Vacuum degasser with supercritical drying function

Abstract

The utility model discloses a vacuum degassing machine with a supercritical drying function, which belongs to the field of vacuum degassing experimental equipment and comprises a machine body, a supercritical extraction chamber and a heating vacuum degassing chamber. Wherein the supercritical extraction chamber and the heating vacuum degassing chamber are arranged in the machine body in parallel; one side of the supercritical extraction chamber is connected with an air inlet pipe, and the other side of the supercritical extraction chamber is provided with an exhaust port; and the thermal vacuum degassing chamber is respectively provided with a vacuum pump connecting pipe and a backfill gas inlet pipe. According to the vacuum degasser, liquid phase surface tension is not generated when liquid in pore channels of a porous material is removed. And large specific surface tension is prevented from damaging the pore structure of the sample, so that the microstructure of the porous material sample is protected.

Description

Technical Field

[0001] This utility model relates to the field of vacuum degassing machine technology, and in particular to a vacuum degassing machine with supercritical drying function. Background Technology

[0002] In the field of adsorption testing of porous materials, porous material samples need to undergo vacuum degassing activation pretreatment before adsorption testing to remove liquid solvents or adsorbed gases from the pores. Existing vacuum degassing machines only have heating vacuum degassing functions. However, during the process of removing solvents through vacuum degassing, the liquid in the nanoscale micropores of the porous material transforms into a gaseous state, generating strong surface tension due to capillary action, which may damage the pore structure of the porous material.

[0003] In view of the above, this utility model is hereby proposed. Utility Model Content

[0004] The purpose of this invention is to provide a vacuum degasser with supercritical drying function, which can remove solvent from porous material samples while protecting the pore structure of microporous materials during the degassing and activation pretreatment process of adsorption testing, thereby solving the above-mentioned technical problems existing in the prior art.

[0005] The objective of this utility model is achieved through the following technical solution:

[0006] The chamber consists of the main body, a supercritical extraction chamber, and a heated vacuum degassing chamber; among which,

[0007] The supercritical extraction chamber and the heated vacuum degassing chamber are arranged side by side inside the machine body;

[0008] One side of the supercritical extraction chamber is connected to an air inlet pipe, and the other side is provided with an exhaust port;

[0009] The heating vacuum degassing chamber is equipped with a vacuum pump connecting pipe and a backfill gas inlet pipe.

[0010] Compared with the prior art, the vacuum degassing machine with supercritical drying function provided by this utility model has the following advantages:

[0011] By arranging a supercritical extraction chamber and a heated vacuum degassing chamber side-by-side within the apparatus, during the degassing and activation pretreatment process for adsorption testing, the supercritical extraction chamber first removes the solvent from the porous material sample via supercritical drying, and then the heated vacuum degassing chamber activates the supercritical medium-extracted and dried porous material sample through heated vacuum degassing. This achieves the removal of liquid from the porous material channels without generating liquid phase surface tension. This avoids generating large specific surface tension that could damage the sample's pore structure, thus protecting the microstructure of the porous material sample. Attached Figure Description

[0012] To more clearly illustrate the technical solutions of the embodiments of this utility model, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0013] Figure 1 A schematic diagram of the structure of a vacuum degasser with supercritical drying function provided in an embodiment of this utility model. Detailed Implementation

[0014] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments, which do not constitute a limitation on the present utility model. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.

[0015] First, the following explanations are provided for the terms that may be used in this article:

[0016] The term "and / or" means that either or both can be achieved simultaneously. For example, X and / or Y means that it includes both "X" or "Y" as well as the three cases of "X and Y".

[0017] The terms “including,” “comprising,” “containing,” “having,” or other similar semantic descriptions should be interpreted as non-exclusive inclusion. For example, “including a technical feature element (such as raw material, component, ingredient, carrier, dosage form, material, size, part, component, mechanism, device, step, process, method, reaction conditions, processing conditions, parameter, algorithm, signal, data, product or article of manufacture, etc.)” should be interpreted as including not only the expressly listed technical feature element, but also other technical feature elements that are not expressly listed and are well-known in the art.

