CN112125299A - Gas-driven multi-channel laminar material stripping device - Google Patents

Gas-driven multi-channel laminar material stripping device Download PDF

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CN112125299A
CN112125299A CN201910549394.9A CN201910549394A CN112125299A CN 112125299 A CN112125299 A CN 112125299A CN 201910549394 A CN201910549394 A CN 201910549394A CN 112125299 A CN112125299 A CN 112125299A
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gas
liquid
reactor body
tubule
inlet
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张智亮
金海伦
缪鑫峰
居挺
李扬
计建炳
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/19Preparation by exfoliation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/431Straight mixing tubes with baffles or obstructions that do not cause substantial pressure drop; Baffles therefor
    • B01F25/4314Straight mixing tubes with baffles or obstructions that do not cause substantial pressure drop; Baffles therefor with helical baffles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/431Straight mixing tubes with baffles or obstructions that do not cause substantial pressure drop; Baffles therefor
    • B01F25/4316Straight mixing tubes with baffles or obstructions that do not cause substantial pressure drop; Baffles therefor the baffles being flat pieces of material, e.g. intermeshing, fixed to the wall or fixed on a central rod
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/431Straight mixing tubes with baffles or obstructions that do not cause substantial pressure drop; Baffles therefor
    • B01F25/4319Tubular elements
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C01B21/0648After-treatment, e.g. grinding, purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/06Sulfides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/431Straight mixing tubes with baffles or obstructions that do not cause substantial pressure drop; Baffles therefor
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention discloses a gas-driven layered material multi-channel stripping device, which comprises a circular reactor body with a hollow interior, wherein the reactor body is provided with an inlet pipeline and an outlet pipeline, the inlet pipeline is respectively provided with a liquid inlet and a gas inlet, and the liquid inlet is communicated with the gas inlet; this internal helical blade and the multichannel tubule of being equipped with of reactor peel off the component, helical blade be fixed in the axial the entry end of reactor body, the multichannel tubule is peeled off the component and is fixed in this internal outlet pipe side of being close to of reactor and hugging closely the inner wall of reactor body, the multichannel tubule peel off the size of component with the size phase-match of reactor body. The device can enable the matching of the fluid resistance loss and the shearing rate in each channel to reach the optimal value, can obviously improve the stripping effect, avoids fragmentation of the material and obtains the high-quality two-dimensional layered material.

Description

Gas-driven multi-channel laminar material stripping device
Technical Field
The invention relates to a gas-driven multi-channel layered material stripping device, and belongs to the technical field of two-dimensional nano material preparation.
Background
Since the first discovery of graphene by Geim et al in 2004, research on two-dimensional materials has attracted extensive attention worldwide. Liquid phase stripping is a general technology which is expected to realize large-scale and low-cost preparation of high-quality two-dimensional layered materials. In the liquid phase peeling process, normal force and lateral shearing force are the main forces for peeling, wherein the shearing force is the ideal force for peeling the layered material against van der waals force. Research shows that the stripping of two-dimensional materials such as graphene and the like is up to 104s-1Critical shear rate of (d). To achieve this critical shear rate, harsh operating conditions, such as high pressure shear or high speed stirring, are typically required, which often requires complex, expensive equipment, low stripping efficiency, and is not conducive to scale-up; the additional harsh operating conditions also cause fragmentation of the layered material, reducing the quality of the product.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a gas-driven multi-channel laminar material stripping device. The stripping device can realize the high-speed movement of the pneumatic driving liquid in the multi-channel tubule, and can achieve the minimum shearing rate required by the stripping of the layered material under the mild operation condition, thereby realizing the preparation of the high-quality and high-concentration two-dimensional layered material.
The invention provides a gas-driven layered material multi-channel stripping device, which comprises a circular reactor body with a hollow interior, wherein the reactor body is provided with an inlet pipeline and an outlet pipeline, the inlet pipeline is respectively provided with a liquid inlet and a gas inlet, and the liquid inlet is communicated with the gas inlet; this internal helical blade and the multichannel tubule of being equipped with of reactor peel off the component, helical blade be fixed in the axial the entry end of reactor body, the multichannel tubule is peeled off the component and is fixed in this internal outlet pipe side of being close to of reactor and hugging closely the inner wall of reactor body, the multichannel tubule peel off the size of component with the size phase-match of reactor body.
