CN116617943A - High-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid and application - Google Patents

High-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid and application Download PDF

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Publication number
CN116617943A
CN116617943A CN202310802593.2A CN202310802593A CN116617943A CN 116617943 A CN116617943 A CN 116617943A CN 202310802593 A CN202310802593 A CN 202310802593A CN 116617943 A CN116617943 A CN 116617943A
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China
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reaction kettle
pressure
temperature
reaction
flexible
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郭海浩
李王晔
祁冬梅
赵育飞
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China University of Geosciences
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China University of Geosciences
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Priority to CN202310802593.2A priority Critical patent/CN116617943A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/002Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention provides a high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid, which comprises a reaction kettle main body and a reaction kettle cover plate, wherein the reaction kettle cover plate is used for sealing the reaction kettle main body to form a reaction kettle cavity; the high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature hot-liquid fluid also comprises at least one heat-conducting flexible reaction cavity, wherein the flexible reaction cavity is arranged in the reaction kettle body and is in a sealing state; the first guide pipe sequentially penetrates through the reaction kettle cover plate and the flexible reaction cavity from outside to inside so that one end of the first guide pipe is communicated with the flexible reaction cavity, and the other end of the first guide pipe is communicated with the collector. The invention also provides an application of the high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature hot-liquid fluid. The high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature high-pressure hot liquid fluid can be used for in-situ extraction of the hot liquid fluid under high-temperature high-pressure conditions.

Description

High-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid and application
Technical Field
The invention relates to the technical field of geochemistry, in particular to a geochemistry reaction device for experiments, and more particularly relates to a high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid and application thereof.
Background
The hydrothermal fluid, one of the important constituent materials on earth, plays a critical role in the various layers of the earth's surface and interior. Fluid has higher physicochemical activity than solid rock and minerals occupying the body of the earth's interior, and is an important medium for mass and energy transfer within the earth. Like human blood, fluid exchanges and circulates between different layers of the earth through geological processes such as diving action, magma movement and the like, and has important influence on element migration and circulation in the earth.
In the earth science and environmental science, how elements migrate in the hydrothermal fluid, how minerals or rocks react with the hydrothermal fluid, etc. are often required to be studied through high-temperature high-pressure experiments, which is of great importance for the study of the circulation of substances in the earth system. However, because the hydrothermal fluid is a liquid substance mainly comprising aqueous solution, the hydrothermal fluid has the characteristics of strong fluidity, strong volatility, low viscosity, difficult quenching and the like under the conditions of high temperature and high pressure, and has high requirements on a high-temperature high-pressure experimental device, and the conventional device is difficult to develop the experiment of the hydrothermal fluid under the conditions of high temperature and high pressure.
In addition, after the experiment of the existing device is finished, mineral substances in the reaction fluid are precipitated by quenching, so that the analysis of the chemical components of the hydrothermal fluid is difficult to develop, and the physical and chemical properties of the experimental substances can not be observed in situ and quantitatively tested in real time.
Disclosure of Invention
In view of the above, the invention provides a high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature high-pressure hot-liquid fluid and application thereof, which can simultaneously complete high-temperature high-pressure experiments and in-situ extraction of hot-liquid fluid under high-temperature high-pressure conditions, can accurately control the sample quantity of related hydrothermal experiments, and can also improve the test precision of the same.
In a first aspect, the invention provides a high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid, which comprises a reaction kettle main body and a reaction kettle cover plate, wherein the reaction kettle cover plate is used for sealing the reaction kettle main body to form a reaction kettle cavity;
the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid also comprises at least one heat-conducting flexible reaction cavity, wherein the flexible reaction cavity is arranged in the reaction kettle main body and is in a sealing state;
the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature high-pressure hot-liquid fluid further comprises at least one high-temperature high-pressure resistant first conduit and at least one collector, wherein the collector is arranged outside the reaction kettle cavity, the first conduit sequentially penetrates through the reaction kettle cover plate and the flexible reaction cavity from outside to inside so that one end of the first conduit is communicated with the flexible reaction cavity, and the other end of the first conduit is communicated with the collector.
