CN112279289A - Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs - Google Patents
Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs Download PDFInfo
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- CN112279289A CN112279289A CN202010672821.5A CN202010672821A CN112279289A CN 112279289 A CN112279289 A CN 112279289A CN 202010672821 A CN202010672821 A CN 202010672821A CN 112279289 A CN112279289 A CN 112279289A
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- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 49
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title abstract description 6
- 238000010924 continuous production Methods 0.000 title abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 34
- 238000000197 pyrolysis Methods 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims abstract description 14
- 238000007789 sealing Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000005485 electric heating Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 6
- 238000011437 continuous method Methods 0.000 claims description 3
- 239000002910 solid waste Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000010808 liquid waste Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001754 furnace pyrolysis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- General Physics & Mathematics (AREA)
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Abstract
The invention belongs to the field of nano material production, and relates to a semi-continuous production method and a semi-continuous production device for preparing nano materials by pyrolyzing Metal Organic Frameworks (MOFs). The device comprises a conveying pipe, a heating furnace and a lead screw; the conveying pipe passes through the heating furnace, and the front end of the conveying pipe is provided with a feeding hole (a powder bin comprising an air inlet pipe and a cover is arranged on the conveying pipe); the lower part of the rear end is connected with a discharge hole (containing a discharge valve) and then connected with a slag hole (connected with a collecting tank and a vent hole in series); the end of the pipe is provided with a sealing cover; the upper end of the discharge valve and the slag outlet are provided with electric heating heat preservation belts; the tube is internally provided with a rotary screw driven by a motor. The production method provided by the invention comprises the following steps: and (3) placing the MOFs powder into a bin, closing an air inlet cover, ventilating, conveying the powder into a furnace by a lead screw for pyrolysis, recovering residues by a collecting tank, discharging the obtained material from a discharge port, repeating the steps, and performing semi-continuous production on the nano material. The invention provides a preparation method of intermittent feeding and semi-automatic conveying and discharging materials, which can solve the problems of low yield and long non-production time of the traditional method, and the device is simple and easy to operate.
Description
Technical Field
The invention discloses a semi-continuous method for preparing MOFs-derived nano materials by pyrolyzing MOFs and a system device thereof, belonging to the technical field of nano materials.
Background
Metal-Organic Frameworks (MOFs) are zeolite-like materials with periodic network structures formed by self-assembly of oxygen-and nitrogen-containing polydentate Organic ligands connected with Metal atoms or Metal atom clusters by coordination bonds, and are widely used in gas adsorption, separation, heterogeneous catalytic reaction and photoelectromagnetic properties, drug storage and sustained release, sensors, and other fields. Compared with conventional porous materials, MOFs have the following characteristics: firstly, the materials are various in types and strong in functionality, and the currently synthesized MOFs are more than five thousand. Second, high specific surface area and porosity. MOFs materials belong to porous materials and are currently discovered to have ultra-high specific surface area (S)LangmuirCan exceed 10400 m at most2g-1) While also possessing crystalline materials with ultra-high porosity (up to 90% free volume). Third, the hole size is adjustable. The MOFs material with the pore diameter from a few angstroms to dozens of nanometers can be synthesized by modulating the types of the organic ligand and the metal ion. Fourth, relatively poor thermal and chemical stability. The poor thermal stability and chemical stability of the MOFs mean that the MOFs structure collapses under the action of external environments such as high temperature, high humidity, various organic solvents and the like, and the fundamental reason is that coordination bonds between metal ions and organic ligands are broken under the action of external factors. This is a drawback inherent in the MOFs formation method and a drawback that researchers cannot ignore. However, there is a certain disadvantage, and due to the disadvantage of unstable MOFs, people have conducted high temperature pyrolysis on various MOFs materials to prepare functional nanomaterials, and there are many related reports on the literature and patents at present. For example, chinese patent CN 201911345852.3 reports the preparation of Co-TPM and its pyrolysis under inert atmosphere to obtain a Co-doped Co-carbon-based electrocatalyst material; chinese patent CN 201910700518.9 reports that roasting M-BDC (M = Cu, Zn, Y, La, Ce, Ti, Zr, V, Cr, Mn, Fe, Co, Ni, etc.) in air can obtain a two-dimensional oxide catalytic material, which has a good effect on volatile organic compound removal; chinese patent 201810896057.2 reports the preparation of nano short rod-like MOFs and the high-temperature pyrolysis of the nano short rod-like MOFs to obtain the sea urchin-like metal oxide porous photocatalytic material.