Further, multichannel tubule stripping element constitute by circular orifice plate and tubule, the tubule welding the circular orifice plate trompil department, the tubule with the axial direction of reactor body is parallel and with circular orifice plate perpendicular, the internal diameter of tubule with the trompil aperture phase-match of circular orifice plate, the diameter of circular orifice plate with the diameter phase-match of reactor body.
Furthermore, the diameter of the reactor body is 10-2000mm, and the length is 20-20000 mm.
Furthermore, the diameter of the spiral blade is 5-1500mm, and the length is 10-10000 mm.
Furthermore, the diameter of the circular hole plate is 10-2000mm, the hole diameter of the holes on the plate is 0.1-100mm, the hole spacing is 1-20mm, the number of the holes is 1-2000, and the holes are arranged in a regular triangle, a square straight line or a square staggered mode.
Furthermore, the length of the single tubule is 10-10000 mm.
Further, preferably, the diameter of the reactor body is 10-500mm, and the length is 1000-10000 mm.
Further, preferably, the diameter of the helical blade is 5-500mm, and the length is 500-5000 mm.
Further, preferably, the diameter of the circular hole plate is 10-500mm, and the number of the holes is 2-500.
Still further, preferably, the total length of the single tubule is 500-.
Further, the circular orifice plate is fixed in the reactor body through a flange.
Still further, the stripping device provided by the invention is applied to stripping of the layered material.
Further, the application is as follows:
the application is carried out in the following devices: the device comprises a liquid raw material storage tank, a feeding pump, a compressed gas source, a stripping device, a gas-liquid separator and a product storage tank; the inlet of the feed pump is connected with the liquid raw material storage tank, and the outlet of the feed pump is sequentially connected with the liquid flow control valve, the liquid flowmeter and the liquid inlet of the stripping device; the compressed gas source is sequentially connected with the gas flow control valve, the gas flowmeter, the gas pressure gauge and the gas outlet of the stripping device; a discharge pipeline of the stripping device is connected with an inlet of the gas-liquid separator; the gas-liquid separator is provided with a gas outlet and a liquid outlet, and the liquid outlet of the gas-liquid separator is sequentially connected with the product storage tank, the valve, the infusion pump and the liquid raw material storage tank to form reflux;
the application is as follows: dispersing the layered material in a solvent, fully stirring to obtain a dispersion liquid of the layered material, and placing the dispersion liquid in a liquid raw material storage tank; opening a feeding pump and a compressed gas source, then opening a liquid flow valve control valve, closing the valve, opening a gas flow control valve, simultaneously introducing the layered material dispersion liquid and the compressed gas into a stripping device, and carrying out a stripping reaction in the stripping device; the gas-liquid mixture flowing out of the outlet pipeline of the stripping device enters an inlet of a gas-liquid separator, the gas in the gas-liquid mixture is emptied from a gas outlet of the gas-liquid separator, the liquid in the gas-liquid mixture flows into a product storage tank from a liquid outlet of the gas-liquid separator to obtain the layered material dispersion liquid stripped for the first time, a liquid flow valve control valve is closed, the valve is opened, an infusion pump is started, the layered material dispersion liquid stripped for the first time is continuously introduced into an inlet of a feeding pump and flows back to the stripping device to form a circulation system, the dispersion liquid stripped for the circulation is obtained after the circulation is carried out for multiple times, and the dispersion liquid stripped for the circulation is stored in the product storage tank for later use; collecting the circularly stripped dispersion liquid, centrifuging, taking supernatant, and freeze-drying to obtain the layered material powder.
Compared with the prior art, the invention has the beneficial effects that: the diameter and the length of the helical blade in the device are designed, so that gas and liquid are uniformly mixed; more importantly, by designing the length, the number of channels (opening number) and the channel spacing (hole spacing) of the multi-channel stripping pipe, the matching of the fluid resistance loss and the shearing rate in each channel can reach the optimal value under mild operation conditions, the stripping effect can be obviously improved, the fragmentation of the material is avoided, and the high-quality two-dimensional layered material is obtained. The device can be widely applied to stripping of layered materials such as graphene, boron nitride, molybdenum disulfide and the like.
