Purification device, purification system and purification method

Abstract

The invention discloses a purification device, a purification system and a purification method.The purification device comprises a channel, an adsorption mechanism and an electric energy supply mechanism, the channel is used for conveying a mixture containing nanometer materials, the adsorption mechanism is arranged inside the channel, and the electric energy supply mechanism is arranged inside or outside the channel; the electric energy supply mechanism is used for applying electric energy to the nanometer material so that at least part of the nanometer material in the mixture can be adsorbed to the adsorption mechanism and / or the nanometer material adsorbed to the adsorption mechanism can be promoted to be desorbed, and the purification device has the advantages of being simple in structure, good in purification effect and capable of meeting the large-scale industrial production requirement. The continuous flow production of the nano material is favorably realized.

Description

Technical Field

[0001] The present application relates to the technical field of separation and purification of nanomaterials, and in particular to a purification device, a purification system and a purification method. Background Art

[0002] Nanomaterials refer to nanoparticle materials with at least one dimension in the nanometer scale (1nm to 100nm) in the three-dimensional space, or materials composed of nanoparticle materials as basic units. Nanomaterials have characteristics such as volume effect, surface effect, quantum size effect, and macroscopic quantum tunneling effect, thus showing characteristics that conventional materials do not have in terms of electricity, magnetism, and light, and can be widely used in technical fields such as semiconductor devices, environmental protection, and biomedicine.

[0003] At present, nanomaterials can be synthesized by solution method, which has the advantages of simple preparation process, easy control of process conditions, low cost and wide application range. For the solution method synthesis of nanomaterials, the product is a dispersion containing nanomaterials, and the dispersion contains impurities such as synthesis precursors, precursor solvents, reaction environment solvents, reaction by-products, etc. The product needs to be purified to obtain nanomaterials with higher purity. Conventional purification methods mainly include anti-solvent precipitation purification method and extraction purification method, which have the disadvantages of cumbersome purification process and are not conducive to the continuous flow production of nanomaterials.

[0004] Therefore, it is necessary to provide a purification device, a purification system and a purification method to simplify the purification process, which is of great significance to the continuous flow production of nanomaterials. Summary of the invention

[0005] The present application provides a purification device, a purification system and a purification method to simplify the purification process of nanomaterials.

[0006] In a first aspect, the present application provides a purification device, the purification device comprising:

[0007] A channel for conveying a mixture containing the nanomaterial;

[0008] an adsorption mechanism, disposed inside the channel; and

[0009] The electric energy supply mechanism is arranged inside or outside the channel, and is used to apply electric energy to the nanomaterial to make at least part of the nanomaterial in the mixture adsorbed on the adsorption mechanism, and / or promote the desorption of the nanomaterial adsorbed on the adsorption mechanism.

[0010] Optionally, the adsorption mechanism comprises an adsorbent; and / or

[0011] The power supply mechanism comprises a first electrode and a second electrode arranged opposite to each other, the first electrode and the second electrode are independently arranged inside or outside the channel, the first electrode and the second electrode have opposite polarities, wherein the adsorption mechanism is located between the first electrode and the second electrode; and / or

[0012] The purification device further comprises a mechanical energy supply mechanism, which is used to apply mechanical energy to the adsorption mechanism to promote desorption of the nanomaterial adsorbed on the adsorption mechanism; optionally, the mechanical energy supply mechanism is an ultrasonic generator.

[0013] Optionally, the nanomaterial includes one or more of nano metal oxide, alloy quantum dots, nano metal and nano carbon material; and / or

[0014] The adsorbent has a porous structure. Optionally, the adsorbent includes one or more of activated carbon, graphite, aluminum oxide, silicon oxide, magnesium oxide, zirconium oxide, aluminum phosphate, silicon aluminum phosphate, zeolite, beryllium oxide ceramics, adsorption resin and polyacrylamide.

[0015] Optionally, the nanomaterial is a nanoparticle material, the pore size of at least some of the pores in the porous structure is larger than the average particle size of the nanoparticle material, and the pore size of at least some of the pores in the porous structure is less than 50 μm.

[0016] In a second aspect, the present application further provides a nanomaterial purification system, the purification system comprising any one of the purification devices described in the first aspect.

[0017] Optionally, the purification device further comprises a first feed inlet and a first discharge port, wherein the first feed inlet is communicable with the channel, and the first discharge port is communicable with the channel;

[0018] The purification system also includes a first storage device, which is used to accommodate a dispersing solvent, and the dispersing solvent is used to disperse and desorb the nanomaterial from the adsorption mechanism; the first storage device is provided with a second discharge port, and the second discharge port is communicable with the first feed port; and / or, the purification system also includes a second storage device, which is used to accommodate a dispersion liquid, and the dispersion liquid contains the nanomaterial desorbed from the adsorption mechanism, and the second storage device includes a third feed port, and the third feed port is communicable with the first discharge port; and / or, the purification system also includes a third storage device, which is used to accommodate the mixture containing the nanomaterial, and the third storage device includes a fourth discharge port, and the fourth discharge port is communicable with the first feed port.

[0019] Optionally, the third storage device further comprises a fourth feed inlet, and the fourth feed inlet is communicable with the first discharge port, and / or the fourth feed inlet is communicable with the discharge port of the nano-material synthesis device.

[0020] In a third aspect, the present application provides a method for purifying a nanomaterial, which is performed by using a purification device as described in any one of the first aspects or a purification system as described in any one of the second aspects, and the purification method comprises the steps of:

[0021] A mixture containing the nanomaterial is introduced into the channel. When the mixture flows through the power supply mechanism, the power supply mechanism provides a first electric field. Under the action of the first electric field, the nanomaterial in the mixture moves toward the direction close to the adsorption mechanism, and at least part of the nanomaterial is adsorbed on the adsorption mechanism; and

[0022] Stop introducing the mixture, then introduce a dispersing solvent into the channel to desorb the nanomaterial adsorbed on the adsorption mechanism and disperse it in the dispersing solvent to obtain purified nanomaterial.

[0023] Optionally, the electric field direction of the first electric field is perpendicular to the flow direction of the mixture.

