Purification apparatus for single-walled carbon nanotubes

Abstract

The utility model belongs to the technical field of purification device, concretely relates to a purification device for single-wall carbon nanotube, and the novel model includes: high pressure reation kettle and the stirring mechanism of setting on high pressure reation kettle, wherein high pressure reation kettle is adapted to with supercritical fluid system intercommunication, the stirring mechanism is adapted to stirring mixed supercritical fluid in high pressure reation kettle, the stage decompression valve is connected with high pressure reation kettle pipeline in one end, is connected with post -treatment system pipeline in the other end, first valve, one end is connected with high pressure reation kettle pipeline, the other end is connected with closed loop system pipeline, second valve, one end is connected with high pressure reation kettle pipeline, the other end is connected with collecting jar pipeline, and the purification device for single-wall carbon nanotube passes through supercritical fluid purification to reach the original structure of effective reservation single-wall carbon nanotube and excellent electrical, mechanical performance, solves the problem that the conductivity of existing pickling method causes the decline.

Description

Technical Field

[0001] This utility model belongs to the field of purification device technology, specifically relating to a purification device for single-walled carbon nanotubes. Background Technology

[0002] Single-walled carbon nanotubes (SUVs), as nanomaterials with a unique one-dimensional tubular structure, exhibit irreplaceable application value in fields such as flexible electronic devices, energy storage materials, and composite material reinforcements due to their excellent electrical conductivity, mechanical strength, and chemical stability. However, the preparation processes of SUVs (such as chemical vapor deposition and arc discharge methods) often leave behind a large number of impurities, requiring purification treatment.

[0003] Existing patent CN215288024U discloses a purification device for large-diameter carbon nanotubes. The description includes: by setting up an acid mist emission port and a cooler, the acid mist is recycled; by setting up a filter and a pH adjustment device, the used waste acid is reprocessed and recycled. This allows for the purification of large-diameter carbon nanotubes, enabling the reuse of large amounts of acid solution, saving production costs and reducing environmental pollution. However, this purification method uses acid washing, but strong acids corrode the surface of single-walled carbon nanotubes, introducing numerous defects (such as carboxyl and hydroxyl groups), leading to decreased conductivity. Simultaneously, it generates toxic waste liquid containing heavy metal ions, resulting in high environmental treatment costs and contradicting the concept of green production.

[0004] Therefore, in order to solve the above problems, it is necessary to design a purification device for single-walled carbon nanotubes. Utility Model Content

[0005] The purpose of this invention is to provide a purification device for single-walled carbon nanotubes to solve the technical problems mentioned in the background art.

[0006] To solve the above-mentioned technical problems, this utility model provides a purification device for single-walled carbon nanotubes, comprising:

[0007] High-pressure reactor and a stirring mechanism mounted on the high-pressure reactor; wherein

[0008] The high-pressure reactor is suitable for connection with a supercritical fluid system;

[0009] The stirring mechanism is suitable for stirring and mixing supercritical fluids in a high-pressure reactor.

[0010] The graded pressure reducing valve is connected at one end to the high-pressure reactor pipeline and at the other end to the post-processing system pipeline.

[0011] The first valve is connected at one end to the high-pressure reactor pipeline and at the other end to the closed-loop system pipeline.

[0012] The second valve is connected at one end to the high-pressure reactor pipeline and at the other end to the collection tank pipeline.

[0013] Furthermore, the high-pressure reactor includes: a reactor body and a reactor cover for sealing the reactor body;

[0014] The stirring mechanism includes: a stirring shaft disposed within the vessel body and several layers of blades disposed on the stirring shaft; wherein

[0015] The upper part of the stirring shaft penetrates through the vessel lid and is connected to the vessel lid bearing; and

[0016] Each layer of the blade assembly includes: at least three stirring blades arranged in a circular array;

[0017] Each of the aforementioned stirring blades is mounted on the stirring shaft.