However, the pyrolysis of MOFs has the problem that most of the organisms are decomposed and lost, the amount of the obtained solid material is generally less than 30% of the mass of the initial MOFs, and in order to obtain a sufficient amount of samples, people often need to use a tube furnace to perform an intermittent production operation mode, including loading, pyrolyzing and unloading MOFs powder, cleaning a reaction pipeline polluted by organic wastes, and then loading the MOFs powder, which is repeated, so that the unproductive time is long.
Disclosure of Invention
The present invention has been made to overcome the above problems and it is an object of the present invention to provide a semi-continuous method for preparing nanomaterials by pyrolyzing MOFs and a system apparatus therefor.
In order to realize the purpose, the invention adopts the following technical scheme that:
a system device for preparing nano materials by pyrolyzing MOFs comprises a conveying pipe, a heating furnace and a lead screw; the conveying pipe penetrates through the heating furnace, the front end part of the conveying pipe is provided with an MOFs powder feeding port, an MOFs powder bin is arranged on the feeding port, the rear end part of the conveying pipe sequentially receives a rice material discharging port and then is connected with a slag outlet, the slag outlet is connected with a collecting tank, and a vent is arranged on the collecting tank; the tail end of the conveying pipe is sealed by a sealing cover; the lead screw is arranged in the conveying pipe, the outer surface of the lead screw is provided with a spiral groove, and the lead screw is driven by an external motor to rotate.
Furthermore, an inner hole is formed in the center, perpendicular to the inner wall of the conveying pipe, of the sealing cover at the tail end of the conveying pipe, and the screw rod is connected with the inner hole through a rotating bearing.
Further, the device also comprises an air inlet pipe arranged on the conveying pipe, and the inlet pipe conveys inert gas or air.
Furthermore, the air inlet pipe penetrates through the air inlet cover to enter the powder bin and approach the feed inlet, and the powder bin is communicated with the conveying pipe through the feed inlet.
Compared with the prior art of pyrolyzing MOFs by using a tube furnace, the invention has the following advantages: according to the invention, after a proper amount of MOFs powder is loaded into the powder bin, the screw rod is used for conveying and discharging, so that the semi-continuous preparation of the MOFs-derived nano material is realized, the production strength is improved, and the problems of low yield and long non-production time in the existing tubular furnace pyrolysis MOFs process are solved.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a left side view of the seal cover at the end of the air delivery pipe.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
With reference to fig. 1, the MOFs semi-automatic pyrolysis device comprises a motor (1), a coupler (2), a screw rod front end shaft (3), a powder bin (4), an air inlet pipe (5), an air inlet cover (6), a feed inlet (7), a conveying pipe (8), a tube furnace (9), a screw rod (10), a discharge valve (11), a discharge outlet (12), a slag outlet (13), a collection tank (14), a vent (15), a sealing cover (16) and an electric heating heat preservation belt (17). The conveying pipe (8) is horizontally and fixedly arranged in the tubular furnace (9), the middle section of the conveying pipe (8) can be heated and heated in a heating area of the tubular furnace (9), and two ends of the conveying pipe (8) extend out of a furnace body of the tubular furnace. A feed inlet (7) is arranged on the upper side of the front end of the conveying pipe (8), and the powder bin (4) is vertically connected with the feed inlet (6). Sample bleeder valve (11) is connected at first to the rear end downside of conveyer pipe (8), and discharge gate (12) are connected to the bleeder valve, then conveyer pipe rear end downside links to each other with slag notch (13) again, and slag notch (13) are connected with collection tank (14) perpendicularly, and in addition, the rear end of conveyer pipe (8) is to sealed lid (16), bleeder valve (11) upper end pipeline and slag notch (3) use electric heat preservation area (17) to keep warm. The air inlet pipe (5) penetrates through the air inlet cover (6) to enter the powder bin (4) and approach the feed inlet, so that atmosphere is provided for MOFs pyrolysis, and the powder bin can be swept to remove residual MOFs powder. Gas generated by the MOFs pyrolysis can be discharged through a slag outlet (13), a collecting tank (14) and a vent (15), and organic liquid-solid waste generated by the pyrolysis can be recovered in the collecting tank (14). The screw rod (10) horizontally penetrates through the conveying pipe (8), and the motor (1) is connected with a front end shaft (3) of the screw rod through the coupler (2). After the motor 1 is started, a lead screw (10) can be driven to carry out spiral transmission in the stainless steel pipe. The conveying pipe (8) is a stainless steel pipe.