[0024] Optionally, the step of desorbing the nanomaterial adsorbed on the adsorption mechanism and dispersing it in the dispersion solvent includes: removing the first electric field, applying mechanical energy to the adsorption mechanism and / or the power supply mechanism providing a second electric field, the electric field direction of the second electric field being opposite to the electric field direction of the first electric field.

[0025] The present application provides a purification device, a purification system and a purification method, which have the following technical effects:

[0026] The purification device of the embodiment of the present application has the advantages of simple structure, good purification effect on nanomaterials, and high yield of purified nanomaterials. In addition, the purification device can meet the needs of large-scale industrial production, effectively improve the purification efficiency of nanomaterials, and is conducive to the realization of continuous flow production of nanomaterials.

[0027] The purification system of the embodiment of the present application includes the purification device, which can realize the continuous flow production of nanomaterials, meet the needs of large-scale industrial production, effectively improve the purification efficiency and output of nanomaterials, and help reduce purification costs.

[0028] The purification effect of the purification method of the embodiment of the present application on the nanomaterial is no worse than that of the traditional anti-solvent precipitation purification method and extraction purification method. Compared with the traditional anti-solvent precipitation purification method and extraction purification method, the purification method of the embodiment of the present application has a simpler operating procedure, a higher yield of purified nanomaterials, and is conducive to reducing purification costs. It is more suitable for large-scale industrial production and can realize continuous flow production of nanomaterials. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] The technical solution and other beneficial effects of the present application will be made apparent by describing in detail the specific implementation methods of the present application in conjunction with the accompanying drawings.

[0030] Figure 1 A schematic diagram of the structure of a purification device provided in an embodiment of the present application;

[0031] Figure 2 A schematic diagram of the structure of a purification system provided in an embodiment of the present application;

[0032] Figure 3 It is a weight-temperature characteristic curve diagram of the purified nano ZnO solid samples in Example 1, Example 2 and the comparative example of the present application.

[0033] The reference numerals are as follows:

[0034] 10: purification device; 20: first storage device; 30: second storage device; 40: third storage device; 100: purification system; 200: nanomaterial synthesis device; 101: channel; 102: adsorption mechanism; 103: electric energy supply mechanism; 104: mechanical energy supply mechanism; 110: discharge port of nanomaterial synthesis device; 111: first feed port; 112: first discharge port; 201: second discharge port; 301: third feed port; 401: fourth discharge port; 402: fourth feed port; 1031: first electrode; 1032: second electrode. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present application will be described clearly and completely below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present application.

[0036] Unless otherwise defined, all professional and scientific terms used herein have the same meanings as those familiar to those skilled in the art. In addition, any methods and materials similar or equivalent to those described herein may be applied to the present invention. The preferred implementation methods and materials described herein are for demonstration purposes only and are not intended to limit the content of this application.

[0037] It should be noted that the order of description of the following embodiments is not intended to limit the preferred order of the embodiments. The various embodiments of the present application may be in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the invention; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single values ​​within the range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated in this article, it is meant to include any cited numbers (fractions or integers) within the indicated range.

[0038] In the description of the present application, the term “including” means “including but not limited to”.

[0039] The term "at least one" means one or more, and "multiple" means two or more. The term "at least one", "at least one of the following" or similar expressions refer to any combination of these items, including any combination of single items or plural items. For example, "at least one of a, b or c" or "at least one of a, b and c" can be expressed as: a, b, c, ab (i.e. a and b), ac, bc or abc, where a, b and c can be single or plural, respectively.

[0040] In the present application, the description of "layer A is formed on one side of layer B" or "layer A is formed on the side of layer B away from layer C" may mean that layer A is directly formed on one side of layer B or on the side of layer B away from layer C, that is, layer A is in direct contact with layer B; it may also mean that layer A is indirectly formed on one side of layer B or on the side of layer B away from layer C, that is, other film layers may be formed between layer A and layer B.

[0041] The selection scope of the term "and / or" includes any one of two or more related listed items, and also includes any and all combinations of the related listed items, and the said any and all combinations include any combination of two related listed items, any more related listed items, or all related listed items. For example, "A and / or B" includes three parallel solutions of A, B and A+B. For another example, the technical solution of "A, and / or, B, and / or, C, and / or, D" includes any one of A, B, C, and D (that is, the technical solution connected by "logical or"), and also includes any and all combinations of A, B, C, and D, that is, the combination of any two or any three of A, B, C, and D, and also includes the combination of four items of A, B, C, and D (that is, the technical solution connected by "logical and").

[0042] The term "particle size" refers to the diameter of a nanoparticle.

[0043] The term "pore size" refers to the diameter of a pore when it is considered as a circle.

[0044] The terms "multiple", "multi-layer" or similar expressions refer to two (layers) or more, for example, three (layers), four (layers), five (layers), eight (layers), ten (layers), twenty (layers), thirty (layers), forty (layers), one hundred (layers) or a value between any two of the foregoing.

[0045] The present application embodiment provides a nanomaterial purification device for purifying nanomaterials carrying positive or negative charges, such as Figure 1 As shown, the purification device 10 includes a channel 101 , an adsorption mechanism 102 , and an electric energy supply mechanism 103 .

[0046] The channel 101 is used to transport a mixture containing nanomaterials, and the mixture may be, for example, a product of synthesizing nanomaterials by a solution method. The channel 101 may be, for example, a hollow tubular structure, and the material of the channel 101 includes, but is not limited to, one or more of glass and a first metal, wherein the first metal includes, but is not limited to, one or more of carbon-manganese steel, stainless steel, and a nickel-based alloy.

[0047] The nanomaterial carries positive or negative charge, and the amount of charge carried by the nanomaterial is not specifically limited. Those skilled in the art know how to make the nanomaterial carry the target charge. Taking nanoparticle materials as an example, the nanomaterial can be made to carry the target charge by adjusting the number of surface defect states and the polarity of the ligands; in addition, the nanomaterial can be tested by a standard zeta potential test method to detect whether it carries positive or negative charge.