The invention is used in a high-temperature high-pressure reaction kettle for extracting high-temperature hot-liquid fluid in situ, a reaction kettle cavity is assembled by the reaction kettle body and the reaction kettle cover plate, a heat-conducting flexible reaction cavity is also arranged in the reaction kettle cavity, the temperature inside the flexible reaction cavity is kept consistent with the temperature inside the reaction kettle cavity due to the heat conduction effect of the flexible reaction cavity, and the pressure inside the flexible reaction cavity is kept consistent with the pressure inside the reaction kettle cavity due to the heat conduction effect of the flexible reaction cavity. More importantly, the flexible reaction chamber has good ductility and compressibility, is suitable for transmitting pressure and is easy to recover the shape after reaction, so that the flexible reaction chamber is suitable for being used as a reaction vessel under high-temperature and high-pressure conditions.
The high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a first guide pipe and at least one collector, wherein the first guide pipe sequentially penetrates through the reaction kettle cover plate and the flexible reaction cavity from outside to inside, one end of the first guide pipe is communicated with the flexible reaction cavity, and the collector is arranged outside the reaction kettle cavity and is communicated with the other end of the first guide pipe, so that the flexible reaction cavity is communicated with the external collector through the first guide pipe. When the geochemical reaction at high temperature and high pressure is carried out, the hot liquid fluid in the flexible reaction cavity can be directly output to the collector through the first guide pipe by controlling the pressure and is used for subsequent detection and analysis, so that the hot liquid fluid under the conditions of high temperature and high pressure is extracted in situ, the sample quantity of a related hydrothermal experiment can be accurately controlled, and the testing precision of the hot liquid fluid can be improved. The high-temperature high-pressure reaction kettle for in-situ extraction of the hot liquid fluid can realize the reaction of the hot liquid at the temperature of 250-550 ℃ and the pressure of 20-55 MPa, and chemical component analysis can be carried out by sampling after in-situ physical and chemical property observation and experiment. In addition, through setting up into inside and outside double-chamber structure, prevent that reaction liquid from polluting the reation kettle body, and the dress appearance volume is big.
Preferably, the flexible reaction cavity comprises a flexible metal sleeve, an upper clamping plate and a lower clamping plate, wherein an annular flange is arranged at a port of the flexible metal sleeve, a first through hole is formed in the upper clamping plate, and a second through hole is formed in the lower clamping plate;
when the flexible reaction cavity is assembled, the upper clamping plate is abutted against one surface of the annular flange, and the lower clamping plate is abutted against the other surface of the annular flange, so as to seal the flexible metal sleeve; the first conduit sequentially passes through the first through hole and the second through hole to realize the communication between the first conduit and the flexible reaction cavity. Therefore, the lower clamping plate is sleeved with the flexible metal sleeve and is abutted against the lower end of the annular flange, and the upper clamping plate is abutted against the upper end of the annular flange, so that the flexible metal sleeve is closed to form a flexible reaction cavity. In addition, the first conduit sequentially passes through the first through hole and the second through hole from top to bottom, and the flexible metal sleeve is inserted into the port of the flexible metal sleeve, so that the flexible reaction cavity is communicated with the outside through the first conduit, and the in-situ extraction of high-temperature hot liquid fluid from the flexible reaction cavity is facilitated.
Preferably, the corresponding positions of the annular flange, the upper clamping plate and the lower clamping plate are respectively provided with a locking hole, and when the flexible reaction cavity is assembled, the screw rod sequentially penetrates through the locking holes of the upper clamping plate, the annular flange and the lower clamping plate to be used for sealing the flexible metal sleeve. Thus, the upper and lower clamping plates clamp the upper and lower surfaces of the annular flange from the upper and lower ends to close the ports of the flexible metal sleeve. The corresponding positions of the annular flange, the upper clamping plate and the lower clamping plate are respectively provided with a locking hole, the screw rod sequentially penetrates through the locking holes of the annular flange, the upper clamping plate and the lower clamping plate, and the annular flange is tightly pressed by the upper clamping plate and the lower clamping plate, so that the flexible reaction cavity can be better sealed.
Preferably, the flexible metal sleeve is a flexible reaction cavity made of inert metal materials. The inert metal material has good acid and alkali corrosion resistance and ductility, so the inert metal material is relatively suitable for high-temperature and high-pressure reaction of hot fluid with different chemical components, and the chemical stability makes the inert metal material very suitable for being made into a reaction cavity to carry out chemical reaction experiments, and can be cleaned by strong acid at normal temperature for recycling.
