CN110339791B - Multifunctional synthesis equipment suitable for metal organic framework material - Google Patents

Multifunctional synthesis equipment suitable for metal organic framework material Download PDF

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Publication number
CN110339791B
CN110339791B CN201910574308.XA CN201910574308A CN110339791B CN 110339791 B CN110339791 B CN 110339791B CN 201910574308 A CN201910574308 A CN 201910574308A CN 110339791 B CN110339791 B CN 110339791B
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suction filtration
gas
organic framework
path
filtration mechanism
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CN110339791A (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 Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field related to material synthesis equipment, and discloses multifunctional synthesis equipment suitable for metal organic framework materials, which comprises a gas replacement mechanism, a suction filtration mechanism, an ultrasonic heating mechanism, a first liquid path and a second liquid path, wherein the gas replacement mechanism is detachably connected to the suction filtration mechanism, and the suction filtration mechanism and part of the gas replacement mechanism are accommodated in the ultrasonic heating mechanism; the first liquid path and the second liquid path are respectively arranged on the gas replacement mechanism and the suction filtration mechanism; the gas displacement mechanism is used for accommodating reactants and providing corresponding atmosphere for the reaction of the reactants, and a synthetic product obtained after the reaction of the reactants is transmitted to the suction filtration mechanism; the suction filtration mechanism is used for separating and drying the metal organic framework material of the synthesized product, soluble impurities and a solvent; the second liquid channel is used for discharging waste liquid in the suction filtration mechanism; the ultrasonic heating mechanism is used for heating the suction filtration mechanism so as to dry the metal organic framework material. The invention improves the synthesis rate and has stronger applicability.

Description

Multifunctional synthesis equipment suitable for metal organic framework material
Technical Field
The invention belongs to the technical field related to material synthesis equipment, and particularly relates to multifunctional synthesis equipment suitable for metal organic framework materials.
Background
The metal organic framework materials (called MOFs for short) are organic-inorganic hybrid materials and are formed by self-assembling organic ligands and metal salts, and the metal organic framework materials are extremely diverse in types, diversified in structure and excellent in porous characteristics, so that the metal organic framework materials are widely applied to the fields of gas adsorption and separation, catalysis, energy storage and the like.
At present, there are many synthesis methods of metal organic framework materials, such as an ultrasonic method, a solvothermal method, a stirring method, a microwave heating method, and the like, and among them, the solvothermal method is the most conventional synthesis method, and the solvothermal method requires the use of a plurality of instruments such as an ultrasonic machine, a centrifuge, an oven, a vacuum oven, and the like, and the finally obtained metal organic framework materials are inevitably lost along with the transfer of products in containers in different instruments; meanwhile, various instruments are required to be operated in the synthesis process, which also brings inconvenience to experimenters.
The gas atmosphere required for synthesizing different organic framework materials is different, part of the metal organic framework material synthesis can be completed in the air, and part of the metal organic framework material synthesis process needs the participation of special gas, such as oxygen or carbon dioxide; and in addition, part of metal organic framework materials are synthesized in inert gas because the atmospheric environment interferes with the synthesis process. In addition, after the metal organic framework material is synthesized, impurities in the metal organic framework material need to be removed, the process is called as activation (or purification) of the metal organic framework material, the specific implementation method of the activation process is to sequentially use deionized water and organic solvents (ethanol, acetone and the like) to ultrasonically clean solid products for many times, separate the solid products, and finally dry and separate the solid products to obtain the solid products, wherein the solid product separation process is difficult, a centrifugal method is usually used in a laboratory, but the method is long in time consumption, high in loss, low in yield and not suitable for industrial production; another method is to remove soluble impurities and solvents by filtration, but the filtration rate is very slow at atmospheric pressure. Accordingly, there is a need in the art to develop a multifunctional synthesis apparatus with better synthesis rate, which is suitable for metal organic frame materials.
Disclosure of Invention
Aiming at the defects or improvement requirements in the prior art, the invention provides multifunctional synthesis equipment suitable for metal organic framework materials, which is based on the environment and synthesis characteristics required by the synthesis of the metal organic framework materials, and improves devices according to different requirements of the synthesis of the metal organic framework materials, so that the synthesis equipment can independently complete the whole synthesis process of the metal organic framework materials, and simultaneously avoids the loss in the purification process of samples, so that the synthesis of the metal organic framework materials is faster and more convenient, the synthesis rate is higher, and the applicability is stronger.
