CN110339791A - A kind of multi-functional synthesis device suitable for metal-organic framework material - Google Patents

A kind of multi-functional synthesis device suitable for metal-organic framework material Download PDF

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Publication number
CN110339791A
CN110339791A CN201910574308.XA CN201910574308A CN110339791A CN 110339791 A CN110339791 A CN 110339791A CN 201910574308 A CN201910574308 A CN 201910574308A CN 110339791 A CN110339791 A CN 110339791A
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metal
organic framework
fluid path
framework material
gas
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CN110339791B (en
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冯光
王佳胜
陈明玉
牛良
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Huazhong University of Science and Technology
Shenzhen Huazhong University of Science and Technology Research Institute
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Huazhong University of Science and Technology
Shenzhen Huazhong University of Science and Technology Research Institute
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/085Funnel filters; Holders therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J14/00Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/223Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
    • B01J20/226Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • C08G83/008Supramolecular polymers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to materials synthesis equipment correlative technology fields, it discloses a kind of multi-functional synthesis devices suitable for metal-organic framework material, equipment includes gas displacement mechanism, filters mechanism, Ultrasonic Heating mechanism, the first fluid path and the second fluid path, gas displacement mechanism is removably attachable to filter mechanism, filters mechanism and portion gas displacement mechanism is contained in Ultrasonic Heating mechanism;First fluid path and the second fluid path are separately positioned on gas displacement mechanism and filter in mechanism;Gas displacement mechanism sends the synthetic product after reactant reaction to suction filtration mechanism for accommodating reactant and providing corresponding atmosphere for the reaction of reactant;Mechanism is filtered to be used for the metal-organic framework material and soluble impurity of synthetic product and the separation and drying of solvent;Second fluid path filters waste liquid within the organization for being discharged;Ultrasonic Heating mechanism is used to heat so that metal-organic framework material is dried suction filtration mechanism.The present invention improves synthetic ratio, and applicability is stronger.

Description

A kind of multi-functional synthesis device suitable for metal-organic framework material
Technical field
The invention belongs to materials synthesis equipment correlative technology fields, and being suitable for metal more particularly, to one kind has machine frame The multi-functional synthesis device of frame material.
Background technique
Metal-organic framework material (referred to as " MOFs ") is class I organic-inorganic hybridized material, by organic ligand and metal Salt is self-assembly of, and the type of metal-organic framework material is extremely more, and diversified structure and outstanding porosity characteristic make metal Organic framework materials be widely used in the absorption of gas with separate, be catalyzed, the fields such as energy storage.
Currently, there are many kinds of the synthetic methods of metal-organic framework material, for example, it is ultrasonic method, solvent-thermal method, paddling process, micro- Wave heating method etc., and wherein solvent-thermal method is most conventional synthetic method, solvent-thermal method needs use ultrasonic machine, centrifuge, Numerous instruments such as baking oven, vacuum drying oven, as the product in container shifts in different instruments, finally obtained metal has machine frame Frame material will necessarily lose;Meanwhile synthesis process needs to operate a variety of different instruments, this also brings not to experimenter Just.
The atmosphere for synthesizing different organic framework materials requirements is different, and the synthesis of part metals organic framework materials can It completes in air, and part metals organic framework materials synthesis process needs the participation of special gas, such as oxygen or two Carbonoxide;There are also part metals organic framework materials, atmospheric environment interferes synthesis process, needs to close in inert gas At.In addition, needing to remove the impurity in metal-organic framework material, this process is known as after metal-organic framework material synthesis The activation (or being known as purifying) of metal-organic framework material, the specific implementation method of activation process is successively to use deionization Water, organic solvent (ethyl alcohol, acetone etc.) repeated ultrasonic clean solid product, isolate solid product, finally dry isolated Solid product, wherein the process of solid product separation is more difficult, the method for usually used centrifugation in laboratory, but this method Time-consuming, and loss is more, and yield is lower, is not suitable for industrialized production;Another method is to remove soluble impurity by filtration method And solvent, but the rate of filtration is extremely slow under normal pressure.Correspondingly, there is develop a kind of synthetic ratio to be preferably suitable for gold for this field Belong to the technical need of the multi-functional synthesis device of organic framework materials.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides one kind to be suitable for metal organic frame material The multi-functional synthesis device of material, the environment needed based on metal-organic framework material synthesis and synthesis feature, are had for metal The different of machine frame materials synthesis require to improve device, allow the synthesis device individually to complete metal organic The synthesis overall process of frame material, while the loss during sample cleanup is avoided, so that the conjunction of metal-organic framework material At more efficient and convenient, synthetic ratio is higher, and applicability is stronger.