[0048] In some embodiments of the present application, the nanomaterial is one or more of nanometal oxides, alloy quantum dots, nanometals, and nanocarbon materials. The nanometal oxides may be doped or undoped. The undoped nanometal oxides are selected, for example, from ZnO, TiO2, SnO2, BaO, Ta2O3, Al2O3, ZrO2, nickel oxide, molybdenum oxide, tungsten oxide, chromium oxide, or copper oxide, wherein NiO is exemplified as nickel oxide, MoO3 as molybdenum oxide, WO3 as tungsten oxide, V2O5 as vanadium oxide, and CuO or Cu2O as copper oxide; the doped nanometal oxides are selected, for example, from one or more of zinc magnesium oxide, zinc calcium oxide, zinc zirconium oxide, zinc gallium oxide, zinc aluminum oxide, zinc lithium oxide, zinc titanium oxide, yttrium zinc oxide, indium tin oxide, and titanium lithium oxide, wherein Zn is exemplified as (1-x) Mg x O, Zn (1-x) Ca x O, Zn (1-x) Zr x O, Zn (1-x) Ga x O, Zn (1-x) Al x O, Zn (1-x) Li x O、Al (1-x) Zn x O, Zn (1-x) Ti x O, Zn (1-x) Y x O、In (1-x) Sn x O and Ti (1-x) Li xO, wherein 0<x≤0.5. The alloy quantum dots may be single-component quantum dots or core-shell structure quantum dots, and the material of the single-component quantum dots, the material of the core of the core-shell structure quantum dots or the material of the shell of the core-shell structure quantum dots is, but is not limited to, at least one of a II-VI group compound, a III-V group compound, a IV-VI group compound or a I-III-VI group compound, wherein the II-VI group compound is selected from CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, ZnO, HgS, HgSe, HgTe, CdSeS, CdSeTe, CdSTe, ZnSeS, ZnSeTe, ZnSTe, HgSeS, HgSeTe, HgSTe, CdZn S, CdZnSe, CdZnTe, CdHgS, CdHgSe, CdHgTe, HgZnS, HgZnSe, HgZnTe, CdZnSeS, CdZnSeTe, CdZnSTe, CdHgSeS, CdHgSeTe, CdHgSTe, HgZnSeS, HgZnSeTe and HgZnSTe, and the III-V compound is selected from GaN, GaP, GaAs, GaSb, AlN, AlP, AlAs, AlSb, InN, InP, InAs, InSb, GaNP, GaNAs, GaNSb, GaPAs, GaPSb, AlNP , AlNAs, AlNSb, AlPAs, AlPSb, InNP, InNAs, InNSb, InPAs, InPSb, GaAlNP, GaAlNAs, GaAlNSb, GaAlPAs, GaAlPSb, GaInNP, GaInNAs, GaInNSb, GaInPAs, GaInPSb, InAlNP, InAlNAs, InAlNSb, InAlPAs and InAlPSb, and the IV-VI group compound is selected from SnS, SnSe, SnTe, PbS, PbSe, PbTe, SnSeS, SnSeTe, SnSTe, One or more of PbSeS, PbSeTe, PbSTe, SnPbS, SnPbSe, SnPbTe, SnPbSSe, SnPbSeTe and SnPbSTe, and the I-III-VI group compound is selected from one or more of CuInS, CuInSe and AgInS. It should be noted that for the material of the aforementioned single-component quantum dot, or the material of the core of the core-shell structure quantum dot, or the material of the shell of the core-shell structure quantum dot, the chemical formula provided only indicates the elemental composition, and does not indicate the content of each element. For example, CdZnSe only indicates that it is composed of three elements: Cd, Zn and Se. If the content of each element is indicated, it corresponds to Cd x Zn 1-xSe, where 0 < x < 1. The metal element in the nanometal is selected from one or more of the metals in Group IA, Group IIA, Group IIIA, Group IVA, Group VA, and transition metals.

[0049] The adsorption mechanism 102 is disposed inside the channel 101. In some embodiments of the present application, the adsorption mechanism 102 includes an adsorbent for adsorbing at least part of the nanomaterials in the mixture. Among them, the adsorbent has a porous structure, and the adsorbent includes, but is not limited to, one or more of activated carbon, graphite, alumina, silica, magnesia, zirconia, aluminum phosphate, aluminosilicate phosphate, zeolite, beryllium oxide ceramic, adsorption resin, and polyacrylamide. The adsorption mechanism 102 can be, for example, a layered structure, and the adsorption mechanism 102 can be disposed inside the channel by non-detachable fixing methods such as bonding and welding or detachable fixing methods such as clamping; as an example, the adsorption mechanism 102 is bonded to the inner wall of the channel 101.

[0050] When the nanomaterials are nanoparticle materials and the adsorbent has a porous structure, in order to balance improving the adsorption effect and the purity of the nanomaterials after purification, in some embodiments of the present application, the aperture of at least part of the pores in the porous structure is larger than the average particle size of the nanoparticle materials to improve the adsorption stability, and the aperture of at least part of the pores in the porous structure is less than 50 μm, such as less than 40 μm, less than 30 μm, less than 20 μm, less than 10 μm, less than 1 μm, less than 0.5 μm, or less than 0.1 μm, to reduce the wettability of the mixture to the adsorbent, thereby improving the purity of the nanoparticle materials.

[0051] The electric energy supply mechanism 103 is used to apply electric energy to the nanomaterials so that at least part of the nanomaterials in the mixture are adsorbed on the adsorption mechanism, and / or to promote the desorption of the nanomaterials adsorbed on the adsorption mechanism 102. The electric energy supply mechanism 103 is disposed inside or outside the channel 101. In some embodiments of the present application, continue to refer to Figure 1 , the electric energy supply mechanism 103 includes a first electrode 1031 and a second electrode 1032 that are oppositely arranged. The first electrode 1031 and the second electrode 1032 are independently disposed inside or outside the channel 101, and the polarities of the first electrode 1031 and the second electrode 1032 are opposite.