Drawings
FIG. 1 is a schematic view of a gas-driven multi-channel layered material exfoliation apparatus.
Fig. 2 is a cross-sectional view at section 1 of fig. 1.
FIG. 3 is a schematic flow chart of the device applied to the preparation of the layered material.
FIG. 1 depicts in notation: a-a liquid inlet; b-a gas inlet; c-a helical blade; d-a circular orifice plate; e-a thin tube; f-an outlet conduit; g-flange; h-reactor bulk.
FIG. 3 depicts in notation: 1-liquid raw material storage tank; 2-a feed pump; 3-a liquid flow control valve; 4-a liquid flow meter; 5-a source of compressed gas; 6-gas flow control valve; 7-a gas flow meter; 8-gas pressure gauge; 9-a stripping device; 10-a gas-liquid separator; 11-product storage tank; 12-a valve; 13-infusion pump.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be described in detail with reference to the accompanying drawings. As shown in fig. 1, the stripping device of the present invention comprises a circular reactor body (h) with a hollow interior, wherein the reactor body (h) is provided with an inlet pipeline and an outlet pipeline (f), the inlet pipeline is provided with a liquid inlet (a) and a gas inlet (b), and the liquid inlet (a) is communicated with the gas inlet (b); this internal helical blade (c) and multichannel tubule of being equipped with of reactor strip the component, helical blade (c) be fixed in the axial the entry end of reactor body (h), multichannel tubule strip the component and is fixed in reactor body (h) in be close to outlet duct (f) side and hug closely the inner wall of reactor body (h), the multichannel tubule strip the size of component with the size phase-match of reactor body (h). Multichannel tubule peel off component constitute by circular orifice plate (d) and tubule (e), tubule (e) welding the circular orifice plate (d) trompil department and with circular orifice plate (d) perpendicular, the internal diameter of tubule (e) with the trompil aperture phase-match of circular orifice plate (d), the diameter of circular orifice plate (d) with the diameter phase-match of reactor body (h). The circular orifice plate (d) is fixed in the reactor body (h) through a flange (g).
The invention adopts a self-made device to prepare the stripping material: the device comprises a liquid raw material storage tank (1), a feeding pump (2), a compressed gas source (5), a stripping device (9), a gas-liquid separator (10) and a product storage tank (11); the inlet of the feed pump (2) is connected with the liquid raw material storage tank (1), and the outlet of the feed pump (2) is sequentially connected with the liquid flow control valve (4), the liquid flowmeter (4) and the liquid inlet of the stripping device (9); the compressed gas source (5) is sequentially connected with a gas flow control valve (6), a gas flowmeter (7), a gas pressure gauge (8) and a gas outlet of the stripping device (9); a discharge pipeline of the stripping device (9) is connected with an inlet of the gas-liquid separator (11); the gas-liquid separator (11) is provided with a gas outlet and a liquid outlet, and the liquid outlet of the gas-liquid separator (11) is sequentially connected with the product storage tank (11), the valve (12), the infusion pump (13) and the liquid raw material storage tank (1) to form reflux;
referring to the attached drawings, when the invention works, the layered material is dispersed in the solvent and fully stirred to obtain the dispersion liquid of the layered material, and the dispersion liquid is placed in the liquid raw material storage tank (1); opening a feed pump (2) and a compressed gas source (5), then opening a liquid flow valve control valve (3), closing a valve (12), opening a gas flow control valve (6), simultaneously introducing the layered material dispersion liquid and the compressed gas into a stripping device (9), and carrying out a stripping reaction in the stripping device (9); the gas-liquid mixture flowing out of the outlet pipeline of the stripping device (9) enters the inlet of a gas-liquid separator (10), the gas in the gas-liquid mixture is emptied from the gas outlet of the gas-liquid separator (10), the liquid in the gas-liquid mixture flows into a product storage tank (11) from the liquid outlet of the gas-liquid separator (10), after the layered material dispersion liquid stripped once is obtained, a liquid flow valve control valve (3) is closed, a valve (12) is opened, an infusion pump (13) is started, the layered material dispersion liquid stripped once is continuously introduced into the inlet of a feed pump (2) and flows back to the stripping device (9) to form a circulation system, after circulation is carried out for multiple times, the dispersion liquid stripped circularly is obtained, and the dispersion liquid stripped circularly is stored in the product storage tank for later use; collecting the circularly stripped dispersion liquid, centrifuging, taking supernatant, and freeze-drying to obtain the layered material powder.