[0018] Furthermore, the stirring mechanism also includes: a bearing housing mounted on the vessel lid and a drive motor mounted on the bearing housing; wherein

[0019] The bearing housing is sleeved on the stirring shaft and connected to the stirring shaft bearing;

[0020] The output shaft of the drive motor is connected to the stirring shaft to drive the stirring shaft to rotate.

[0021] Furthermore, a three-way valve is connected to a pipe on one side of the vessel; wherein

[0022] The other two ends of the three-way valve are respectively connected to the supercritical fluid system and the co-solvent injection unit pipeline.

[0023] Furthermore, the high-pressure reactor also includes: an inlet communicating with the top of the reactor lid, a sealing cap covering the inlet, and a clamp for connecting the inlet and the sealing cap.

[0024] Furthermore, the stirring mechanism also includes: at least three scrapers arranged in a circular array inside the vessel; wherein

[0025] The scraper is connected to the corresponding stirring blades of each layer of blade group;

[0026] The other side of the scraper is in contact with the inner wall of the vessel.

[0027] Furthermore, the first valve is connected to the vessel lid;

[0028] The graded pressure reducing valve is connected to a pipe on one side of the vessel body;

[0029] The second valve is connected to the bottom pipe of the vessel.

[0030] The beneficial effects of this utility model are:

[0031] (I) This utility model involves opening the sealed cap, introducing the single-walled carbon nanotubes to be purified into the reactor through the inlet, closing the sealed cap and sealing it with clamps, and then introducing supercritical fluid and co-solvent into the reactor through a three-way valve to achieve the preset pressure and form a stable supercritical environment. The drive motor is then started, and the stirring shaft rotates the multi-layer blade assembly. The stirring blades ensure thorough mixing of the supercritical fluid and carbon nanotubes, guaranteeing that all carbon nanotubes participate in the reaction, resulting in more uniform purification. The supercritical fluid, containing the co-solvent, dissolves impurities on the surface of the carbon nanotubes. The pressure inside the reactor is then slowly reduced using a staged pressure reducing valve. Force is applied to allow the impurity-containing supercritical fluid to enter the post-treatment system. The first valve is opened, allowing the impurity-containing gas to circulate in the closed-loop system. The drive motor is started, and the stirring shaft drives the multi-layer blade assembly to rotate, which in turn drives the scraper to remove the material adhering to the vessel wall. Finally, the second valve is opened, and the purified single-walled carbon nanotubes are discharged into the collection tank. Through the above steps, the process avoids corroding the surface of carbon nanotubes or introducing defects such as carboxyl and hydroxyl groups, unlike strong acids. It effectively preserves the original structure and excellent electrical and mechanical properties of single-walled carbon nanotubes, solving the problem of decreased conductivity caused by existing acid washing methods.

[0032] Other features and advantages of this invention will be set forth in the description which follows, and will be apparent in part from the description, or may be learned by practicing the invention. The objectives and other advantages of this invention are realized and obtained through the structures particularly pointed out in the description and the accompanying drawings.

[0033] To make the above-mentioned objectives, features and advantages of this utility model more apparent and understandable, preferred embodiments are described below in detail with reference to the accompanying drawings. Attached Figure Description

[0034] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0035] Figure 1 This is a perspective view of a preferred embodiment of the present invention.

[0036] Figure 2 This is a perspective view of a preferred embodiment of the stirring mechanism of this utility model.

[0037] In the picture:

[0038] High-pressure reactor 1, reactor body 101, reactor cover 102, feed inlet 103, sealing cover 104, clamp 105;

[0039] 2. Stirring mechanism, 201. Blade assembly, 202. Stirring blade, 2021. Bearing housing, 203. Drive motor, 204. Scraper, 205.

