CN203396613U - Built-in type in-situ sampling device for high-temperature high-pressure reaction kettle - Google Patents

Abstract

The utility model discloses a built-in type in-situ sampling device for a high-temperature high-pressure reaction kettle. The built-in type in-situ sampling device comprises a compression ring (1), a temperature and pressure measuring kettle plug (2), a sealing ring (10), a sampling kettle plug (11) and a rotary knob torsion bar (9), wherein a sampler (5) is arranged in a kettle body (3), one end of the sampler (5) is connected with the rotary knob torsion bar (9) through a sealing cover (8), the other end of the sampler (5) is fixed on the temperature and pressure measuring kettle plug (2) through a base (4), the sampler (5) is in threaded connection with the sealing cover (8), a sealing element (6) is arranged in a gap between the sampler (5) and the sealing cover (8), and an intercommunicating hole (7) is formed in the upper part of the sampler (5). The built-in type in-situ sampling device can be used for effectively solving the problem in the prior art that an in-situ sampling technology in the high-temperature high-pressure reaction kettle cannot simultaneously meet the requirements of rapidness, single phase state and sample composition no-loss.

Description

A built-in in-situ sampling device for high-temperature and high-pressure reactors

technical field

The utility model relates to a high-temperature and high-pressure in-situ sampling device, in particular to a built-in in-situ sampling device suitable for high-temperature and high-pressure reactors, belonging to the field of reactor sampling devices.

Background technique

High-temperature and high-pressure reactor is a common high-temperature and high-pressure experimental device, which is widely used in high-temperature and high-pressure water fluid properties and water-fluid-solid interactions in the earth's interior, supercritical water-cooled reactors in nuclear power plants, and high-temperature and high-pressure simulation experiments in the field of chemical and chemical research. At the same time, it is also a common production equipment in the petrochemical industry, clean coal-fired utilization, artificial crystal cultivation and other industrial fields. It is characterized by providing a high-temperature and high-pressure reaction environment. In order to detect the progress of the chemical reaction in the autoclave, it is necessary to sample the high-temperature and high-pressure fluid in the autoclave to determine the chemical composition. However, due to the extremely harsh environment of high temperature and high pressure, efficient, accurate and reliable in-situ sampling technology has always been an important goal in the development of high temperature and high pressure experimental technology.

At present, the high-temperature and high-pressure in-situ sampling technologies that have been invented mainly include in-situ sampling valve technology, built-in needle valve sealed sampler technology and artificial inclusion sampling technology: (1) in-situ sampling valve technology uses a capillary tube to make One end communicates with the sample chamber of the high-temperature pressure vessel, and the other end communicates with the sampler in the normal temperature and pressure area. A high-pressure valve is installed in the middle of the capillary near the cold area, and the valve is closed before sampling. When the experiment reaches the set state, the valve is opened, and the fluid sample in the sample chamber of the high-temperature pressure vessel flows out from the capillary into the sampler, thereby obtaining the fluid sample in the sample system under high temperature and high pressure. The in-situ sampling valve technology is currently widely used in high-temperature and high-pressure reactors, but in this technology, the sampling process is actually a process in which the temperature and pressure of the sample drop sharply. Sudden pressure drops often result in solid material settling from the fluid into the dead space of the valve, the contact surfaces of the valve and the fluid, and the inner wall of the capillary, resulting in a loss of mass in the fluid sample in the sampler. (2) Built-in needle valve sealed sampler technology, which is similar to placing a high-pressure valve inside an autoclave to seal and capture fluid. The basic components of this technology include a built-in sampling container, valve stem, needle valve and seals. Among them, the built-in sampling container is a titanium alloy metal container with one end open and passivated on the inner and outer surfaces. Titanium alloy metal rod, one end of which is made into a conical shape and the inner edge of the sampler to form a needle valve mechanism, the other end is located in the normal temperature and pressure area outside the high temperature pressure vessel, and the middle part runs through the seal located in the high temperature and high pressure area; the seal It is made of graphite with high temperature resistance, easy deformation and slip effect. In the high-temperature and high-pressure experiment, the cylindrical high-temperature pressure vessel is erected along the axial direction, and the in-situ sealing of the sample in the sampler can be realized by rotating the valve stem located in the normal temperature and pressure zone. The built-in needle-valve sealed sampler technology is mainly used in geoscience high-temperature and high-pressure experiments, but there are some problems in the application of this technology: graphite seals cannot avoid contact with fluid, which will lead to a certain degree of sample contamination; The seal between the valve stem and the seal is a heat seal. The rotation of the valve stem needs to overcome the friction between the valve stem and the seal in the high temperature and high pressure area. The limited strength of the valve stem at high temperature will undoubtedly affect the temperature and pressure of this technology. make an impact. (3) In situ sampling technology of artificial inclusions, the principle of which is to place transparent minerals containing microcracks (usually produced by thermal shock) in the sample chamber, where the microcracks in the transparent minerals communicate with the environment in which the minerals are located. During the high-pressure experiment, the transparent minerals undergo a dissolution-recrystallization process in the fluid, so that the microscopic cracks are closed to form inclusions one by one. At this time, the fluid in the sample system is sealed in situ by the inclusions and formed without damage. This technology can be widely used in high-temperature and high-pressure experimental devices such as autoclaves, flow reactors, piston cylinders, and polyhedral large cavities. However, people have found that this technology has the following disadvantages in long-term practice: this technology is only suitable for the sample system itself In the case of carrier minerals with artificial inclusions that would otherwise contaminate the sample due to the addition of the carrier mineral; since inclusion closure requires a long time for crystal growth to complete, this technique is hardly usable at high temperatures for kinetic studies High-pressure experiments; for high-temperature and high-pressure experiments with relatively slow kinetic processes, the fluid composition captured by different inclusions is different due to the different sealing time of different inclusions, so this technique is not suitable for kinetic processes Slow high temperature and high pressure experiment.