Referring to fig. 2, the sealing cover (16) is provided with an inner hole (18) perpendicular to the left wall surface center of the conveying pipe (8), and the screw rod (10) is connected with the inner hole (18) through a rotating bearing to realize rotation.
The system has the innovation point of the connection relation of all the parts, and the detailed structure and control of the parts, such as the motor, the shaft coupling, the powder bin, the air inlet cover, the air inlet pipe, the conveying pipe, the screw rod, the tube furnace, the discharge valve, the collecting tank, the sealing cover, the electric heating belt and the like, in the system can be realized by adopting the conventional technology in the field, and the details are not repeated herein.
The specific operation is as follows:
when the motor (1) is not started, the air inlet cover (6) is opened, a proper amount of MOFs powder is added into the powder bin (4), part of the MOFs powder is deposited on a lead screw (10) in a stainless steel pipe (8), the air inlet cover (6) is closed, and air is introduced from the air inlet pipe (5). Starting the motor (1), starting the screw rod (10) to perform spiral transmission, conveying a proper amount of MOFs powder to a constant-temperature heating zone in the tube furnace (9), closing the motor (1), and performing pyrolysis after setting pyrolysis temperature and time. As the clearance between the screw rod (10) and the inner wall of the stainless steel pipe (8) is very small, the MOFs powder cannot be leaked and accumulated in the stainless steel pipe (8). The gas inlet pipe (5) can sweep the MOFs powder entering the stainless steel pipe (8) in the coal powder bin (4) while providing atmosphere for the pyrolysis of the MOFs, and the phenomenon that the MOFs powder is accumulated and cannot fall is avoided. When the MOFs powder is pyrolyzed, the generated organic liquid-solid waste materials are collected in a collecting tank (14), and the generated tail gas is discharged through a slag outlet (13), the collecting tank (14) and a vent (15). After the pyrolysis is finished, the discharge valve (11) is opened, and the obtained nano material is discharged from the discharge hole (12) under the screw transmission action of the screw rod (10).
Claims (5)
1. A semi-continuous system apparatus for pyrolyzing Metal Organic Frameworks (MOFs) to produce nanomaterials, comprising: the device comprises a motor (1), a coupler (2), a front end shaft (3), a powder bin (4), an air inlet pipe (5), an air inlet cover (6), a feed inlet (7), a conveying pipe (8), a tube furnace (9), a screw rod (10), a discharge valve (11), a discharge outlet (12), a slag outlet (13), a collecting tank (14), a vent (15), a sealing cover (16) and an electric heating heat preservation belt (17); the conveying pipe (8) penetrates through the tube furnace (9), a feeding hole (7) is formed in the upper side of the front end of the conveying pipe (8), a powder bin (4) is arranged on the feeding hole (7), and an air inlet cover (6) is arranged at the top of the powder bin (4); the lower side of the rear end of the conveying pipe (8) is firstly connected with a discharge valve (11), and the discharge valve is connected with a discharge hole (12); the lower side of the rear end of the conveying pipe (8) is connected with a slag hole (13), the slag hole (13) is vertically connected with a collecting tank (14), and a drain opening (15) is arranged on the collecting tank (14); the tail end of the conveying pipe (8) is provided with a sealing cover; an electric heating heat preservation belt (17) is arranged from the rear end of the conveying pipe (8) to the sealing cover, the upper end of the discharge valve (11) and the outer side of the slag outlet (3); the screw rod (10) is arranged in the conveying pipe (8) and is driven by an external motor to rotate.