Preferably, the flexible metal sleeve is a flexible reaction cavity made of gold, silver, copper or platinum, and the upper clamping plate, the lower clamping plate and the first guide pipe are all made of titanium materials and are subjected to high-temperature annealing treatment. Gold, silver, copper or platinum has good acid and alkali corrosion resistance and ductility, hardly reacts with various acid and alkali except aqua regia under certain temperature and pressure conditions, and the chemical stability makes the gold, silver, copper or platinum very suitable for being prepared into a reaction chamber to carry out chemical reaction experiments, and can be cleaned by strong acid at normal temperature for repeated use. More importantly, gold, silver, copper or platinum has good ductility and compressibility, is suitable for transmitting pressure and is easy to recover shape after reaction, and therefore, is suitable for being used as a reaction vessel under high-temperature and high-pressure conditions. The upper clamping plate, the lower clamping plate and the first guide pipe are made of titanium material, and are subjected to high-temperature annealing treatment, and the surface of titanium is oxidized after high-temperature annealing to form an inert acid-alkali resistant oxide layer.
More preferably, the flexible metal sleeve is arranged in a cylinder shape, and the thickness of the flexible metal sleeve is 0.2-1 mm.
Preferably, the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a reaction kettle clamp, wherein the reaction kettle clamp comprises a groove for accommodating a port of a reaction kettle main body and the edge of a reaction kettle cover plate, a screw hole is formed in the reaction kettle clamp, and the screw hole penetrates through the groove from the side surface of the reaction kettle clamp;
when the reaction kettle cavity is assembled, the edge of the reaction kettle cover plate is abutted to the port of the reaction kettle main body, the edge of the reaction kettle cover plate and the port of the reaction kettle main body are embedded into the groove of the reaction kettle clamp, and the screw rod penetrates through the screw hole to be abutted to the reaction kettle main body or the reaction kettle cover plate. Therefore, the reaction kettle cover plate and the reaction kettle main body can be better clamped by the reaction kettle clamp, the reaction kettle is prevented from being sealed inaccurately under the high-temperature and high-pressure condition, and the safety of the reaction kettle is improved. The screw holes are arranged to further facilitate fine adjustment of the positions of the reaction kettle cover plate and the reaction kettle main body, and the adjusting screw further compresses the reaction kettle after the positions of the reaction kettle cover plate and the reaction kettle main body are aligned.
Preferably, the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a sealing gasket, wherein the sealing gasket is arranged between the reaction kettle cover plate and the reaction kettle main body;
when the reaction kettle cavity is assembled, the edge of the reaction kettle cover plate is abutted against one surface of the sealing gasket, and the port of the reaction kettle main body is abutted against the other surface of the sealing gasket. Therefore, the sealing gasket is arranged to better clamp the reaction kettle cover plate and the reaction kettle main body, so that the reaction kettle is prevented from being sealed inaccurately under the high-temperature and high-pressure conditions.
More preferably, the sealing gasket is a red copper sealing gasket.
Preferably, the reactor further comprises a temperature control system, wherein the temperature control system comprises an annular heating furnace and a thermocouple, and the annular heating furnace is arranged to surround the reactor main body and is used for heating the reactor main body;
the thermocouple is arranged in the reaction kettle main body and used for detecting the temperature of the reaction kettle main body. Therefore, the temperature of the reaction kettle can be controlled in real time by arranging the annular heating furnace and the thermocouple.
Preferably, the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a pressure control system, wherein the pressure control system comprises an air compressor, a pressure gauge and a second conduit, one end of the second conduit is connected with the air compressor, and the other end of the second conduit is communicated with the cavity of the reaction kettle;
when the air compressor is used, water is pressed into the reaction kettle cavity to control the pressure in the reaction kettle main body, and the pressure gauge is used for monitoring the pressure in the reaction kettle cavity. Therefore, the pressure of the reaction kettle can be controlled in real time by arranging the air compressor and the pressure gauge, and the water storage tank can be additionally arranged in specific application.
In a second aspect, the invention also provides the use of a high temperature, high pressure reactor for in situ extraction of high temperature hot liquid fluids.
The high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature high-pressure hot-liquid fluid is applied to geochemical reaction, can accurately simulate high-temperature high-pressure reaction conditions, can also extract the high-temperature high-pressure hot-liquid fluid from the flexible reaction cavity in situ based on requirements at any time, can accurately control the sample amount of an in-situ extraction experiment, and can also improve the test accuracy.
Advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the embodiments of the invention.
Drawings
For a clearer description of the present invention, reference will be made to the following detailed description of embodiments taken in conjunction with the accompanying drawings.
FIG. 1 is a schematic structural diagram of a high temperature and high pressure reactor for in situ extraction of hot liquid fluid according to the present invention;
FIG. 2 is a schematic view of the flexible reaction chamber of FIG. 1;
FIG. 3 is a cross-sectional view of the flexible reaction chamber of FIG. 1;
fig. 4 is a schematic structural view of the reaction vessel cavity in fig. 1.