[0018] The term "composed of" excludes any technical features not expressly listed. When used in a claim, it closes the claim to exclude all technical features other than those expressly listed, except for associated conventional impurities. If the term appears only in a clause of a claim, it limits the claim to the elements expressly listed in that clause; elements recited in other clauses are not excluded from the overall claim.

[0019] Unless otherwise explicitly specified or limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal connection between two components. Those skilled in the art can understand the specific meaning of the above terms in this document according to the specific circumstances.

[0020] When concentration, temperature, pressure, size, or other parameters are expressed as numerical ranges, such ranges should be understood to specifically disclose all ranges formed by any pairing of upper limits, lower limits, or preferred values ​​within that range, regardless of whether the range is explicitly stated; for example, if the numerical range "2 to 8" is stated, then that range should be interpreted to include ranges such as "2 to 7", "2 to 6", "5 to 7", "3 to 4 and 6 to 7", "3 to 5 and 7", "2 and 5 to 7", etc. Unless otherwise stated, the numerical ranges described herein include both their endpoints and all integers and fractions within that range.

[0021] The terms “center,” “longitudinal,” “lateral,” “length,” “width,” “thickness,” “upper,” “lower,” “front,” “back,” “left,” “right,” “vertical,” “horizontal,” “top,” “bottom,” “inner,” “outer,” “clockwise,” and “counterclockwise” indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience and simplification of description and do not imply that the device or component referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this document.

[0022] The solution provided by this utility model is described in detail below. Contents not described in detail in the embodiments of this utility model are prior art known to those skilled in the art. Where specific conditions are not specified in the embodiments of this utility model, they shall be performed according to conventional conditions in the art or conditions recommended by the manufacturer. Reagents or instruments used in the embodiments of this utility model whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0023] like Figure 1 As shown, an embodiment of the present invention provides a vacuum degassing machine with supercritical drying function, comprising:

[0024] The apparatus consists of three parts: a main body 3, a supercritical extraction chamber 1, and a heated vacuum degassing chamber 2; among which,

[0025] The supercritical extraction chamber 1 and the heated vacuum degassing chamber 2 are arranged side by side inside the body 3;

[0026] One side of the supercritical extraction chamber 1 is connected to an air inlet pipe, and the other side is provided with an exhaust port;

[0027] The heating vacuum degassing chamber 2 is equipped with a vacuum pump connecting pipe 25 and a backfill gas inlet pipe 27.

[0028] Preferably, in the above-mentioned vacuum degassing machine, the supercritical extraction chamber 1 includes: a supercritical high-pressure chamber 11, a high-pressure chamber transparent cover 12, an inlet solenoid valve 13, an exhaust solenoid valve 14, a cooling device 15, and a heating device 16; wherein,

[0029] The supercritical high-pressure chamber 11 has an air inlet connected to the air inlet pipe on one side and an exhaust port connected to the exhaust pipe on the other side. The supercritical high-pressure chamber 11 is a sample cell for placing the sample medium for supercritical medium extraction and drying.

[0030] The intake solenoid valve 13 is installed on the intake pipe connected to the intake port of the supercritical high-pressure chamber 11, and can control the gas entering the supercritical high-pressure chamber; the front end of the intake pipe is connected to a CO2 cylinder 4 with a siphon tube.

[0031] The transparent cover 12 of the high-pressure chamber is fastened to the upper opening of the sample cell of the supercritical high-pressure chamber 11. It is transparent and can be used to observe the sample and the state of the supercritical medium inside the supercritical high-pressure chamber.

[0032] The exhaust solenoid valve 14 is installed on the exhaust pipe connected to the exhaust port of the supercritical high-pressure chamber, and can control the discharge of carbon dioxide and impurities from the supercritical high-pressure chamber.

[0033] The cooling device 15 and the heating device 16 are both installed on the supercritical high-pressure chamber 11, which can control the temperature inside the supercritical high-pressure chamber 11 and keep the sample medium extracted inside the supercritical high-pressure chamber at the supercritical temperature.