[0052] Among them, the materials of the first electrode 1031 and the second electrode 1032 are independently selected from one or more of a second metal, a carbon material and a metal oxide, wherein the metal includes but is not limited to one or more of Al, Ag, Cu, Mo, Au, Ba, Pt, Ca, Ir, Ni and Mg, the carbon material includes but is not limited to one or more of graphite, carbon nanotubes, graphene and carbon fiber, and the second metal oxide includes but is not limited to one or more of indium tin oxide (ITO), fluorine-doped tin oxide (FTO), antimony tin oxide (ATO), aluminum-doped zinc oxide (AZO), gallium-doped zinc oxide (GZO), indium-doped zinc oxide (IZO), magnesium-doped zinc oxide (MZO), SnO2, ZnO and In2O3. The first electrode 1031 and the second electrode 1032 may also be composite electrodes, which have a structure similar to a "sandwich", wherein the materials of the upper and lower layers are respectively doped or undoped transparent metal oxides, and the material of the middle layer is metal, for example, it may be one or more of AZO / Ag / AZO, AZO / Al / AZO, ITO / Ag / ITO, ITO / Al / ITO, ZnO / Ag / ZnO, ZnO / Al / ZnO, TiO2 / Ag / TiO2, TiO2 / Al / TiO2, ZnS / Ag / ZnS, ZnS / Al / ZnS, TiO2 / Ag / TiO2, and TiO2 / Al / TiO2. The first electrode 1031 and the second electrode 1032 may be strip electrodes respectively.

[0053] It should be noted that the first electrode 1031 and the second electrode 1032 can be disposed inside the channel 101 at the same time, or disposed outside the channel 101 at the same time, or one of them can be disposed inside the channel 101 and the other can be disposed outside the channel 101. In order to improve the service life of the first electrode 1031 and the second electrode 1032, in some embodiments of the present application, the first electrode 1031 and the second electrode 1032 are respectively disposed outside the channel 101. Figure 1 , the first electrode 1031 and the second electrode 1032 are, for example, respectively disposed on the outer wall of the channel 101, and the adsorption mechanism 102 is disposed on the inner wall of the channel 101 corresponding to the position of the first electrode 1031 so that the adsorption mechanism 102 is close to the first electrode 1031. It is understandable that the adsorption mechanism 102 can also be disposed on the inner wall of the channel 101 corresponding to the position of the second electrode 1032 so that the adsorption mechanism 102 is close to the second electrode 1032.

[0054] In addition, when the first electrode 1031 or the second electrode 1032 is arranged inside the channel 101, for the convenience of operation, in some embodiments of the present application, the first electrode 1031 or the second electrode 1032 is arranged on the inner wall of the channel 101, and the adsorption mechanism 102 is arranged on the side of the first electrode 1031 away from the inner wall of the channel 101, or the adsorption mechanism 102 is arranged on the side of the second electrode 1032 away from the inner wall of the channel 101.

[0055] In order to promote the desorption of the nanomaterial adsorbed on the adsorption mechanism 102, thereby improving the yield of the purified nanomaterial, in some embodiments of the present application, continue to refer to Figure 1 The purification device 10 further includes a mechanical energy supply mechanism 104, which is used to apply mechanical energy to the adsorption mechanism 102 to desorb the nanomaterial adsorbed on the adsorption mechanism 102. As an example, the mechanical energy supply mechanism 104 is an ultrasonic generator.

[0056] It should be noted that the mechanical energy supply mechanism 104 can be arranged inside or outside the channel 101. When the mechanical energy supply mechanism 104 is arranged inside the channel 101, the mechanical energy supply mechanism 104 can be directly connected to the adsorption mechanism 102. The mechanical energy supply mechanism 104 can also be indirectly connected to the adsorption mechanism 102 through the first electrode 1031 or the second electrode 1032. For example, the mechanical energy supply mechanism 104 is arranged on the inner wall of the channel 101, the first electrode 1031 is arranged on the side of the mechanical energy supply mechanism 104 away from the inner wall, and the adsorption mechanism 102 is arranged on the side of the first electrode 1031 away from the mechanical energy supply mechanism 104. When the mechanical energy supply mechanism 104 is arranged outside the channel 101, the mechanical energy supply mechanism 104 is indirectly connected to the adsorption mechanism 102 through the first electrode 1031 or the second electrode 1032. For example, continue to refer to Figure 1 The first electrode 1031 is disposed on the outer wall of the channel 101, the adsorption mechanism 102 is disposed on the inner wall of the channel 101 corresponding to the position of the first electrode 1031, and the mechanical energy supply mechanism 104 is disposed on the side of the first electrode 1031 away from the outer wall.

[0057] The purification principle of the nanomaterial by the purification device of the embodiment of the present application is as follows: a mixture containing nanomaterials passes through the purification device, and the mixture enters the channel 101. When the mixture flows through the power supply mechanism 103, the power supply mechanism 103 provides a first electric field (for example, a first electric field is formed between the first electrode 1031 and the second electrode 1032). Under the action of the first electric field, the nanomaterials in the mixture move toward the direction close to the adsorption mechanism 102, and at least part of the nanomaterials are adsorbed on the adsorption mechanism 102; when the adsorption mechanism 102 reaches a preset adsorption level, the mixture is stopped from being introduced, and then a dispersing solvent is introduced into the channel; then, the first electric field is removed, so that the nanomaterials adsorbed on the adsorption mechanism 102 are desorbed and dispersed in the dispersing solvent, thereby obtaining purified nanomaterials. During the desorption process, the power supply mechanism 103 can provide a second electric field (for example, a second electric field is formed between the first electrode 1031 and the second electrode 1032, and the electric field direction of the second electric field is opposite to the electric field direction of the first electric field) and / or apply mechanical energy to the adsorption mechanism 102 to promote rapid desorption of nanomaterials.

[0058] The purification device of the embodiment of the present application has the advantages of simple structure, good purification effect on nanomaterials, and high yield of purified nanomaterials. In addition, the purification device can meet the needs of large-scale industrial production, effectively improve the purification efficiency of nanomaterials, and is conducive to the realization of continuous flow production of nanomaterials.