Detailed Description
The following description is of the preferred embodiments of the present invention, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the principle of the invention, and these modifications and variations are also regarded as the scope of the invention.
The invention provides a high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid, which comprises a reaction kettle main body and a reaction kettle cover plate, wherein the reaction kettle cover plate is covered on the reaction kettle main body to form a reaction kettle cavity. The high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid also comprises a flexible reaction cavity, and particularly, the flexible reaction cavity is a sealed reaction cavity, accommodates relevant geochemical reaction raw materials and provides a reaction space. When the flexible reaction cavity is assembled, the flexible reaction cavity is arranged in the reaction kettle main body, has a heat conduction function, and can transmit heat in the high-temperature high-pressure reaction kettle to the flexible reaction cavity, so that the flexible reaction cavity has a function of simulating high-temperature reaction conditions; and because the flexible reaction cavity has certain flexibility, the pressure in the reaction kettle can be conducted into the flexible reaction cavity, so that the flexible reaction cavity has the function of simulating high-pressure reaction conditions. In a specific embodiment, the high temperature and high pressure reactor for in situ extraction of high temperature hot liquid fluid may comprise one or more flexible reaction chambers for containing the same or different reaction materials, based on actual requirements.
In addition, the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a first conduit and a collector, wherein the collector is arranged outside the reaction kettle cavity and used for collecting the high-temperature hot-liquid fluid extracted in situ from the flexible reaction cavity, and the specific structure is as follows: the first guide pipe sequentially penetrates through the reaction kettle cover plate and the flexible reaction cavity from outside to inside so that the lower end of the first guide pipe is communicated with the flexible reaction cavity, and the upper end of the first guide pipe is communicated with the collector. When the high-temperature hot-liquid fluid is specifically collected, the high-temperature hot-liquid fluid in the flexible reaction cavity can be extracted into the collector by controlling the pressure in the reaction kettle or the pressure in the collector, so that the high-temperature hot-liquid fluid is extracted in situ and is used for subsequent detection and analysis. Meanwhile, the flexible reaction cavity is isolated from the reaction kettle body, so that the reaction kettle body is not polluted, and the sample loading amount is large. In a specific embodiment, the first conduit and the collector are made of materials resistant to high temperature and high pressure, so that damage caused by high temperature and high pressure in a test is prevented, and leakage of hot fluid is prevented. The number of first ducts and collectors may be set based on actual requirements, the same duct may communicate with different collectors, or several first ducts and several collectors may communicate one-to-one.
In a specific embodiment, the flexible reaction chamber comprises a flexible metal sleeve (similar to a sleeve), an upper clamping plate and a lower clamping plate, wherein the port of the flexible metal sleeve is provided with an annular flange (similar to the sleeve port of the flexible metal sleeve is provided with an annular flange), the upper clamping plate is provided with a first through hole, and the lower clamping plate is provided with a second through hole. When the flexible reaction cavity is assembled, the upper clamping plate is abutted against the upper end face of the annular flange, and the lower clamping plate is sleeved with the flexible metal sleeve from bottom to top and is abutted against the lower end face of the annular flange, so that the flexible metal sleeve is sealed through a flange-like structure. The first conduit sequentially passes through the first through hole and the second through hole from top to bottom so as to realize the communication between the first conduit and the flexible reaction cavity. In other embodiments, the flexible reaction chamber may be sealed in other ways, ensuring that the flexible reaction chamber communicates with the external collector only through the first conduit.
In a specific embodiment, locking holes are formed in corresponding positions of the annular flange, the upper clamping plate and the lower clamping plate, and when the flexible reaction cavity is assembled, the screw rod sequentially penetrates through the locking holes of the upper clamping plate, the annular flange and the lower clamping plate from top to bottom and is locked with a nut on the bottom surface of the lower clamping plate, so that the flexible metal sleeve is sealed. In other embodiments, the annular flange, upper clamp plate and lower clamp plate may also be locked by other means, such as by welding.
In a specific embodiment, the flexible metal sleeve is a flexible reaction chamber made of an inert metal material. In particular, it may be a flexible reaction chamber made of gold, silver, copper or platinum. More preferably, the flexible metal sleeve is arranged in a cylinder shape, and the thickness of the flexible metal sleeve is 0.2-1 mm.