In order to achieve the purpose, the invention provides multifunctional synthesis equipment suitable for metal organic framework materials, which comprises a gas replacement mechanism, a suction filtration mechanism, an ultrasonic heating mechanism, a first liquid path and a second liquid path, wherein the gas replacement mechanism is detachably connected to the suction filtration mechanism, and the suction filtration mechanism and part of the gas replacement mechanism are accommodated in the ultrasonic heating mechanism; the first liquid path and the second liquid path are respectively arranged on the gas replacement mechanism and the suction filtration mechanism;
adding a solvent into the gas displacement mechanism through the first liquid path; the gas displacement mechanism is used for accommodating reactants and providing corresponding atmosphere for the reaction of the reactants, and a synthetic product obtained after the reaction of the reactants is transmitted to the suction filtration mechanism; the suction filtration mechanism is used for separating and drying the metal organic framework material of the synthesized product, soluble impurities and a solvent; the second liquid channel is used for discharging waste liquid in the suction filtration mechanism; the ultrasonic heating mechanism mixes reactants through ultrasonic vibration and is also used for heating the suction filtration mechanism so as to dry the metal organic framework material.
Further, after the synthetic product enters the suction filtration mechanism from the gas replacement mechanism, liquid is added into the gas replacement mechanism through the first liquid path, and then the ultrasonic heating mechanism carries out ultrasonic cleaning on the gas replacement mechanism.
Further, the gas replacement mechanism comprises a first gas path, a second gas path, an upper cavity and a first funnel, wherein the first gas path and the second gas path are respectively arranged on the upper cavity; the upper cavity is cylindrical, and the first funnel is arranged in the upper cavity and is positioned at the opening end of the upper cavity; the first gas path is connected with the gas cylinder, and predetermined gas is introduced into the upper cavity through the first gas path to create reaction atmosphere required by reactant reaction; the second air path is connected to the vacuum pump, and the upper cavity is vacuumized through the vacuum pump and the second air path.
Further, the gas replacement mechanism further comprises a fourth valve, and the fourth valve is arranged on the funnel mouth of the first funnel.
Further, the gas replacement mechanism further comprises a box cover, the box cover is detachably arranged at one end, far away from the suction filtration mechanism, of the upper cavity, and the first liquid path is arranged on the box cover.
Further, the suction filtration mechanism comprises a second funnel, a lower cavity and a third gas path, wherein the second funnel is arranged in the lower cavity, and the third gas path is arranged on the lower cavity and is positioned between the second funnel and the second liquid path; and the third air path is connected to a vacuum pump.
Further, the suction filtration mechanism also comprises a filter membrane, wherein the filter membrane is arranged on the second funnel and is used for filtering out the solvent and soluble impurities in the synthesized product.
Further, the filter membrane is made of stainless steel.
Furthermore, the second liquid path comprises a stainless steel tube and a seventh valve, one end of the stainless steel tube extends into the suction filtration mechanism, and the seventh valve is arranged on the stainless steel tube.
Further, the first fluid path comprises a pipeline and a first valve, and the first valve is arranged on the pipeline; one end of the pipeline extends into the gas replacement mechanism; the pipe is made of glass.
In general, compared with the prior art, the multifunctional synthesis equipment suitable for the metal organic framework material provided by the invention mainly has the following beneficial effects:
1. the gas displacement mechanism is used for accommodating reactants and providing corresponding atmosphere for the reaction of the reactants, and a synthetic product obtained after the reaction of the reactants is transmitted to the suction filtration mechanism; the suction filtration mechanism is used for separating and drying the metal organic framework material of the synthesized product from soluble impurities and a solvent, and the synthesis equipment can independently realize the whole process of the synthesis of the metal organic framework material, so that the synthesis process of the metal organic framework material can avoid the repeated use of a plurality of instruments and the repeated transfer of samples, the workload of operators is reduced, the MOFs yield is improved, and the large-scale production of the MOFs becomes possible.