[0059] The present application also provides a nanomaterial purification system, such as Figure 2 As shown, the purification system 100 includes any one of the purification devices 10 described above.

[0060] In some embodiments of the present application, the purification device 10 includes a first feed port 111 and a first discharge port 112, wherein the first feed port 111 is connectable with the channel 101, the first discharge port 112 is connectable with the channel 101, the first feed port 111 may be one or more, and the first discharge port 112 may be one or more. It should be noted that "connectable" means that A and B can always maintain a connected state; or, A and B are conditionally connected and are not always in a connected state.

[0061] In some embodiments of the present application, see Figure 2The purification system 100 further includes a first storage device 20, which is used to contain a dispersion solvent. As described above, the dispersion solvent is used to disperse and desorb the nanomaterials adsorbed by the adsorption mechanism 102, so as to facilitate the collection of purified nanomaterials. The first storage device 20 includes one or more second outlets 201, and the second outlets 201 can be connected to the first inlet 111. Specifically, the second outlet 201 and the first inlet 111 can be connected by a pipeline, and one or more of a manual valve, an automatic valve and a flow meter can be set on the pipeline. The second outlet 201 can be connected to the first inlet 111 by opening the valve, and the second outlet 201 can be isolated from the first inlet 111 by closing the valve. It can be understood that the first storage device 20 may also include one or more second feed ports (not marked) to facilitate the feeding of dispersed solvent; in addition, the first storage device 20 may also be configured with a liquid level sensor, and the liquid level sensor may include an alarm module. When the liquid level in the first storage device 20 is lower than a preset value, the liquid level sensor will alert the operator.

[0062] In some embodiments of the present application, see Figure 2 The purification system 100 also includes a second storage device 30, which is used to accommodate a dispersion liquid, and the dispersion liquid includes the nanomaterial desorbed from the adsorption mechanism 102 and a dispersion solvent. The second storage device 30 includes one or more third feed ports 301, and the third feed port 301 can be connected to the first discharge port 112. Specifically, the third feed port 301 and the first discharge port 112 can be connected by a pipeline, and one or more manual valves, automatic valves and flow meters can be set on the pipeline. It can be understood that the second storage device 30 can also include one or more third discharge ports (not shown) to facilitate the discharge of the dispersion liquid; in addition, the second storage device 30 can also be configured with a liquid level sensor.

[0063] In some embodiments of the present application, see Figure 2 The purification system 100 further includes a third storage device 40, which is used to contain a mixture containing nanomaterials, and the mixture can be, for example, a product of synthesizing nanomaterials by a solution method. The third storage device 40 includes one or more fourth discharge ports 401, and the fourth discharge ports 401 can be connected to the first feed port 111. Specifically, the fourth discharge port 401 can be connected to the first feed port 111 through a pipeline, and one or more of a manual valve, an automatic valve, and a flow meter can be set on the pipeline. It can be understood that the third storage device 40 can also be configured with a liquid level sensor.

[0064] Further, see Figure 2The third storage device 40 further includes one or more fourth inlets 402, and the fourth outlet 401 can be connected to the first outlet 112 to realize the recycling of the mixture, thereby saving resources and improving economic benefits. Specifically, the fourth outlet 401 can be connected to the first outlet 112 through a pipeline, and one or more of a manual valve, an automatic valve and a flow meter can be set on the pipeline.

[0065] In order to achieve continuous flow production of nanomaterials, in some embodiments of the present application, please refer to Figure 2 The fourth feed port 402 can be connected to the discharge port 110 of the nanomaterial synthesis device 200. Specifically, the fourth feed port 402 can be connected to the discharge port 110 of the nanomaterial synthesis device through a pipeline, and one or more of a manual valve, an automatic valve and a flow meter can be set on the pipeline.

[0066] It should be noted that the purification system 100 can also be added with a PLC control mechanism to improve the level of automated operation of the purification system 100. The PLC control mechanism includes a main control module, an information processing module, a storage module, and a communication module, wherein the main control module includes an artificial intelligence control touch screen, and each pipeline branch is provided with an automatic valve that is communicatively connected to the PLC control mechanism. The communication module of the PLC control mechanism can establish a communication connection with a user terminal (such as a mobile phone, a computer, etc.) through a wireless network.

[0067] by Figure 2Taking the purification system 100 shown in the figure as an example, the purification principle of the nanomaterial by the purification system 100 of the embodiment of the present application is as follows: the fourth outlet 401 of the third storage device 40 is connected to the first inlet 111 of the purification device 10, and the fourth inlet 402 of the third storage device 40 is connected to the first outlet 112 of the purification device 10, and the second outlet 201 of the first storage device 20 is disconnected from the first inlet 111 of the purification device 10, and the third inlet 301 of the second storage device 30 is disconnected from the first outlet 112 of the purification device 10, so that the mixture containing the nanomaterial in the third storage device 40 enters the purification device 10 through the fourth outlet 401 and the first inlet 111 to perform the adsorption process, and the fluid discharged from the first outlet 112 flows back to the third storage device 40, and the fourth inlet 402 can be connected to the outlet 110 of the nanomaterial synthesis device to continuously replenish the mixture. When the adsorption mechanism 102 reaches a preset adsorption degree, the fourth discharge port 401 of the third storage device 40 is disconnected from the first feed port 111 of the purification device 10, and the second discharge port 201 of the first storage device 20 is connected to the first feed port 111 of the purification device 10, so that the dispersed solvent in the first storage device 20 enters the purification device 10 through the second discharge port 201 and the first feed port 111. When the mixture in the channel of the purification device 10 is fully replaced by the dispersed solvent, the fourth feed port 402 is disconnected from the first discharge port 112, and the first electric field is removed, so that the nanomaterial adsorbed on the adsorption mechanism 102 is desorbed and dispersed in the dispersed solvent, thereby obtaining a purified nanomaterial; finally, the second discharge port 201 is disconnected from the first feed port 111, and the third feed port 301 is connected to the first feed port 111, so that the dispersed liquid containing the purified nanomaterial enters the third storage device 40.