In a specific embodiment, the upper clamping plate, the lower clamping plate and the first guide pipe are all made of high-temperature-resistant metal materials. Specifically, the material can be made of titanium and is subjected to high-temperature annealing treatment.
In a specific embodiment, the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a reaction kettle clamp, wherein the reaction kettle clamp comprises a groove structure, and a screw hole is arranged on the reaction kettle clamp and penetrates through the side surface of the reaction kettle clamp to the groove. When the reaction kettle cavity is assembled, the edge of the reaction kettle cover plate is abutted against the port of the reaction kettle main body, the edge of the reaction kettle cover plate and the port of the reaction kettle main body are embedded into the groove of the reaction kettle clamp, and the screw passes through the screw hole to be abutted against the reaction kettle main body or the reaction kettle cover plate, so that the reaction kettle cover plate is extruded to cover the reaction kettle main body tightly. In other embodiments, the reactor cover plate and the reactor body may be fastened by other connection mechanisms instead of the reactor clamp, for example, by providing a buckle.
In a specific embodiment, the high temperature high pressure reactor for in situ extraction of the hot liquid fluid further comprises a sealing gasket. When the reaction kettle cavity is assembled, the edge of the reaction kettle cover plate is abutted against one surface of the sealing gasket, and the port of the reaction kettle main body is abutted against the other surface of the sealing gasket. In a specific embodiment, the sealing gasket may be selected to be a red copper gasket.
In a specific embodiment, the high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature hot-liquid fluid can be heated and controlled by an external temperature control system, and the temperature control system can also be arranged on the reaction kettle. Specifically, the temperature control system comprises an annular heating furnace and a thermocouple, wherein the annular heating furnace is arranged to surround the reaction kettle main body and is used for heating the reaction kettle main body, and the thermocouple is arranged in the reaction kettle main body and is used for detecting the temperature of the reaction kettle main body. In other embodiments, the annular furnace and thermocouple may also be replaced by other heating mechanisms or temperature detectors.
In a specific embodiment, the high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature hot-liquid fluid can realize a high-pressure effect by controlling the temperature, and a pressure control system can also be arranged on the reaction kettle. Specifically, the pressure control system comprises an air compressor, a pressure gauge and a second conduit, one end of the second conduit is connected with the air compressor, and the other end of the second conduit is communicated with the cavity of the reaction kettle. When the air compressor is used, water is pressed into the reaction kettle cavity to control the pressure in the reaction kettle main body, and the pressure gauge is used for monitoring the pressure in the reaction kettle cavity.
Example 1
As shown in fig. 1, the structure of the high-temperature high-pressure reactor for in-situ extraction of high-temperature hot liquid fluid according to the present embodiment is schematically shown. Fig. 1 is a high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid, which comprises a reaction kettle main body 1 and a reaction kettle cover plate 2, wherein the reaction kettle cover plate 2 is covered on the reaction kettle main body 1 to form a reaction kettle cavity. In a specific embodiment, the reactor cavity may be a conventional stainless steel reactor.
The high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid also comprises a flexible reaction cavity 3, and specifically, the flexible reaction cavity 3 is a sealed reaction cavity, accommodates relevant geochemical reaction raw materials and provides a reaction space. When the flexible reaction cavity 3 is assembled, the flexible reaction cavity 3 is arranged in the reaction kettle main body 1, and the flexible reaction cavity 3 has a heat conduction function, so that heat in the high-temperature high-pressure reaction kettle can be transmitted to the flexible reaction cavity 3, and the flexible reaction cavity 3 has a function of simulating high-temperature reaction conditions; and because the flexible reaction cavity 3 has certain flexibility, the pressure in the reaction kettle can be conducted into the flexible reaction cavity 3, so that the flexible reaction cavity 3 has the function of simulating high-pressure reaction conditions.
In a specific embodiment, the high temperature and high pressure reactor for in situ extraction of high temperature hot liquid fluid may comprise one or more flexible reaction chambers 3, one or more flexible reaction chambers 3 being adapted to contain the same or different reaction materials, based on the actual requirements. In this embodiment, a flexible reaction chamber 3 is provided in the high-temperature high-pressure reactor for in-situ extraction of the high-temperature hot-liquid fluid.