To achieve the above object, the present invention provides a kind of multi-functional synthesis suitable for metal-organic framework material to set Standby, the equipment includes gas displacement mechanism, filters mechanism, Ultrasonic Heating mechanism, the first fluid path and the second fluid path, the gas Displacement mechanism is removably attachable to the suction filtration mechanism, and the gas displacement mechanism of the suction filtration mechanism and part is contained in institute State Ultrasonic Heating mechanism;First fluid path and second fluid path are separately positioned on the gas displacement mechanism and the suction filtration In mechanism;
Solvent is added into the gas displacement mechanism by first fluid path;The gas displacement mechanism is for accommodating Reactant and corresponding atmosphere is provided for the reaction of reactant, and sends the synthetic product after reactant reaction to the suction filtration Mechanism;The mechanism that filters is used for the metal-organic framework material and soluble impurity of the synthetic product and the separation of solvent And it is dry;Second fluid path is for being discharged the suction filtration waste liquid within the organization;The Ultrasonic Heating mechanism passes through ultrasonic vibration Reactant is mixed, is also used to heat the suction filtration mechanism to carry out the metal-organic framework material It is dry.
Further, after synthetic product is from the gas displacement mechanism into the suction filtration mechanism, pass through first liquid Adding liquid in gas displacement mechanism described in road direction, then the Ultrasonic Heating mechanism carries out ultrasound to the gas displacement mechanism Cleaning.
Further, the gas displacement mechanism includes the first gas circuit, the second gas circuit, upper cavity and the first funnel, described First gas circuit and second gas circuit are separately positioned on the upper cavity;The upper cavity is cylindrical, first funnel It is arranged in the upper cavity, is located at the open end of the upper cavity;First air circuit connection passes through described in gas cylinder One gas circuit is passed through predetermined gas into the upper cavity with reaction atmosphere needed for building reactant reaction;Second gas circuit connects It is connected to vacuum pump, the upper cavity is vacuumized by the vacuum pump and second gas circuit.
Further, the gas displacement mechanism further includes the 4th valve, and first funnel is arranged in the 4th valve On spout of funnel.
Further, the gas displacement mechanism further includes case lid, and the case lid is removably disposed in the upper cavity Far from described one end for filtering mechanism, first fluid path is arranged on the case lid.
Further, the suction filtration mechanism includes the second funnel, lower chamber and third gas circuit, and the second funnel setting exists In the lower chamber, the third gas circuit is arranged on the lower chamber, and it is located at second funnel and second liquid Between road;The third air circuit connection is in vacuum pump.
Further, the suction filtration mechanism further includes filter membrane, and the filter membrane is arranged on second funnel, is used to filter Except the solvent and soluble impurity in synthetic product.
Further, the filter membrane is using made of stainless steel.
Further, second fluid path includes stainless steel tube and the 7th valve, and one end of the stainless steel tube is protruded into described It filters in mechanism, the 7th valve is arranged on the stainless steel tube.
Further, first fluid path includes pipeline and the first valve, and first valve is arranged on the pipeline;It is described One end of pipeline is protruded into the gas displacement mechanism;The pipeline is using made of glass.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, it is provided by the invention suitable Multi-functional synthesis device for metal-organic framework material mainly has the advantages that
1. the gas displacement mechanism is used to accommodate reactant and provide corresponding atmosphere for the reaction of reactant, and will be anti- Synthetic product after answering object to react sends the suction filtration mechanism to;The suction filtration mechanism is for there is the metal of the synthetic product Metal organic frame can be implemented separately in the separation and drying of machine frame frame material and soluble impurity and solvent, the synthesis device The overall process of the synthesis of material, this makes the synthesis process of metal-organic framework material can be to avoid the use back and forth of more instruments With the transfer repeatedly of sample, reduce the workload of operator, improve MOFs yield so that large-scale production MOFs become can Energy.
2. the gas displacement mechanism is met for accommodating reactant and providing corresponding atmosphere for the reaction of reactant MOFs under particular atmosphere and various air pressures, which is synthesized, to be required.