The following examples and experimental examples are given to further illustrate the apparatus and method according to the present invention.
Example 1
Graphite is dispersed in N-methylpyrrolidone to prepare graphite suspension with the concentration of 60mg/ml, the graphite suspension and air from an air compressor with the flow rate of 20L/h and the flow rate of 600L/h are respectively fed into a reactor body with the diameter of 30mm and the length of 2.1m from corresponding inlets by a plunger pump, the graphite suspension and the air are fully mixed by a helical blade with the diameter of 25mm and the length of 1m, the mixture enters a pore plate with the diameter of 30mm, the pore plate with the pore diameter of 2mm and the pore number of 4, a single tubule with the length of 1m is separated in a tubule stripping element, a gas-liquid mixture discharged from the tubule stripping element is separated by a gas-liquid separator, liquid in the mixture is conveyed to a product storage tank, and the graphene with the average layer number of 2 layers can be obtained after 2 times.
Example 2
The method comprises the steps of dispersing hexagonal boron nitride in 50% volume fraction ethanol aqueous solution to prepare boron nitride suspension with the concentration of 50mg/ml, enabling the boron nitride suspension to enter a reactor body with the diameter of 50mm and the length of 1.6m from a corresponding inlet through a plunger pump at the flow rate of 10L/h and air from an air compressor and the flow rate of 1500L/h respectively, enabling the boron nitride suspension to be fully mixed through a helical blade with the diameter of 40mm and the length of 1m, enabling the boron nitride suspension to enter a pore plate with the diameter of 50mm, enabling the pore plate to have the pore diameter of 2mm, enabling the pore plate to have the pore number of 16, enabling a single thin tube to have the length of 0.5m, enabling a gas-liquid mixture coming out of the thin tube stripping element to be separated through a gas-liquid separator, conveying liquid in the gas-liquid separator to a product storage tank.
Example 3
Dispersing blocky molybdenum disulfide in N-methyl pyrrolidone to prepare molybdenum disulfide suspension with the concentration of 20mg/ml, respectively feeding the molybdenum disulfide suspension and air with the flow of 5000L/h from corresponding inlets into a reactor body with the diameter of 100mm and the length of 4.2m by using a plunger pump at the flow of 50L/h, fully mixing the molybdenum disulfide suspension and the air with the flow of 5000L/h by using a helical blade with the diameter of 80mm and the length of 2m, feeding the mixture into a pore plate with the diameter of 100mm, wherein the pore plate has the pore diameter of 5mm, the pore plate has the pore number of 30, and a single tubule has the length of 2m, separating a gas-liquid mixture discharged from a tubule stripping element by using a gas-liquid separator, conveying the liquid into a product storage tank, circulating for 3 times in this way, and obtaining the molybdenum disulfide with the average layer number.

Claims (10)

1. A gas-driven multi-channel stripping device for a layered material is characterized in that: the device comprises a circular reactor body (h) with a hollow interior, wherein an inlet pipeline and an outlet pipeline (f) are arranged on the reactor body (h), a liquid inlet (a) and a gas inlet (b) are respectively arranged on the inlet pipeline, and the liquid inlet (a) is communicated with the gas inlet (b); this internal helical blade (c) and multichannel tubule of being equipped with of reactor strip the component, helical blade (c) be fixed in the axial the entry end of reactor body (h), multichannel tubule strip the component and is fixed in reactor body (h) in be close to outlet duct (f) side and hug closely the inner wall of reactor body (h), the multichannel tubule strip the size of component with the size phase-match of reactor body (h).