In summary, in-situ sampling technology is extremely important for high-temperature and high-pressure experiments in fluid-containing multiphase systems. However, various in-situ sampling technologies currently used are difficult to simultaneously meet the requirements of rapidity, single-phase state, and non-destructive sample composition. Therefore, the development of a high-temperature and high-pressure in-situ sampling technology that is fast, single-phase, and sample composition-free has become an international problem that needs to be solved urgently in the field of high-temperature and high-pressure experimental research on fluid-containing multiphase material systems.

Contents of the invention

The technical problem to be solved by the utility model is to provide a built-in in-situ sampling device for high-temperature and high-pressure reactors to solve the problems that the current in-situ sampling technology cannot simultaneously achieve fast, single-phase state and non-destructive sample composition.

Technical scheme of the utility model:

A built-in in-situ sampling device for high-temperature and high-pressure reaction kettles, including pressure rings, temperature and pressure measurement kettle plugs, sealing rings, sampling kettle plugs and knob levers, a sampler is set in the kettle body, and one end of the sampler passes through the The sealing cover is connected with the knob rod, and the other end of the sampler is fixed on the plug of the temperature and pressure measuring kettle through the base. The upper part of the sampler has a connecting hole.

The above-mentioned sampler has holes and threads inside, and a shank at the bottom.

The aforementioned sealing cover is provided with holes inside and has threads on the outside.

Jacks are provided on the foregoing base.

The aforesaid sealing cover and the knob force rod are connected by a bolt.

The beneficial effects of the utility model:

In the sampling process of the utility model, since the sampler and the sealing cover are connected by threads, the relative movement between the sampler and the sealing cover can be realized by twisting the knob force rod outside the autoclave, and then the connecting hole on the sampler can be realized. The rapid closure, that is, the utility model can realize the real-time, fast and in-situ sampling of the sampler in the autoclave under the high temperature and high pressure state. At the same time, the movement of the sealing cover can withstand the seal, thereby better isolating the liquid in the sampler from the liquid in the kettle, and since the sampler is sealed until the sampler is taken out after the autoclave is quenched and released, the whole process of sampling The device is always in a sealed state, so the utility model has the characteristics of no damage to the sample composition during the sampling process. In addition, the utility model can realize the in-situ sampling of the single-phase fluid in the multi-phase coexistence system by adjusting the height of the handle of the sampler. As mentioned above, compared with the prior art, the utility model can effectively solve the problem that the current in-situ sampling technology cannot simultaneously achieve fast, single-phase state and non-destructive sample composition.