[0034] Preferably, in the above-mentioned vacuum degasser, the supercritical extraction chamber 1 further includes:

[0035] The first filter 18 is connected to the air inlet pipe connected to one side of the supercritical high-pressure chamber and is used to filter impurity particles in the air inlet provided by the cylinder 4.

[0036] The second filter 19 is connected to the exhaust pipe on the other side of the supercritical high-pressure chamber and can filter sample particles and impurities in the exhaust gas.

[0037] The damping tube 111 is connected to the exhaust pipe on the other side of the supercritical high-pressure chamber and can control the flow rate of the exhaust gas.

[0038] Flow meter 112, connected to the end of the exhaust pipe, can measure the flow rate of discharged carbon dioxide and impurity gases;

[0039] Pressure gauge 110 is installed in the supercritical high-pressure chamber and can read the pressure of the supercritical high-pressure chamber.

[0040] By setting up the damping tube 111, the flow rate of the gas in the entire exhaust gas path is controlled. When the flow rate is large, the gas flow rate in the pipeline is reduced by adjusting the damping tube to avoid the sample flying due to excessively fast exhaust, which could then contaminate or clog the second filter.

[0041] The flow meter 112 can be set to determine whether the exhaust pipe is blocked, and it can also help determine whether the pressure of the CO2 cylinder 4 at the air inlet meets the usage requirements. The flow meter is set at the vent A.

[0042] Preferably, in the above-mentioned vacuum degassing machine, the heated vacuum degassing chamber 2 includes: a sample tube heating furnace 21, a sample tube vacuum interface 22, a vacuum pressure gauge 28, and a vacuum pump 29; wherein,

[0043] The sample tube heating furnace 21 has a sample tube accommodating space inside, which can heat the sample tube to cooperate with the vacuum pump for vacuum degassing of the sample.

[0044] The sample tube vacuum interface 22 can seal the upper opening of each sample tube in the sample tube heating furnace to the gas exhaust.

[0045] The gas exhaust 23 is connected to the vacuum interface of the sample tube at one end, and to the vacuum pump 29 via the vacuum pump connecting pipe 25 and the first valve 24 at the other end. It is also connected to the backfill gas inlet pipe 27 via the pipeline and the second valve 26. The outer end of the backfill gas inlet pipe 27 is the backfill gas inlet B, which can connect the gas paths of all sample tubes in parallel and control the centralized gas intake and exhaust.

[0046] The vacuum pressure gauge 28 is installed at the first valve and can read the pressure of each sample tube in the sample tube heating furnace through the air exhaust.

[0047] The vacuum pump 29 can evacuate each sample tube to a vacuum state.

[0048] In summary, the vacuum degassing machine of this invention, by arranging a supercritical extraction chamber and a heated vacuum degassing chamber side by side within the machine body, achieves the following in the degassing and activation pretreatment process of adsorption testing: first, the supercritical extraction chamber removes the solvent from the porous material sample through supercritical extraction and drying; then, the heated vacuum degassing chamber performs heated vacuum degassing and activation on the porous material sample after supercritical medium extraction and drying. This ensures that no liquid phase surface tension is generated when removing liquid from the pores of the porous material sample, thereby protecting the pore structure of the porous material sample.

[0049] To more clearly demonstrate the technical solution and its effects provided by this utility model, the following detailed description of the solution provided by the embodiments of this utility model is provided with reference to specific examples.

[0050] Example 1

[0051] like Figure 1 As shown, this embodiment provides a heated vacuum degassing machine with supercritical drying function, which consists of a supercritical high-pressure chamber 1 and a heated vacuum degassing chamber 2 arranged side by side within the machine body; wherein,

[0052] The supercritical extraction chamber 1 consists of a supercritical high-pressure chamber 11 and its inlet and outlet gas path structure. The porous material sample is placed in the supercritical high-pressure chamber 11 and dried by supercritical medium extraction. It is then transferred to the sample tube heater 21 in the heated vacuum degassing chamber 2 for heated vacuum degassing and activation. This heated vacuum degassing mechanism can remove the solvent from the porous material sample through supercritical extraction and drying within the same device, followed by heated vacuum degassing and activation of the supercritical medium-extracted and dried porous material sample in the heated vacuum degassing chamber. This process removes liquid from the pores of the porous material sample without generating liquid phase surface tension, thus protecting the pore structure of the porous material sample.