2. The apparatus of claim 1, wherein: multichannel tubule peel off component constitute by circular orifice plate (d) and tubule (e), tubule (e) welding the circular orifice plate (d) trompil department, tubule (e) with the axial direction parallel of reactor body (h) and with circular orifice plate (d) perpendicular, the internal diameter of tubule (e) with the trompil aperture phase-match of circular orifice plate (d), the diameter of circular orifice plate (d) with the diameter phase-match of reactor body (h).
3. The apparatus of claim 1, wherein: the reactor body (h) has a diameter of 10-2000mm and a length of 20-20000 mm.
4. The apparatus of claim 3, wherein: the diameter of the helical blade (c) is 5-1500mm, and the length is 10-10000 mm.
5. The apparatus of claim 3, wherein: the diameter of the circular pore plate (d) is 10-2000mm, the aperture of the holes on the plate is 0.1-100mm, the hole spacing is 1-20mm, the number of the holes is 1-2000, and the holes are staggered according to regular triangle, square straight line or square.
6. The apparatus of claim 5, wherein: the length of the single tubule is 10-10000 mm.
7. The apparatus of claim 1, wherein: the reactor body has a diameter of 10-500mm and a length of 1000-10000 mm; the diameter of the helical blade is 5-500mm, and the length is 500-5000 mm; the diameter of the circular hole plate is 10-500mm, and the number of the holes is 2-500; the total length of the single tubule is 500-5000 mm.
8. The apparatus of claim 1, wherein: the circular orifice plate (d) is fixed in the reactor body (h) through a flange (g).
9. Use of a device according to claim 1 for peeling off a layered material.
10. The use of claim 9, wherein: the application is carried out in the following devices: the device comprises a liquid raw material storage tank (1), a feeding pump (2), a compressed gas source (5), a stripping device (9), a gas-liquid separator (10) and a product storage tank (11); the inlet of the feed pump (2) is connected with the liquid raw material storage tank (1), and the outlet of the feed pump (2) is sequentially connected with the liquid flow control valve (4), the liquid flowmeter (4) and the liquid inlet of the stripping device (9); the compressed gas source (5) is sequentially connected with a gas flow control valve (6), a gas flowmeter (7), a gas pressure gauge (8) and a gas outlet of the stripping device (9); a discharge pipeline of the stripping device (9) is connected with an inlet of the gas-liquid separator (11); the gas-liquid separator (11) is provided with a gas outlet and a liquid outlet, and the liquid outlet of the gas-liquid separator (11) is sequentially connected with the product storage tank (11), the valve (12), the infusion pump (13) and the liquid raw material storage tank (1) to form reflux;
the application is as follows: dispersing the layered material in a solvent, fully stirring to obtain a dispersion liquid of the layered material, and placing the dispersion liquid in a liquid raw material storage tank (1); opening a feed pump (2) and a compressed gas source (5), then opening a liquid flow valve control valve (3), closing a valve (12), opening a gas flow control valve (6), simultaneously introducing the layered material dispersion liquid and the compressed gas into a stripping device (9), and carrying out a stripping reaction in the stripping device (9); the gas-liquid mixture flowing out of the outlet pipeline of the stripping device (9) enters the inlet of a gas-liquid separator (10), the gas in the gas-liquid mixture is emptied from the gas outlet of the gas-liquid separator (10), the liquid in the gas-liquid mixture flows into a product storage tank (11) from the liquid outlet of the gas-liquid separator (10), after the layered material dispersion liquid stripped once is obtained, a liquid flow valve control valve (3) is closed, a valve (12) is opened, an infusion pump (13) is started, the layered material dispersion liquid stripped once is continuously introduced into the inlet of a feed pump (2) and flows back to the stripping device (9) to form a circulation system, after circulation is carried out for multiple times, the dispersion liquid stripped circularly is obtained, and the dispersion liquid stripped circularly is stored in the product storage tank for later use; collecting the circularly stripped dispersion liquid, centrifuging, taking supernatant, and freeze-drying to obtain the layered material powder.
CN201910549394.9A 2019-06-24 2019-06-24 Gas-driven multi-channel laminar material stripping device Pending CN112125299A (en)

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