The high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a first guide pipe 4, a collector 5 and a collector 6, wherein the collector 5 and the collector 6 are both arranged outside the reaction kettle cavity and used for collecting the high-temperature hot-liquid fluid extracted in-situ from the flexible reaction cavity 3, and the specific connection structure is as follows: the first conduit 4 sequentially penetrates through the reaction kettle cover plate 2 and the flexible reaction cavity 3 from outside to inside so that the lower end of the first conduit 4 is communicated with the flexible reaction cavity 3, and the upper end of the first conduit 4 is respectively communicated with the collector 5 and the collector 6. In practice, a valve may be provided on the first conduit 4 or the collector 5 and the collector 6, and after opening the valve, the hydrothermal fluid is transferred to the collector 5 and the collector 6 along the first conduit 4 because the pressure of the collector 5 and the collector 6 is smaller than the pressure of the flexible reaction chamber 3. The design of two sample collection can ensure the accurate determination of the chemical composition of the solution in the solution analysis test experiment. In other embodiments, for simplifying design or operation, only one collector may be included, or two first conduits are in one-to-one communication with two collectors, so as to extract the solution in the flexible reaction chamber 3 in situ in a split manner, thereby meeting the requirement of real-time analysis and detection. In this embodiment, the first conduit 4 is a titanium conduit, and the collectors 5 and 6 are titanium sampling containers.
In a specific embodiment, as shown in fig. 1 to 3, the flexible reaction chamber 3 includes a flexible metal sleeve 31, an upper clamping plate 32 and a lower clamping plate 33, wherein the flexible metal sleeve 31 is similar to a sleeve with only an upper end opening, the upper end opening of the flexible metal sleeve 31 is provided with an annular flange 311, the upper clamping plate 32 is provided with a first through hole 320, and the lower clamping plate 33 is provided with a second through hole 330. When the flexible reaction chamber 3 is assembled, the upper clamping plate 32 is abutted against the upper end face of the annular flange 311 from top to bottom, and the lower clamping plate 33 is sleeved with the flexible metal sleeve 31 from bottom to top through the second through hole 330 and is abutted against the lower end face of the annular flange 311. Thereby, the upper clamping plate 32 and the lower clamping plate 33 are assembled in a flange-like structure to seal the upper end opening of the flexible metal sleeve 31, thereby forming the closed flexible reaction chamber 3. The upper clamping plate 32 is provided with a first through hole 320, and when in use, the first conduit 4 can pass through the first through hole 320 from top to bottom and be inserted into the flexible metal sleeve 31 from the upper end opening of the flexible metal sleeve 31, so that the first conduit 4 is communicated with the flexible reaction cavity 3.
In a specific embodiment, the corresponding positions of the annular flange 311, the upper clamping plate 32 and the lower clamping plate 33 are respectively provided with a locking hole 34, and when the flexible reaction chamber 3 is assembled, a screw rod sequentially passes through the locking holes 34 of the upper clamping plate 32, the annular flange 311 and the lower clamping plate 33 from top to bottom and is locked by nuts on the bottom surface of the lower clamping plate 33, so that the flexible metal sleeve 31 is sealed. In other embodiments, the annular flange 311, upper clamp plate 32, and lower clamp plate 33 may be connected in other ways.
In a specific embodiment, the flexible metal sleeve 31 is a flexible reaction chamber made of an inert metal material, and more specifically, may be a flexible reaction chamber made of gold, silver, copper or platinum. In this embodiment, the flexible metal sleeve 31 is provided in a cylindrical shape, and the thickness of the flexible metal sleeve 31 is 0.2-1 mm, and the metal foil can ensure the flexibility of the flexible metal sleeve 31.
In a specific embodiment, as shown in fig. 4, the high temperature and high pressure reactor for in situ extraction of high temperature hot liquid fluid further comprises a reactor clamp 7. After the edge 21 of the reaction kettle cover plate is covered on the port 11 of the reaction kettle main body, the edge 21 of the reaction kettle cover plate and the port 11 of the reaction kettle main body are clamped by the groove of the reaction kettle clamp 7, so that the pressure release effect of the reaction kettle is prevented, and the safety of the reaction kettle can be enhanced. In a more specific embodiment, screw holes 71 may also be provided on the reactor clamp 7, and the screw holes 71 penetrate from the side of the reactor clamp 7 to the grooves. When the sealing device is used, the screw rod can pass through the screw hole 71 to be abutted against the edge 21 of the cover plate of the reaction kettle, so that the sealing performance of the reaction kettle is further enhanced. In other embodiments, the screw may pass through the screw hole 71, the reaction kettle cover edge 21 and the reaction kettle main body port 11, which also has the function of enhancing the sealing performance of the reaction kettle.