[0040] 3. Stage pressure reducing valve; 4. First valve; 5. Second valve; 6. Three-way valve. Detailed Implementation

[0041] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model. Example 1

[0042] like Figures 1 to 2 As shown, this embodiment provides a purification device for single-walled carbon nanotubes, comprising:

[0043] The reactor comprises a high-pressure reactor 1 and a stirring mechanism 2 mounted on the high-pressure reactor 1; wherein the high-pressure reactor 1 is adapted to be connected to a supercritical fluid system; the stirring mechanism 2 is adapted to stir and mix the supercritical fluid within the high-pressure reactor 1; a staged pressure reducing valve 3, one end of which is connected to a pipeline of the high-pressure reactor 1, and the other end of which is connected to a pipeline of the post-treatment system; a first valve 4, one end of which is connected to a pipeline of the high-pressure reactor 1, and the other end of which is connected to a pipeline of the closed-loop system; a second valve 5, one end of which is connected to a pipeline of the high-pressure reactor 1, and the other end of which is connected to a pipeline of the collection tank; wherein the high-pressure reactor 1 is preferably designed to withstand pressure greater than or equal to 30 MPa and has an inner wall coated with a polytetrafluoroethylene anti-corrosion layer; wherein the supercritical fluid system consists of a fluid storage tank, a cryogenic pump, a preheater, etc., to inject supercritical fluid into the high-pressure reactor 1; wherein the supercritical fluid... CO2 is the preferred choice; the staged pressure reducing valve 3 is preferably a three-stage pressure reducing valve 3, driven by piezoelectric ceramic, with a fast response time, to control the slow release of pressure in the high-pressure reactor 1, avoiding sudden phase change of the supercritical fluid (such as from supercritical state to gaseous state) due to a sudden pressure drop, preventing carbon nanotube agglomeration or impurity re-adsorption, and protecting the post-treatment system from high-pressure impact; the stirring mechanism 2 is set to ensure full contact between the supercritical fluid and carbon nanotubes, improving the impurity dissolution rate; the first valve 4 and the second valve 5 are, but are not limited to, remotely controllable valves; when the first valve 4 is opened, the supercritical fluid vaporizes and carries impurities through the closed-loop system for safe recovery and harmless treatment; when the second valve 5 is opened, the purified single-walled carbon nanotubes are discharged into the collection tank, realizing product separation.

[0044] The high-pressure reactor 1 includes a reactor body 101 and a reactor cover 102 for sealing the reactor body 101; the stirring mechanism 2 includes a stirring shaft 201 disposed within the reactor body 101 and several layers of blade groups 202 disposed on the stirring shaft 201; wherein the upper part of the stirring shaft 201 passes through the reactor cover 102 and is connected to the reactor cover 102 bearing; and each layer of the blade group 202 includes at least three circularly arranged stirring blades 2021; each stirring blade 2021 is disposed on the stirring shaft 201; wherein the rotation of each stirring blade 2021 causes the supercritical fluid to mix with the carbon nanotubes, thereby enhancing the mass transfer efficiency, ensuring sufficient contact between the supercritical fluid and the carbon nanotubes, and improving the impurity dissolution rate.

[0045] The stirring mechanism 2 further includes: a bearing seat 203 disposed on the lid 102 and a drive motor 204 disposed on the bearing seat 203; wherein the bearing seat 203 is sleeved on the stirring shaft 201 and is connected to the stirring shaft 201 bearing; the output shaft of the drive motor 204 is connected to the stirring shaft 201 to drive the stirring shaft 201 to rotate; wherein by setting the bearing seat 203, the stirring shaft 201 is fixed, the radial shaking during rotation is reduced, and the stirring stability is ensured.

[0046] A three-way valve 6 is connected to a pipe on one side of the vessel body 101; the other two ends of the three-way valve 6 are respectively connected to the pipes of the supercritical fluid system and the cosolvent injection unit; by setting the three-way valve 6 to connect the vessel body 101, the supercritical fluid system and the cosolvent injection unit, supercritical fluid and cosolvent (such as ethanol, acetone) can be introduced alone or simultaneously; the cosolvent can enhance the solubility of supercritical fluid for specific impurities (such as metal catalyst residue, amorphous carbon), and the ratio of the two can be flexibly adjusted by the three-way valve 6 to meet the purification requirements of different impurity components.