2. The device according to claim 1, characterized in that the sealing cover (16) is provided with an inner hole perpendicular to the center of the left side wall surface of the conveying pipe (8), and the screw rod (10) is connected with the inner hole through a rotating bearing.
3. The device according to claim 1, characterized in that it further comprises an intake pipe (5) arranged on the delivery pipe (8), the intake pipe (5) delivering inert gas or air.
4. The device according to claim 3, characterized in that the air inlet pipe (5) passes through the air inlet cover (6) to enter the powder bin (4) and is close to the feed inlet (4), and the powder bin (4) is communicated with the conveying pipe (8) through the feed inlet (7).
5. A semi-continuous method for preparing nano-materials by pyrolyzing MOFs, which comprises the following steps: filling a proper amount of MOFs powder into a powder bin (4), closing an air inlet cover (6), closing a discharge valve (11), introducing gas, starting a motor (1), conveying the MOFs powder to a tube furnace (9) heating area by using a lead screw, closing the motor (1), heating up and pyrolyzing, wherein during pyrolysis, liquid and solid waste is deposited and recovered in a collecting tank, tail gas is discharged from an emptying port (15), after pyrolysis is finished, the tube furnace is cooled to room temperature, opening the discharge valve (11), starting the motor (1), and discharging the obtained nano material at a discharge port by using the lead screw.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010672821.5A CN112279289A (en) | 2020-07-14 | 2020-07-14 | Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs |
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| CN202010672821.5A CN112279289A (en) | 2020-07-14 | 2020-07-14 | Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs |
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| CN112279289A true CN112279289A (en) | 2021-01-29 |
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| CN202010672821.5A Pending CN112279289A (en) | 2020-07-14 | 2020-07-14 | Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008015927A1 (en) * | 2008-03-27 | 2009-10-01 | Brück, Alexandra | Conversion process for organic material to produce combustible gases involves using feed unit to transport organic material to tubular furnace shaft |
| CN107311146A (en) * | 2016-04-25 | 2017-11-03 | 山西中兴环能科技有限公司 | A kind of serialization prepares the device and method of nano-carbon material |
| CN207030958U (en) * | 2017-06-27 | 2018-02-23 | 山西中兴环能科技有限公司 | A kind of serialization prepares the device of nano-carbon material |
| CN207081007U (en) * | 2017-07-01 | 2018-03-09 | 南京理工大学 | A kind of powder continuous heat system |
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2020
- 2020-07-14 CN CN202010672821.5A patent/CN112279289A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008015927A1 (en) * | 2008-03-27 | 2009-10-01 | Brück, Alexandra | Conversion process for organic material to produce combustible gases involves using feed unit to transport organic material to tubular furnace shaft |
| CN107311146A (en) * | 2016-04-25 | 2017-11-03 | 山西中兴环能科技有限公司 | A kind of serialization prepares the device and method of nano-carbon material |
| CN207030958U (en) * | 2017-06-27 | 2018-02-23 | 山西中兴环能科技有限公司 | A kind of serialization prepares the device of nano-carbon material |
| CN207081007U (en) * | 2017-07-01 | 2018-03-09 | 南京理工大学 | A kind of powder continuous heat system |
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Application publication date: 20210129 |
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