In a specific embodiment, as shown in fig. 4, the high-temperature and high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a sealing gasket 8, wherein the sealing gasket 8 is arranged between the reaction kettle cover plate 2 and the reaction kettle main body 1. When the reaction kettle cavity is assembled, the edge 21 of the reaction kettle cover plate is abutted against the upper surface of the sealing gasket 8, and the port 11 of the reaction kettle body is abutted against the lower surface of the sealing gasket 8. In this embodiment, the sealing gasket is a red copper sealing gasket.
In a specific embodiment, as shown in fig. 1, the high temperature and high pressure reactor for in situ extraction of the hot liquid fluid further comprises a temperature control system. Specifically, the temperature control system includes an annular heating furnace 91 and a thermocouple 92, the annular heating furnace 91 being disposed around the reaction kettle body 1 for heating the reaction kettle body 1. A thermocouple 92 is provided in the reaction kettle body 1 for detecting the temperature of the reaction kettle body 1. In this embodiment, the number of thermocouples 92 may be 3, and the thermocouples are disposed at three positions of the reaction kettle body 1, that is, at the upper, middle and lower positions, respectively, for detecting the temperatures of the reaction kettle body 1 at different positions. In other embodiments, the heating furnace may be provided with other shapes, or may be provided at the bottom of the heating reactor body 1 or at other positions, and the thermocouple 92 may be replaced by other temperature detecting devices.
In a specific embodiment, the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a pressure control system, wherein the pressure control system comprises an air compressor 101, a pressure gauge 102 and a second conduit 103, the upper end of the second conduit 103 is connected with the air compressor 101, and the lower end of the second conduit 103 is communicated with the reaction kettle cavity. In use, water is pressed into the reaction kettle cavity through the air compressor to increase the pressure in the reaction kettle body 1. The pressure gauge 102 is communicated with the second conduit 103 and is used for monitoring the internal pressure of the reaction kettle cavity. In other embodiments, the second conduit 103 may be further provided with a pressure release valve, so as to reduce the pressure in the reaction kettle body 1 when the critical pressure is exceeded, thereby achieving the purpose of controlling the pressure in the reaction kettle body 1 to be lower than the safe pressure.
In a specific embodiment, the high-temperature and high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a heat preservation layer 12, wherein the heat preservation layer 12 is arranged to surround the reaction kettle body 1, so that the heat in the reaction kettle body 1 can be prevented from leaking too quickly. More specifically, the heat-insulating layer 12 can also encircle the annular heating furnace 91, and the annular heating furnace 91 encircles the reaction kettle main body 1, so that heat can be better locked.
Example 2
The application of the chemical reaction is illustrated to explain the specific application process of the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot liquid fluid. And (3) carrying out Ba isotope fractionation experiments between barite and NaCl fluid at the temperature of 250-500 ℃ and under the pressure of 40 MPa.
The experiment is difficult to realize chemical component measurement of the solution after in-situ extraction reaction by the existing experimental equipment due to higher temperature and pressure, and the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid in the embodiment 1 can meet the requirement. Firstly, calculating the volume of experimental liquid to be added according to the experimental temperature and pressure and the volume of a sample cavity; then we add BaSO into the flexible reaction chamber 3 made of gold 4 And NaCl-BaCl 2 A solution. After the flexible reaction cavity 3 is sealed by a sealing ring made of titanium, the flexible reaction cavity is placed into a stainless steel reaction kettle main body, a cover plate and a clamp are added, the flexible reaction cavity is sealed by nuts, the flexible reaction cavity is pressurized to about 20MPa by a pressurizing pump, a thermocouple is inserted, and then the temperature is slowly raised. Monitoring the change of the pressure representation number in the heating process, and paying attention to whether water flows out from the sealing position of the autoclave; if water leaks, stopping the experiment on a horse and waiting for cooling and then checking the sealing problem; if the pressure is continuously increased, the pressure is gradually discharged outwards by a pressure relief device, and the pressure gauge is kept near the target pressure of 40 MPa. In the experiment, 1ml of the experiment solution was taken out 2 times by valve control, and pH test and ICP-MS test were performed to test the concentration of Ba thereinThe Ba isotope composition of the solution was measured by MC-ICP-MS. The high-temperature high-pressure reaction kettle for in-situ extraction of the high-temperature hot-liquid fluid can realize real-time sampling detection of the experimental hot-liquid fluid, and can test the pH value and various chemical compositions of a fluid sample.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (10)

1. The high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid is characterized by comprising a reaction kettle main body and a reaction kettle cover plate, wherein the reaction kettle cover plate is used for sealing the reaction kettle main body to form a reaction kettle cavity;
the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid also comprises at least one heat-conducting flexible reaction cavity, wherein the flexible reaction cavity is arranged in the reaction kettle main body and is in a sealing state;
the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature high-pressure hot-liquid fluid further comprises at least one high-temperature high-pressure resistant first conduit and at least one collector, wherein the collector is arranged outside the reaction kettle cavity, the first conduit sequentially penetrates through the reaction kettle cover plate and the flexible reaction cavity from outside to inside so that one end of the first conduit is communicated with the flexible reaction cavity, and the other end of the first conduit is communicated with the collector.