[0068] The purification system of the embodiment of the present application can realize the continuous flow production of nanomaterials, meet the needs of large-scale industrial production, effectively improve the purification efficiency and output of nanomaterials, and help reduce purification costs.

[0069] The present application also provides a method for purifying nanomaterials, which can be purified by using any of the purification devices or any of the purification systems described above. The purification method comprises the following steps:

[0070] S1. A mixture containing nanomaterials is introduced into the channel 101. When the mixture flows through the power supply mechanism 103, the power supply mechanism 103 provides a first electric field. Under the action of the first electric field, the nanomaterials in the mixture move toward the direction close to the adsorption mechanism 102, and at least part of the nanomaterials are adsorbed on the adsorption mechanism 102.

[0071] S2. Stop introducing the mixture, and then introduce a dispersing solvent into the channel 101 to desorb the nanomaterial adsorbed on the adsorption mechanism 102 and disperse it in the dispersing solvent to obtain purified nanomaterial.

[0072] In step S1, for "under the action of the first electric field, the nanomaterials in the mixture move toward the direction close to the adsorption mechanism, and at least part of the nanomaterials are adsorbed on the adsorption mechanism", the electric field direction of the first electric field remains unchanged, but the electric field strength can be constant or variable, that is, the direction of the electric field force on the nanomaterial in the first electric field is unchanged, but the magnitude of the electric field force on the nanomaterial in the first electric field can be constant or variable. In some embodiments of the present application, the power supply mechanism 103 includes a first electrode 1031 and a second electrode 1032 arranged opposite to each other, the first electrode 1031 and the second electrode 1032 are independently arranged inside or outside the channel 101, the polarities of the first electrode 1031 and the second electrode 1032 are opposite, the adsorption mechanism 102 is located between the first electrode 1031 and the second electrode 1032, and the first electric field is formed between the first electrode 1031 and the second electrode 1032.

[0073] It can be understood that when the first electrode 1031 is arranged on the inner wall of the channel 101 and the adsorption mechanism 102 is arranged on the side of the first electrode 1031 away from the inner wall of the channel 101, or when the first electrode 1031 is arranged on the outer wall of the channel 101 and the adsorption mechanism 102 is arranged on the inner wall of the channel 101 corresponding to the position of the first electrode 1031, if the nanomaterial carries a positive charge, then for the first electric field formed between the first electrode 1031 and the second electrode 1032, the direction of the first electric field is from the second electrode 1032 to the first electrode 1031; if the nanomaterial carries a negative charge, the direction of the first electric field is from the first electrode 1031 to the second electrode 1032. It can be understood that when the second electrode 1032 is arranged on the inner wall of the channel 101 and the adsorption mechanism 102 is arranged on the side of the second electrode 1032 away from the inner wall of the channel 101, or when the second electrode 1032 is arranged on the outer wall of the channel 101 and the adsorption mechanism 102 is arranged on the inner wall of the channel 101 corresponding to the position of the second electrode 1032, the situation of the first electric field can refer to the above.

[0074] The electric field direction of the first electric field and the flow direction of the mixture may be parallel or at a specific angle, and the angle may be, for example, 30°, 45°, 60°, or 90°. In order to facilitate the control of process conditions and simplify the operation, in some embodiments of the present application, the electric field direction of the first electric field is perpendicular to the flow direction of the mixture. The electric field strength of the first electric field may be, for example, 0.1 V / cm to 20 V / cm.

[0075] In step S2, the dispersing solvent may be an inorganic solvent or an organic solvent, wherein the inorganic solvent is, but is not limited to, water, and the organic solvent is, but is not limited to, one or more of alkanes, aromatic hydrocarbons, halogenated alkanes, alcohol compounds, ether compounds, furan compounds, pyridine compounds, and amide compounds, wherein the alkanes are, but are not limited to, nonane, decane, dodecane, terpene, butylcyclohexane, n-octane, n-hexane, n-heptane, n-nonane, n-decane, cyclohexane, and cyclopentane, and the aromatic hydrocarbons are, but are not limited to, diethylbenzene, trimethylolbenzene, cyclopentane ... One or more of benzene, propylbenzene, isopropylbenzene, p-toluene isopropylbenzene, butylbenzene and 1-methylnaphthalene or indene; halogenated alkanes include but are not limited to one or more of dichloromethane, chloroform and carbon tetrachloride; alcohol compounds include but are not limited to one or more of methanol, ethanol, propanol, butanol, ethylene glycol and glycerol; ether compounds include but are not limited to ethylene glycol monomethyl ether; furan compounds include but are not limited to tetrahydrofuran; pyridine compounds include but are not limited to pyridine; amide compounds include but are not limited to N,N-dimethylformamide.

[0076] As for step S2, it can be understood that the introduction of the mixture can be stopped when the adsorbent in the adsorption mechanism 102 reaches the adsorption saturation state, and of course, the introduction of the mixture can be stopped when the adsorbent in the adsorption mechanism 102 is not adsorbed saturated. When the conductivity of the adsorption mechanism 102 is stable or the concentration of the nanomaterial in the dispersed solvent is stable, it is proved that the adsorbent has reached the adsorption saturation state.

[0077] In step S2, in order to improve the efficiency and effect of desorption and increase the yield of nanomaterials, in some embodiments of the present application, after the first electric field is removed, mechanical energy is applied to the adsorption mechanism 102 and / or the electric energy supply mechanism 103 provides a second electric field, and the electric field direction of the second electric field is opposite to the electric field direction of the first electric field, so as to promote the desorption of the nanomaterials and dispersion in the dispersion solvent. The mechanical energy supply mechanism 104 mentioned above can be used to apply mechanical energy to the adsorption mechanism 102.

[0078] In some embodiments of the present application, the power supply mechanism 103 includes a first electrode 1031 and a second electrode 1032 arranged opposite to each other, and the first electrode 1031 and the second electrode 1032 are, for example, strip electrodes. When a second electric field is formed between the first electrode 1031 and the second electrode 1032, the electric field direction of the second electric field remains unchanged, but the electric field strength may be constant or variable, that is, the direction of the electric field force received by the nanomaterial in the second electric field remains unchanged, but the magnitude of the electric field force received by the nanomaterial in the second electric field may be constant or variable, and the direction of the electric field force received by the nanomaterial in the second electric field is opposite to the direction of the electric field force received by the nanomaterial in the first electric field, so as to achieve desorption. The electric field strength of the second electric field may be, for example, 0.1V / cm to 20V / cm.