[0053] The above description is merely a preferred embodiment of this utility model, but the scope of protection of this utility model is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this utility model should be included within the scope of protection of this utility model. Therefore, the scope of protection of this utility model should be determined by the scope of the claims. The information disclosed in the background section is intended only to enhance the understanding of the overall background technology of this utility model and should not be construed as an admission or implication in any way that such information constitutes prior art known to those skilled in the art.

Claims

1. A vacuum degasser with supercritical drying function, characterized in that, include: The chamber consists of the main body, a supercritical extraction chamber, and a heated vacuum degassing chamber; among which, The supercritical extraction chamber and the heated vacuum degassing chamber are arranged side by side inside the machine body; One side of the supercritical extraction chamber is connected to an air inlet pipe, and the other side is provided with an exhaust port; The heating vacuum degassing chamber is equipped with a vacuum pump connecting pipe and a backfill gas inlet pipe.

2. The vacuum degasser with supercritical drying function according to claim 1, characterized in that, The supercritical extraction chamber includes: a supercritical high-pressure chamber, a transparent cover for the high-pressure chamber, an inlet solenoid valve, an exhaust solenoid valve, a cooling device, and a heating device; wherein... The supercritical high-pressure chamber has an air inlet connected to the air inlet pipe on one side and an exhaust port connected to the exhaust pipe on the other side. The supercritical high-pressure chamber is a sample cell for placing the sample medium for supercritical medium extraction and drying. The intake solenoid valve is installed on the intake pipe connected to the intake port of the supercritical high-pressure chamber, and can control the gas entering the supercritical high-pressure chamber. The transparent cover of the high-pressure chamber is attached to the upper opening of the sample cell in the supercritical high-pressure chamber. It is transparent and allows observation of the sample and the state of the supercritical medium inside the supercritical high-pressure chamber. The exhaust solenoid valve is installed on the exhaust pipe connected to the exhaust port of the supercritical high-pressure chamber, and can control the discharge of carbon dioxide and impurity gases from the supercritical high-pressure chamber. The cooling device and heating device are both installed on the supercritical high-pressure chamber, which can control the temperature inside the supercritical high-pressure chamber and keep the supercritical high-pressure chamber at a supercritical temperature.

3. The vacuum degasser with supercritical drying function according to claim 2, characterized in that, The supercritical extraction chamber also includes: The first filter is connected to the air inlet pipe on one side of the supercritical high-pressure chamber and can filter impurity particles in the air intake. The second filter is connected to the exhaust pipe on the other side of the supercritical high-pressure chamber and can filter sample particles and impurities in the exhaust gas. The damping tube, connected to the exhaust pipe on the other side of the supercritical high-pressure chamber, can control the flow rate of the exhaust gas. A flow meter, connected to the end of the exhaust pipe, can measure the flow rate of carbon dioxide and impurity gases discharged from the supercritical high-pressure chamber. A pressure gauge is installed in the supercritical high-pressure chamber to read the pressure of the supercritical high-pressure chamber.

4. The vacuum degassing machine with supercritical drying function according to any one of claims 1-3, characterized in that, The heating vacuum degassing chamber includes: a sample tube heating furnace, a sample tube vacuum interface, a vacuum pressure gauge, and a vacuum pump; wherein... The sample tube heating furnace has an internal sample tube accommodating space, which can heat the sample tube to cooperate with the vacuum pump for vacuum degassing of the sample. The sample tube vacuum interface can seal the upper opening of each sample tube in the sample tube heating furnace to the gas exhaust. The gas exhaust is connected at one end to the vacuum interface of the sample tube, and at the other end to the vacuum pump via the vacuum pump connecting pipe and the first valve, and to the backfill gas inlet pipe via the pipeline and the second valve. It can connect the gas paths of all sample tubes in parallel and control the centralized gas intake and exhaust. The vacuum pressure gauge is installed at the first valve and can read the pressure of each sample tube in the sample tube heating furnace through the air exhaust. The vacuum pump can evacuate each sample tube to a vacuum state.

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