3. the suction filtration mechanism further includes filter membrane, the filter membrane is arranged on second funnel, is used to filter out synthesis Solvent and soluble impurity in product.
4. the third air circuit connection vacuum pump, to be vacuumized to the lower chamber, so that MOFs sample and solvent And be dissolved in impurity therein can quick separating, reduce filtration time, so that the purification of sample and drying process are more quick.
Detailed description of the invention
Fig. 1 is the schematic diagram of the multi-functional synthesis device provided by the invention suitable for metal-organic framework material.
In all the appended drawings, identical appended drawing reference is used to denote the same element or structure, in which: the first valve of 1-, 2- Second valve, 3- third valve, the 4th valve of 4-, the 5th valve of 5-, the 6th valve of 6-, the 7th valve of 7-, 8- case lid, the first fluid path of 9-, 10- chamber Body, 101- upper cavity, 102- lower chamber, the junction 103-, 11- filter membrane, 12- Ultrasonic Heating mechanism, the first funnel of 13-, 14- Two funnels.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below Not constituting a conflict with each other can be combined with each other.
Referring to Fig. 1, the multi-functional synthesis device provided by the invention suitable for metal-organic framework material, the synthesis Equipment includes gas displacement mechanism, filters mechanism, Ultrasonic Heating mechanism 12, the first fluid path 9 and the second fluid path, the gas displacement Mechanism is removably attachable to the suction filtration mechanism, and the suction filtration mechanism is arranged in the Ultrasonic Heating mechanism 12;Described One fluid path 9 is connected to the gas displacement mechanism, adds solvent into the gas displacement mechanism by first fluid path 9. Second fluid path is connected to the suction filtration mechanism, is used to be discharged the waste liquid generated in the suction filtration mechanism.Wherein, the gas Body is replaced atmosphere within the organization and is changed with the metal-organic framework material currently synthesized, has to meet the metal currently synthesized The synthesis demand of machine frame frame material.The synthetic product progress metal for filtering mechanism and being used to synthesize the gas displacement mechanism The separation and drying of organic framework materials and soluble impurity and solvent.The Ultrasonic Heating mechanism 12 by ultrasonic vibration come pair The gas displacement mechanism is cleaned by ultrasonic, while it is also used to heat the suction filtration mechanism to complete to synthesis The drying of metal-organic framework material.
The gas displacement mechanism includes the first gas circuit, the second gas circuit, upper cavity 101, case lid 8, the first funnel 13 and the Four valves 4, the upper cavity 101 are cylindrical shape, and first gas circuit and second gas circuit are separately positioned on the upper cavity 101 Side, one end of first gas circuit is set in the upper cavity 101, and the other end is connected to gas cylinder.First gas circuit For being passed through gas needed for air, oxygen, carbon dioxide, inert gas etc. react into the upper cavity 101.Second gas The one end on road is set in the upper cavity 101, and the other end is connected to vacuum pump, can be to the gas by second gas circuit Body replaces mechanism and carries out vacuumize process.
In present embodiment, one end that first gas circuit is located in the upper cavity 101 be located at reactant level hereinafter, With gas in substitutional solution;One end that second gas circuit is located in the upper cavity 101 is located at reactant level or more, can lead to Cross vacuum pump or directly complete to be evacuated by atmosphere and gas replenishment process, with build vacuum environment in the upper cavity 101 or Person is directly as outlet side.
First gas circuit includes the first tracheae and the second valve 2, and second valve 2 is arranged on first tracheae, institute The one end for stating the first tracheae is contained in the upper cavity 101, and the other end is connected to the gas cylinder, to pass through the gas cylinder to institute It states in upper cavity 101 and is passed through specific gas, build specific reaction atmosphere.Second gas circuit includes the second tracheae and third valve 3, The third valve 3 is arranged on second tracheae.One end of second tracheae is contained in the upper cavity 101, another End is connected to vacuum pump, to be evacuated to the upper cavity 101, to build the vacuum environment in the upper cavity 101.
The case lid 8 is arranged on one end of the upper cavity 101, covers one end of the upper cavity 101.On described Cavity 101 provides environment for accommodating reactant (metal salt, organic ligand).First funnel 13 is arranged in institute The one end of upper cavity 101 far from the case lid 8 is stated, is contained in the upper cavity 101.The mouth direction of first funnel 13 The case lid 8, the 4th valve 4 are arranged on the spout of funnel of first funnel 13.
