiepoort van de reactieketel tot de temperatuur en de druk van de reactieketel een superkritischekoolstofdioxidetoestand bereiken en/of overschrijden; (3) het openen van een uitlaat die in verbinding staat met een ultrasone verstuiver van de reactieketel, het door de ultrasone verstuiver sturen van materialen die in superkritisch koolstofdioxide opgelost zijn, en het verlagen van druk om nanodeeltjes te condenseren; het verzamelen van nanodeeltjes op een verzamelplaat middels zwaartekrachtsedimentatie.A method for preparing an ultrafine nanoparticle used in a dense reservoir 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 vessel and high pressure; (2) after tightly sealing the reaction vessel, injecting carbon dioxide from an injection port of the reaction vessel, and closing the injection port of the reaction vessel until the temperature and pressure of the reaction vessel reach and/or exceed a supercritical carbon dioxide state; (3) opening an outlet communicating with an ultrasonic nebulizer of the reaction vessel, passing materials dissolved in supercritical carbon dioxide through the ultrasonic nebulizer, and decreasing pressure to condense nanoparticles; collecting nanoparticles on a collection plate by means of gravity sedimentation. 2. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat ionisch metaalcarbide bevat volgens conclusie 1, waarbij een massaverhouding van de absolute alcohol tot het ionische metaalcarbide in stap (1) 1:30 is.The method for preparing an ultrafine nanoparticle used in a dense reservoir 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. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat ionisch metaalcarbide bevat volgens conclusie 1, waarbij stap (1) verder een droogmiddelversneller omvat die gebruikt wordt in combinatie met het ionische metaalcarbide, en een molverhouding van de droogmiddelversneller tot het ionische metaalcarbide 1 : 2 is.The method for preparing an ultrafine nanoparticle 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 of the desiccant accelerator until the ionic metal carbide is 1:2. 4. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat ionisch metaalcarbide bevat volgens conclusie 1, waarbij het ionische metaalcarbide aluminiumcarbide, calciumcarbide, lithiumcarbide of natriumacetylide is.The method for preparing an ultrafine nanoparticle used in a dense reservoir for a desiccant containing ionic metal carbide according to claim 1, wherein the ionic metal carbide is aluminum carbide, calcium carbide, lithium carbide or sodium acetylide. -11- NL2026222-11- NL2026222 5. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat ionisch metaalcarbide bevat volgens conclusie 1, waarbij de droogmiddelversneller in stap (1) natriumethoxide is.The method for preparing an ultrafine nanoparticle to be used in a dense reservoir for a desiccant containing ionic metal carbide according to claim 1, wherein the desiccant accelerator in step (1) is sodium ethoxide. 6. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat ionisch metaalcarbide bevat volgens conclusie 1, waarbij stap (2) specifiek de volgende stappen omvat: het injecteren van koolstofdioxide vanuit de injectiepoort van de reactieketel, het onder druk zetten van koolstofdioxide met een versterkerpomp, het toelaten dat de druk van de koolstofdioxide die geïnjecteerd wordt een kritische druk van de koolstofdioxide van 7 MPa overschrijdt, het stoppen met koolstofdioxide-injectie tot het versterken tot 15 MPa, en het afsluiten van de injectiepoort van de reactieketel, het aanzetten van een verwarmer van de reactieketel tijdens het injecteren van koolstofdioxide, en het aanpassen van de temperatuur boven de kritische druk van de koolstofdioxide, dat wil zeggen tot 60°C; het beginnen te roeren met een balancerende rotor die in de reactieketel geplaatst is om materialen wederzijds beter oplosbaar te maken met superkritisch koolstofdioxide tot de druk en temperatuur gewenste voorwaarden bereiken.The method of preparing an ultrafine nanoparticle used 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 vessel, pressurizing carbon dioxide with a booster pump, allowing the pressure of the carbon dioxide injected to exceed a critical carbon dioxide pressure of 7 MPa, stopping carbon dioxide injection until boosting to 15 MPa, and shutting off the injection port of the reaction vessel, turning on a heater of the reaction vessel while injecting carbon dioxide, and adjusting the temperature above the critical pressure of the carbon dioxide, i.e. to 60°C; starting agitation with a balancing rotor placed in the reaction vessel to make materials more mutually soluble with supercritical carbon dioxide until the pressure and temperature reach desired conditions. 7. Werkwijze voor het bereiden van een ultrafijn nanodeeltje dat gebruikt wordt in een dicht reservoir voor een droogmiddel dat ionisch metaalcarbide bevat volgens conclusie 1, waarbij stap (3) specifiek de volgende stappen omvat: het verwarmen tot 90°C, het openen van de uitlaat van de reactieketel, waarbij de ultrasone verstuiver nanodeeltjes uitzendt die uit de superkritische koolstofdioxide gecondenseerd zijn; het schikken van de nanodeeltjes op een deeltjesverzamelplaat; het afsluiten van de uitlaat en het stoppen met uitzenden wanneer de druk daalt naar de kritische druk van de koolstofdioxide (7 MPa) in de reactieketel.The method of preparing an ultrafine nanoparticle used in a dense reservoir 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 said outlet of the reaction vessel, wherein the ultrasonic atomizer emits nanoparticles condensed from the supercritical carbon dioxide; arranging the nanoparticles on a particle collection plate; shutting off the outlet and stopping emitting when the pressure drops to the critical pressure of the carbon dioxide (7 MPa) in the reaction vessel.
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