[0047] The high-pressure reactor 1 further includes: an inlet 103 communicating with the top of the reactor cover 102, a sealing cover 104 covering the inlet 103, and a clamp 105 for connecting the inlet 103 and the sealing cover 104; wherein the clamp 105 fixes the sealing cover 104 to ensure the airtightness of the high-pressure environment; the inlet 103 is used to feed in the single-walled carbon nanotube raw material to be purified, and the sealing cover 104 and the clamp 105 ensure that the pressure inside the reactor does not leak after the material is fed in.

[0048] The stirring mechanism 2 further includes: at least three circular arrays of scrapers 205 disposed within the vessel body 101; wherein the scrapers 205 are connected to the corresponding stirring blades 2021 of each layer of blade group 202; the other side of the scrapers 205 contacts the inner wall of the vessel body 101; wherein the scrapers 205 are connected to the stirring blades 2021 and rotate synchronously with the stirring blades 2021, and one side of the scrapers contacts the inner wall of the vessel body 101 to scrape off the carbon nanotubes attached to the inner wall of the vessel body 101, thereby avoiding material waste; wherein the scrapers 205 are made of, but are not limited to, rubber.

[0049] The first valve 4 is connected to the vessel cover 102; the staged pressure reducing valve 3 is connected to a pipe on one side of the vessel body 101; and the second valve 5 is connected to a pipe at the bottom of the vessel body 101.

[0050] In this embodiment, the sealing cap 104 is opened, and the single-walled carbon nanotubes to be purified are introduced into the reactor body 101 through the feed port 103. The sealing cap 104 is then closed and sealed with a clamp 105. Supercritical fluid and a co-solvent are introduced into the reactor body 101 through the three-way valve 6 to bring the reactor body 101 to a preset pressure, forming a stable supercritical environment. The drive motor 204 is started, and the stirring shaft 201 drives the multi-layer blade assembly 202 to rotate. The stirring blades 2021 thoroughly mix the supercritical fluid with the carbon nanotubes, ensuring that all carbon nanotubes participate in the reaction, resulting in more uniform purification. The supercritical fluid containing the co-solvent dissolves impurities on the surface of the carbon nanotubes. Through graded reduction... Pressure valve 3 slowly reduces the pressure inside the vessel, allowing the supercritical fluid containing impurities to enter the post-treatment system. First valve 4 is opened, allowing the gas containing impurities to circulate in the closed-loop system. Drive motor 204 is started, and stirring shaft 201 drives multi-layer blade assembly 202 to rotate, which in turn drives scraper 205 to scrape off the material adhering to the vessel wall. Finally, second valve 5 is opened to discharge the purified single-walled carbon nanotubes into the collection tank. Through the above steps, the process avoids corroding the surface of carbon nanotubes or introducing defects such as carboxyl and hydroxyl groups, unlike strong acids. It effectively preserves the original structure and excellent electrical and mechanical properties of single-walled carbon nanotubes, solving the problem of decreased conductivity caused by existing acid washing methods.

[0051] All the devices selected in this application (parts whose specific structures are not specified) are general standard parts or parts known to those skilled in the art. Their structures and principles can be learned by those skilled in the art through technical manuals or conventional experimental methods.

[0052] In the description of the embodiments of this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0053] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0054] In the several embodiments provided in this application, it should be understood that the disclosed systems, apparatuses, and methods can be implemented in other ways. The apparatus embodiments described above are merely illustrative. For example, the division of units is only a logical functional division, and in actual implementation, there may be other division methods. Furthermore, multiple units or components may be combined or integrated into another system, or some features may be ignored or not executed. Additionally, the shown or discussed mutual couplings, direct couplings, or communication connections may be through some communication interfaces; indirect couplings or communication connections between devices or units may be electrical, mechanical, or other forms.