First fluid path includes pipeline and the first valve 1, and first valve 1 is arranged on the pipeline.The pipeline One end enters in the upper cavity 101 after passing through the case lid 8.In present embodiment, the pipeline is using made of glass. Wherein, solvent (water, ethyl alcohol, acetone etc.) is added into the upper cavity 101 by first fluid path.
The suction filtration mechanism includes lower chamber 102, the second funnel 14, filter membrane 11, the 5th valve 5 and third gas circuit, under described Cavity 102 is cylindrical shape, is open towards first funnel 13.Second funnel 14 is arranged in the lower chamber 102, It is open towards the junction 103 formed between the upper cavity 101 and the lower chamber 102.5th valve 5 is arranged in institute On the spout of funnel for stating the second funnel 14.The edge of the filter membrane 11 is connected on the inner wall of the lower chamber 102, and its setting exists On second funnel 14.The third gas circuit includes third tracheae and the 6th valve 6, and one end of the third tracheae passes through described It is protruded into after Ultrasonic Heating mechanism 12 and the lower chamber 102 in the lower chamber 102, the other end is connected to vacuum pump.Described Six valves 6 are arranged on the third tracheae.In present embodiment, the third tracheae is located at the lower section of second funnel 14; The lower chamber 102 and the part upper cavity 101 are contained in the Ultrasonic Heating mechanism 12, the Ultrasonic Heating mechanism 12 With heating function.
Second fluid path includes stainless steel tube and the 7th valve 7, and the lower chamber 102 is protruded into one end of the stainless steel tube Interior, the 7th valve 7 is arranged on the stainless steel tube.Second fluid path is used for useless by what is generated in the lower chamber 102 Liquid discharge.
In present embodiment, the filter membrane 11 is made of stainless steel;First tracheae, second gas Pipe and the third tracheae are made of stainless steel material;The cavity 10 is made of metal material;The conjunction The component for needing to contact with reactant in forming apparatus is not with reactant reaction, the equal high temperature resistant low pressure of component in the cavity 10 (0~300 DEG C, 0~0.1MPa).
Reactant is heated by the Ultrasonic Heating mechanism 12 in the upper cavity 101 and starts to react, and reacts generation Product enters the lower chamber 102 by the 4th valve 4, and is added by first fluid path into the upper cavity 101 Solvent, to be cleaned by ultrasonic to the upper cavity 101.The filter membrane 11 filters out reaction product, while by described Third gas circuit is vacuumized the solvent quickly to filter out in reaction product to the lower chamber 102 and is dissolved in solvent miscellaneous Matter.Finally, the metal-organic framework material of 12 pairs of synthesis of the Ultrasonic Heating mechanism heats, being achieved in metal has machine frame The vacuum drying of frame material, the metal-organic framework material after drying take out the synthesis that metal-organic framework material can be completed.
Multi-functional synthesis device provided by the invention suitable for metal-organic framework material, the synthesis device have single The ability of metal-organic framework material synthesis overall process is solely completed, so that the synthesis process of metal-organic framework material can be to avoid The transfer repeatedly of more instruments used back and forth with sample, reduces the workload of operator, improves metal organic frame material The yield of material makes it possible that metal-organic framework material is mass produced.In addition, the upper cavity of the synthesis device and under Gas circuit is respectively set in cavity, so that it includes the multiple gases atmosphere such as air, moving air, inert gas and vacuum that cavity, which meets, Requirement of experiment;Meanwhile addition metal filtration film and vacuum pump in lower chamber so that metal-organic framework material and soluble impurity and Solvent can quick separating, reduce filtration time, so that the purification of the metal-organic framework material and drying process are more Fast.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include Within protection scope of the present invention.