2. The high-temperature high-pressure reaction kettle according to claim 1, wherein the flexible reaction cavity comprises a flexible metal sleeve, an upper clamping plate and a lower clamping plate, an annular flange is arranged at a port of the flexible metal sleeve, a first through hole is formed in the upper clamping plate, and a second through hole is formed in the lower clamping plate;
when the flexible reaction cavity is assembled, the upper clamping plate is abutted against one surface of the annular flange, and the lower clamping plate is sleeved with the flexible metal sleeve and is abutted against the other surface of the annular flange, so that the flexible metal sleeve is sealed; the first conduit sequentially passes through the first through hole and the second through hole to realize the communication between the first conduit and the flexible reaction cavity.
3. The autoclave of claim 1, wherein the corresponding positions of the annular flange, the upper clamping plate and the lower clamping plate are provided with locking holes, and when the flexible reaction chamber is assembled, the screw rod sequentially passes through the locking holes of the upper clamping plate, the annular flange and the lower clamping plate to be used for sealing the flexible metal sleeve.
4. The high temperature high pressure reactor according to claim 1, wherein the flexible metal sleeve is a flexible reaction chamber made of an inert metal material.
5. The autoclave of claim 4, wherein the flexible metal sheath is a flexible reaction chamber made of gold, silver, copper or platinum, and the upper clamping plate, the lower clamping plate and the first conduit are made of titanium material and are subjected to high-temperature annealing treatment.
6. The high-temperature high-pressure reaction kettle according to claim 1, wherein the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a reaction kettle clamp, the reaction kettle clamp comprises a groove for accommodating a main body port of the reaction kettle and the edge of a reaction kettle cover plate, the reaction kettle clamp is provided with a screw hole, and the screw hole penetrates from the side surface of the reaction kettle clamp to the groove;
when the reaction kettle cavity is assembled, the edge of the reaction kettle cover plate is abutted to the port of the reaction kettle main body, the edge of the reaction kettle cover plate and the port of the reaction kettle main body are embedded into the groove of the reaction kettle clamp, and the screw rod penetrates through the screw hole to be abutted to the reaction kettle main body or the reaction kettle cover plate.
7. The high temperature high pressure reactor according to claim 6, wherein the high temperature high pressure reactor for in situ extraction of high temperature hot liquid fluid further comprises a sealing gasket, the sealing gasket being disposed between the reactor cover plate and the reactor body;
when the reaction kettle cavity is assembled, the edge of the reaction kettle cover plate is abutted against one surface of the sealing gasket, and the port of the reaction kettle main body is abutted against the other surface of the sealing gasket.
8. The high temperature, high pressure reactor according to claim 1, further comprising a temperature control system comprising an annular heating furnace and a thermocouple, the annular heating furnace being disposed around the reactor body for heating the reactor body;
the thermocouple is arranged in the reaction kettle main body and used for detecting the temperature of the reaction kettle main body.
9. The high-temperature high-pressure reaction kettle according to claim 1, wherein the high-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid further comprises a pressure control system, the pressure control system comprises an air compressor, a pressure gauge and a second conduit, one end of the second conduit is connected with the air compressor, and the other end of the second conduit is communicated with a reaction kettle cavity;
when the air compressor is used, water is pressed into the reaction kettle cavity to control the pressure in the reaction kettle main body, and the pressure gauge is used for monitoring the pressure in the reaction kettle cavity.
10. Use of a high temperature high pressure reactor as claimed in claims 1-9.
CN202310802593.2A 2023-07-03 2023-07-03 High-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid and application Pending CN116617943A (en)

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Application Number Priority Date Filing Date Title
CN202310802593.2A CN116617943A (en) 2023-07-03 2023-07-03 High-temperature high-pressure reaction kettle for in-situ extraction of high-temperature hot-liquid fluid and application

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CN116617943A true CN116617943A (en) 2023-08-22

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