[0079] When the first electrode 1031 is disposed on the inner wall of the channel 101 and the adsorption mechanism 102 is disposed on the side of the first electrode 1031 away from the inner wall of the channel 101, or when the first electrode 1031 is disposed on the outer wall of the channel 101 and the adsorption mechanism 102 is disposed on the inner wall of the channel 101 corresponding to the position of the first electrode 1031, if the nanomaterial carries a positive charge, the direction of the second electric field is from the first electrode 1031 to the second electrode 1032; if the nanomaterial carries a negative charge, the direction of the second electric field is from the second electrode 1032 to the first electrode 1031. It can be understood that when the second electrode 1032 is disposed on the inner wall of the channel 101 and the adsorption mechanism 102 is disposed on the side of the second electrode 1032 away from the inner wall of the channel 101, or when the second electrode 1032 is disposed on the outer wall of the channel 101 and the adsorption mechanism 102 is disposed on the inner wall of the channel 101 corresponding to the position of the second electrode 1032, the situation of the second electric field can refer to the above.

[0080] It should be noted that for the above purification process, when the adsorption mechanism 102 is detachably fixed to the channel 101, the adsorption mechanism 102 can be firstly disassembled and then further processed separately to obtain purified nanomaterials.

[0081] The technical scheme and technical effects of the present application are described in detail below through specific embodiments, comparative examples and experimental examples. The following embodiments are only some embodiments of the present application and do not specifically limit the present application.

[0082] Example 1

[0083] This embodiment provides a nanomaterial purification device and a nanomaterial purification method, wherein the purification device has the following features: Figure 1 The structure shown in FIG. 1 is a hollow tubular structure, and the length of the channel 101 is 8 cm; the adsorption mechanism 102 is a layered structure, the thickness of the adsorption mechanism 102 is 1 cm, and the material of the adsorption mechanism 102 is a silicon oxide ceramic with a porous structure (pore size distribution is 10 μm to 50 μm); the first electrode 1031 and the second electrode 1032 are relatively arranged on the outer wall of the channel 101, and the interval between the first electrode 1031 and the second electrode 1032 is 10 cm, the second electrode 1032 is located above the first electrode 1031, and the adsorption mechanism 102 is arranged on the inner wall of the channel 101 corresponding to the position of the first electrode 1031; the mechanical energy supply mechanism 104 is an ultrasonic generator, and the mechanical energy supply mechanism 104 is arranged on the side of the first electrode 1031 away from the outer wall.

[0084] The mixture containing the nano material is a product of synthesizing the nano material by a solution method. The preparation method of the mixture comprises the steps of taking 3L of a 0.3mol / L zinc acetate dihydrate-DMF solution (N,N-dimethylformamide as a solvent) and placing it in a reaction container, and then injecting 3.3L of a 0.3mol / L potassium hydroxide-ethanol solution (ethanol as a solvent) into the zinc acetate dihydrate-DMF solution in the reaction container under normal temperature and pressure conditions within 2 minutes, and continuously stirring for 1 hour to obtain a mixture containing nano ZnO, and through a zeta potential test, the zeta potential of the nano ZnO is -10mV, that is, the nano ZnO in the mixture carries a negative charge.

[0085] The purification method comprises the following steps: 5L of the prepared mixture is introduced into the channel 101 of the purification device 10, a first electric field is formed between the first electrode 1031 and the second electrode 1032, the direction of the first electric field is that the first electrode 1031 points to the second electrode 1032 (that is, the first electrode 1031 is a positive electrode and the second electrode 1032 is a negative electrode), and the voltage between the first electrode 1031 and the second electrode 1032 is 50V, so that at least part of the nano ZnO is adsorbed on the adsorption mechanism 102; after the first electric field is maintained for 10 minutes, ethanol is introduced into the channel 101 of the purification device 10, so that the ethanol completely replaces the original solution, and then the first electric field is removed, and the second electric field is maintained for 10 minutes. A second electric field is formed between the first electrode 1031 and the second electrode 1032, and the direction of the second electric field is that the second electrode 1032 points to the first electrode 1031 (that is, the first electrode 1031 is the negative electrode and the second electrode 1032 is the positive electrode). The voltage between the second electrode 1032 and the first electrode 1031 is also 50V, and the ultrasonic generator (frequency is 40kHz, power is 250W) is turned on at the same time to quickly desorb the nano ZnO adsorbed on the adsorption mechanism 102 and disperse it in ethanol. The time for the second electric field and ultrasonic treatment is 5 minutes, and an ethanol solution containing purified nano ZnO is collected, wherein the purified nano ZnO is 20g.

[0086] Example 2

[0087] This embodiment provides a nanomaterial purification device and a nanomaterial purification method. Compared with the purification device in Example 1, the purification device in this embodiment is different only in that the material of the adsorption mechanism 102 is replaced by a silicon oxide ceramic with a porous structure (pore size distribution is 60μm to 100μm).

[0088] The purification method of the nanomaterial in this embodiment is carried out with reference to Example 1 to obtain an ethanol solution containing purified nano ZnO, wherein the purified nano ZnO is 20 g.

[0089] Comparative Example

[0090] This comparative example provides a method for purifying a nanomaterial, and the purification method comprises the following steps:

[0091] S1.1, taking 50 mL of a mixture containing nano ZnO (preparation method is the same as that in Example 1), adding 120 mL of ethyl acetate to the mixture, mixing to obtain a first mixed system, and then centrifuging the first mixed system at 2000 g to obtain a first precipitate;

[0092] S1.2, dispersing the first precipitate obtained in step S1.1 in 10 mL of ethanol, then adding 25 mL of heptane, mixing to obtain a second mixed system, then centrifuging the second mixed system at 2000 g, collecting and obtaining 200 mg of a second precipitate, which is purified nano-ZnO;

[0093] S1.3, dispersing the second precipitate obtained in step S1.2 in ethanol to obtain an ethanol solution containing purified nano-ZnO.