Description of drawings:

Fig. 1 is a schematic view of the longitudinal section of the utility model.

Detailed ways:

As shown in Figure 1, the utility model is a built-in in-situ sampling device for high-temperature and high-pressure reactors, including a pressure ring 1, a temperature and pressure measurement kettle plug 2, a sealing ring 10, a sampling kettle plug 11 and a knob lever 9. The base 4 is welded or fixed on the temperature and pressure measuring kettle plug 2 with bolts; the inside of the sampler 5 has holes and threads, and a communication hole 7 is opened on the sampler 5, so that the sampler 5 and the kettle can be connected to each other when the experiment is carried out. The inner space is connected as a whole, and there is a handle at the bottom, which can be inserted into the socket on the base 4 to fix the sampler 5. At the same time, the single-phase state in the multiphase coexistence system can be realized by adjusting the height of the handle of the sampler. In-situ sampling of the fluid; the inside of the sealing cover 8 has a through hole, and the outside is provided with threads; the sampler 5 and the sealing cover 8 are connected by threads; A seal 6 is provided between them.

The utility model can be applied to in-situ sampling of fluids under the conditions of normal temperature ~ 500 DEG C and normal pressure ~ 100MPa.

When in use, the temperature and pressure measuring kettle plug 2 fixed with the base 4 is put into the kettle body 3, and then the experimental sample is added into the kettle body; the sealing cover 8 of the sampler 5 is fixed on the knob force On the rod 9, the seal 6 and the sampler 5 are preliminarily screwed on the sealing cover 8 through threads, and the communication hole 7 on the sampler 5 is guaranteed to be in an open position, and then the knob force rod 9 with the sampling device The whole is put into the kettle body, and the handle of the sampler 5 can be snapped into the socket of the base 4 to fix the position of the sampler. Finally, the sampling kettle plug 11 is put into the autoclave and the autoclave is sealed. After the experiment is over, the screw thread of the sealing cover 8 is driven downward by turning the knob force rod 9 placed outside the autoclave to squeeze the sealing member 6 between the sealing cover 8 and the sampler 5, so that the sealing member 6 is deformed. The line sealing effect is achieved, so that the calcite dissolution equilibrium fluid under high temperature and high pressure is sealed in the sampler 5 . After the autoclave is quenched and depressurized, the sampler 5 is taken out. Since the sampler 5 has been isolated from the solution in the kettle after being sealed under high temperature and high pressure, and no longer undergoes material exchange or reaction with the contents of the kettle, the condensate in the sampler 5 can represent For the chemical composition of the fluid in the high temperature and high pressure state, the experimental data under the high temperature and high pressure water fluid condition can be accurately obtained by analyzing the condensate in the sampler 5 . At the same time, the in-situ sampling of the single-phase fluid in the multi-phase coexistence system can be realized by adjusting the height of the sampler insert in the experiment.

Claims (5)

1. A built-in in-situ sampling device for high-temperature and high-pressure reactors, including pressure rings (1), temperature and pressure measurement kettle plugs (2), sealing rings (10), sampling kettle plugs (11) and knob force Rod (9), characterized in that: a sampler (5) is set in the kettle body (3), one end of the sampler (5) is connected to the knob lever (9) through a sealing cover (8), and the sampler (5) The other end is fixed on the temperature and pressure measuring kettle plug (2) through the base (4), the sampler (5) and the sealing cover (8) are threaded, and the connection between the sampler (5) and the sealing cover (8) There is a seal (6) in the gap between them, and there is a communication hole (7) on the upper part of the sampler (5). 2. A built-in in-situ sampling device for high-temperature and high-pressure reactors according to claim 1, characterized in that: the sampler (5) has holes and threads inside, and a handle at the bottom. 3. A built-in in-situ sampling device for high-temperature and high-pressure reactors according to claim 1, characterized in that: the sealing cover (8) has holes inside and threads on the outside. 4. A built-in in-situ sampling device for high-temperature and high-pressure reactors according to claim 1, characterized in that: the base (4) is provided with jacks. 5. A built-in in-situ sampling device for high-temperature and high-pressure reactors according to claim 1, characterized in that: the sealing cover (8) and the knob force rod (9) are connected by bolts.

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