[0055] The units described as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of this embodiment according to actual needs.

[0056] In addition, in the various embodiments of this utility model, each functional unit can be integrated into one processing unit, or each unit can exist physically separately, or two or more units can be integrated into one unit.

[0057] Based on the above-described preferred embodiments of this utility model, and through the foregoing description, those skilled in the art can make various changes and modifications without departing from the technical concept of this utility model. The technical scope of this utility model is not limited to the contents of the specification, but must be determined according to the scope of the claims.

Claims

1. A purification device for single-walled carbon nanotubes, characterized in that, include: High-pressure reactor (1) and stirring mechanism (2) installed on high-pressure reactor (1); in The high-pressure reactor (1) is adapted to be connected to a supercritical fluid system; The stirring mechanism (2) is suitable for stirring and mixing supercritical fluids in the high-pressure reactor (1); The graded pressure reducing valve (3) is connected at one end to the pipeline of the high-pressure reactor (1) and at the other end to the pipeline of the post-treatment system; The first valve (4) is connected at one end to the pipeline of the high-pressure reactor (1) and at the other end to the pipeline of the closed-loop system; The second valve (5) is connected at one end to the pipeline of the high-pressure reactor (1) and at the other end to the pipeline of the collection tank.

2. The purification apparatus for single-walled carbon nanotubes as described in claim 1, characterized in that, The high-pressure reactor (1) includes: a reactor body (101) and a reactor cover (102) for sealing the reactor body (101). The stirring mechanism (2) includes: a stirring shaft (201) disposed within the vessel body (101) and a plurality of blade groups (202) disposed on the stirring shaft (201); wherein The upper part of the stirring shaft (201) penetrates through the vessel cover (102) and is connected to the vessel cover (102) bearing; and Each layer of the blade assembly (202) includes: at least three stirring blades (2021) arranged in a circular array; Each of the stirring blades (2021) is mounted on the stirring shaft (201).

3. The purification apparatus for single-walled carbon nanotubes as described in claim 2, characterized in that, The stirring mechanism (2) further includes: a bearing seat (203) disposed on the lid (102) and a drive motor (204) disposed on the bearing seat (203); wherein The bearing housing (203) is sleeved on the stirring shaft (201) and connected to the bearing of the stirring shaft (201); The output shaft of the drive motor (204) is connected to the stirring shaft (201) to drive the stirring shaft (201) to rotate.

4. The purification apparatus for single-walled carbon nanotubes as described in claim 3, characterized in that, A three-way valve (6) is connected to a pipe on one side of the vessel body (101); wherein The other two ends of the three-way valve (6) are respectively connected to the supercritical fluid system and the co-solvent injection unit pipeline.

5. The purification apparatus for single-walled carbon nanotubes as described in claim 4, characterized in that, The high-pressure reactor (1) further includes: an inlet (103) communicating with the top of the reactor cover (102), a sealing cap (104) covering the inlet (103), and a clamp (105) for connecting the inlet (103) and the sealing cap (104).

6. The purification apparatus for single-walled carbon nanotubes as described in claim 5, characterized in that, The stirring mechanism (2) further includes: at least three scrapers (205) arranged in a circular array within the vessel body (101); wherein The scraper (205) is connected to the corresponding stirring blades (2021) of each layer of blade group (202); The other side of the scraper (205) is in contact with the inner wall of the vessel body (101).

7. The purification apparatus for single-walled carbon nanotubes as described in claim 6, characterized in that, The first valve (4) is connected to the vessel lid (102); The graded pressure reducing valve (3) is connected to a pipe on one side of the vessel body (101); The second valve (5) is connected to the bottom pipe of the vessel body (101).

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