[0094] Experimental example

[0095] The purified nano ZnO in Example 1, Example 2 and the comparative example were subjected to thermogravimetric analysis (TG) test, and the solid nano ZnO sample was subjected to weight loss test using Diamond TG / DTA of Seiko Corporation of Japan to test the change of the mass of the solid nano ZnO sample with temperature at 100°C to 700°C.

[0096] like Figure 3 As shown, the weight-temperature characteristic curve of the solid-state nano ZnO sample derived from Example 1 is slightly different from the weight-temperature characteristic curve of the solid-state nano ZnO sample derived from the comparative example. It can be seen that the purity of the nano ZnO obtained by the purification device and the purification method in Example 1 is slightly different from the purity of the nano ZnO obtained by the purification method in the comparative example, indicating that the purification device and the purification method in Example 1 have good purification effects; in addition, compared with the purification method in the comparative example, the purification method in Example 1 has a simpler process, is more suitable for large-scale industrial production, and can realize continuous flow production of nano materials.

[0097] Depend on Figure 3 It can be seen that the purity of the solid nano ZnO sample from Example 2 is slightly lower than that of the solid nano ZnO sample from Example 1. The reason may be that the pore size distribution of the adsorbent is 60 μm to 100 μm, which increases the wettability of the mixture and reduces the purity of the nano ZnO.

[0098] The above is a detailed introduction to a purification device, purification system and purification method provided in the embodiments of the present application. Specific examples are used herein to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the technical solutions and core ideas of the present application; ordinary technicians in this field should understand that they can still modify the technical solutions recorded in the aforementioned embodiments, or replace some of the technical features therein by equivalents; and these modifications or replacements do not make the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A purification device, characterized in that: The purification device comprises: a channel for conveying a mixture including nanomaterials; an adsorption mechanism, disposed inside the channel; and The electric energy supply mechanism is arranged inside or outside the channel, and is used to apply electric energy to the nanomaterial to make at least part of the nanomaterial in the mixture adsorbed on the adsorption mechanism, and / or promote the desorption of the nanomaterial adsorbed on the adsorption mechanism.

2. The purification device according to claim 1, characterized in that: The adsorption mechanism comprises an adsorbent; and / or The power supply mechanism comprises a first electrode and a second electrode arranged opposite to each other, the first electrode and the second electrode are independently arranged inside or outside the channel, the first electrode and the second electrode have opposite polarities, wherein the adsorption mechanism is located between the first electrode and the second electrode; and / or The purification device further comprises a mechanical energy supply mechanism, which is used to apply mechanical energy to the adsorption mechanism to promote desorption of the nanomaterial adsorbed on the adsorption mechanism; optionally, the mechanical energy supply mechanism is an ultrasonic generator.

3. The purification device according to claim 2, characterized in that: The nanomaterial includes one or more of nano metal oxides, alloy quantum dots, nano metals and nano carbon materials; and / or The adsorbent has a porous structure. Optionally, the adsorbent includes one or more of activated carbon, graphite, aluminum oxide, silicon oxide, magnesium oxide, zirconium oxide, aluminum phosphate, silicon aluminum phosphate, zeolite, beryllium oxide ceramics, adsorption resin and polyacrylamide.

4. The purification device according to claim 3, characterized in that: The nano material is a nano particle material, the pore size of at least some of the pores in the porous structure is larger than the average particle size of the nano particle material, and the pore size of at least some of the pores in the porous structure is less than 50 μm.

5. A purification system, characterized in that: Comprising a purification device as claimed in any one of claims 1 to 4.

6. The purification system according to claim 5, characterized in that The purification device further comprises a first feed inlet and a first discharge port, wherein the first feed inlet is communicable with the channel, and the first discharge port is communicable with the channel; The purification system also includes a first storage device, which is used to accommodate a dispersing solvent, and the dispersing solvent is used to disperse and desorb the nanomaterial from the adsorption mechanism; the first storage device is provided with a second discharge port, and the second discharge port is communicable with the first feed port; and / or, the purification system also includes a second storage device, which is used to accommodate a dispersion liquid, and the dispersion liquid contains the nanomaterial desorbed from the adsorption mechanism, and the second storage device includes a third feed port, and the third feed port is communicable with the first discharge port; and / or, the purification system also includes a third storage device, which is used to accommodate the mixture containing the nanomaterial, and the third storage device includes a fourth discharge port, and the fourth discharge port is communicable with the first feed port.

7. The purification system according to claim 6, characterized in that The third storage device further comprises a fourth feed inlet, and the fourth feed inlet is communicable with the first discharge port; and / or the fourth feed inlet is communicable with the discharge port of the nano-material synthesis device.

8. A method for purifying nanomaterials, characterized in that: Purification is performed using the purification device as described in any one of claims 1 to 4 or the purification system as described in any one of claims 5 to 7, wherein the purification method comprises the steps of: A mixture containing the nanomaterial is introduced into the channel. When the mixture flows through the power supply mechanism, the power supply mechanism provides a first electric field. Under the action of the first electric field, the nanomaterial in the mixture moves toward a direction close to the adsorption mechanism, and at least part of the nanomaterial is adsorbed on the adsorption mechanism. as well as Stop introducing the mixture, then introduce a dispersing solvent into the channel to desorb the nanomaterial adsorbed on the adsorption mechanism and disperse it in the dispersing solvent to obtain purified nanomaterial.

9. The purification method according to claim 8, characterized in that The electric field direction of the first electric field is perpendicular to the flow direction of the mixture.

10. The purification method according to claim 8 or 9, characterized in that: The step of desorbing the nanomaterial adsorbed on the adsorption mechanism and dispersing it in the dispersion solvent includes: removing the first electric field, applying mechanical energy to the adsorption mechanism and / or the power supply mechanism providing a second electric field, wherein the electric field direction of the second electric field is opposite to the electric field direction of the first electric field.

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