Claims (10)

1. a kind of multi-functional synthesis device suitable for metal-organic framework material, it is characterised in that:
The synthesis device includes gas displacement mechanism, filters mechanism, Ultrasonic Heating mechanism (12), the first fluid path (9) and second Fluid path, the gas displacement mechanism are removably attachable to the suction filtration mechanism, and the suction filtration mechanism and the part gas are set Structure of changing planes is contained in the Ultrasonic Heating mechanism (12);First fluid path (9) and second fluid path are separately positioned on described In gas displacement mechanism and the suction filtration mechanism;
By adding solvent in the first fluid path (9) Xiang Suoshu gas displacement mechanism;The gas displacement mechanism is for accommodating Reactant and corresponding atmosphere is provided for the reaction of reactant, and sends the synthetic product after reactant reaction to the suction filtration Mechanism;The mechanism that filters is used for the metal-organic framework material and soluble impurity of the synthetic product and the separation of solvent And it is dry;Second fluid path is for being discharged the suction filtration waste liquid within the organization;The Ultrasonic Heating mechanism (12) passes through ultrasound Vibration is also used to heat to the metal-organic framework material suction filtration mechanism mix reactant It is dried.
2. being suitable for the multi-functional synthesis device of metal-organic framework material as described in claim 1, it is characterised in that: synthesis After product is from the gas displacement mechanism into the suction filtration mechanism, pass through the first fluid path (9) Xiang Suoshu gas displacement machine Adding liquid in structure, then the Ultrasonic Heating mechanism (12) is cleaned by ultrasonic the gas displacement mechanism.
3. being suitable for the multi-functional synthesis device of metal-organic framework material as described in claim 1, it is characterised in that: described Gas displacement mechanism includes the first gas circuit, the second gas circuit, upper cavity (101) and the first funnel (13), first gas circuit and institute The second gas circuit is stated to be separately positioned on the upper cavity (101);The upper cavity (101) is cylindrical, first funnel (13) setting is located at the open end of the upper cavity (101) in the upper cavity (101);First air circuit connection in It is anti-needed for reactant reaction to build to be passed through predetermined gas into the upper cavity (101) by first gas circuit for gas cylinder Answer atmosphere;Second air circuit connection is in vacuum pump, by the vacuum pump and second gas circuit to the upper cavity (101) It is vacuumized.
4. being suitable for the multi-functional synthesis device of metal-organic framework material as claimed in claim 3, it is characterised in that: described Gas displacement mechanism further includes the 4th valve (4), and the 4th valve (4) is arranged on the spout of funnel of first funnel (13).
5. being suitable for the multi-functional synthesis device of metal-organic framework material as claimed in claim 3, it is characterised in that: described Gas displacement mechanism further includes case lid (8), and the case lid (8) is removably disposed in the upper cavity (101) far from the pumping One end of filter structure, first fluid path are arranged on the case lid (8).
6. the multi-functional synthesis device as described in any one in claim 1-5 suitable for metal-organic framework material, feature Be: the suction filtration mechanism includes the second funnel (14), lower chamber (102) and third gas circuit, the second funnel (14) setting In the lower chamber (102), the third gas circuit is arranged on the lower chamber (102), and it is located at second funnel (14) between second fluid path;The third air circuit connection is in vacuum pump.
7. being suitable for the multi-functional synthesis device of metal-organic framework material as claimed in claim 6, it is characterised in that: described Filtering mechanism further includes filter membrane (11), and the filter membrane (11) is arranged on second funnel (14), is used to filter out synthesis and produces Solvent and soluble impurity in object.
8. being suitable for the multi-functional synthesis device of metal-organic framework material as claimed in claim 7, it is characterised in that: described Filter membrane (11) is using made of stainless steel.
9. the multi-functional synthesis device as described in any one in claim 1-5 suitable for metal-organic framework material, feature Be: second fluid path includes stainless steel tube and the 7th valve (7), and the suction filtration mechanism is protruded into one end of the stainless steel tube Interior, the 7th valve (7) is arranged on the stainless steel tube.
10. the multi-functional synthesis device as described in any one in claim 1-5 suitable for metal-organic framework material, feature Be: first fluid path (9) includes pipeline and the first valve (1), and first valve (1) is arranged on the pipeline;The pipe The one end in road is protruded into the gas displacement mechanism;The pipeline is using made of glass.
CN201910574308.XA 2019-06-28 2019-06-28 Multifunctional synthesis equipment suitable for metal organic framework material Active CN110339791B (en)

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Publication number Priority date Publication date Assignee Title
CN111921528A (en) * 2020-06-28 2020-11-13 济南大学 Method and system for preparing slurry bed Fischer-Tropsch synthesis catalyst slurry by pyrolyzing MOFs

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