2. The gas replacement mechanism is used for accommodating reactants and providing corresponding atmosphere for the reaction of the reactants, and meets the synthesis requirements of MOFs under specific atmosphere and various gas pressures.
3. The suction filtration mechanism further comprises a filter membrane, and the filter membrane is arranged on the second funnel and used for filtering out solvent and soluble impurities in the synthesized product.
4. And the third gas path is connected with a vacuum pump to vacuumize the lower cavity, so that the MOFs sample can be quickly separated from the solvent and impurities dissolved in the solvent, the filtering time is shortened, and the purification and drying processes of the sample are quicker.
Drawings
FIG. 1 is a schematic diagram of a multifunctional synthesis apparatus suitable for metal organic framework materials provided by the present invention.
The same reference numbers will be used throughout the drawings to refer to the same or like elements or structures, wherein: 1-a first valve, 2-a second valve, 3-a third valve, 4-a fourth valve, 5-a fifth valve, 6-a sixth valve, 7-a seventh valve, 8-a box cover, 9-a first liquid path, 10-a cavity, 101-an upper cavity, 102-a lower cavity, 103-a junction, 11-a filter membrane, 12-an ultrasonic heating mechanism, 13-a first funnel, and 14-a second funnel.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Referring to fig. 1, the multifunctional synthesis equipment suitable for metal organic framework materials provided by the present invention comprises a gas displacement mechanism, a suction filtration mechanism, an ultrasonic heating mechanism 12, a first liquid path 9 and a second liquid path, wherein the gas displacement mechanism is detachably connected to the suction filtration mechanism, and the suction filtration mechanism is arranged on the ultrasonic heating mechanism 12; the first liquid path 9 is connected to the gas replacement mechanism, and a solvent is added to the gas replacement mechanism through the first liquid path 9. The second liquid path is connected to the suction filtration mechanism and used for discharging waste liquid generated in the suction filtration mechanism. The atmosphere in the gas replacement mechanism is changed along with the currently synthesized metal organic framework material so as to meet the synthesis requirement of the currently synthesized metal organic framework material. The suction filtration mechanism is used for separating and drying the metal organic framework material, soluble impurities and solvent of the synthetic product synthesized by the gas displacement mechanism. The ultrasonic heating mechanism 12 ultrasonically cleans the gas displacement mechanism through ultrasonic vibration, and is also used for heating the suction filtration mechanism to complete drying of the synthesized metal organic framework material.
The gas replacement mechanism comprises a first gas circuit, a second gas circuit, an upper cavity 101, a box cover 8, a first funnel 13 and a fourth valve 4, wherein the upper cavity 101 is cylindrical, the first gas circuit and the second gas circuit are respectively arranged on one side of the upper cavity 101, one end of the first gas circuit is arranged in the upper cavity 101, and the other end of the first gas circuit is connected to a gas cylinder. The first gas path is used for introducing gases required by reactions such as air, oxygen, carbon dioxide, inert gas and the like into the upper cavity 101. One end of the second air path is arranged in the upper cavity 101, the other end of the second air path is connected to the vacuum pump, and the second air path can be used for vacuumizing the gas replacement mechanism.
In this embodiment, one end of the first gas path located in the upper chamber 101 is located below the liquid level of the reactant to displace the gas in the solution; the second gas circuit is located one end in last cavity 101 is located above the reactant liquid level, and accessible vacuum pump or direct through the atmosphere accomplish to bleed and aerify the process to build the vacuum environment in last cavity 101 or directly regard as the end of giving vent to anger.
The first air path comprises a first air pipe and a second valve 2, the second valve 2 is arranged on the first air pipe, one end of the first air pipe is contained in the upper cavity 101, and the other end of the first air pipe is connected with the air bottle, so that specific gas is introduced into the upper cavity 101 through the air bottle to create specific reaction atmosphere. The second air path comprises a second air pipe and a third valve 3, and the third valve 3 is arranged on the second air pipe. One end of the second air pipe is contained in the upper cavity 101, and the other end of the second air pipe is connected to the vacuum pump so as to exhaust the upper cavity 101, so that a vacuum environment in the upper cavity 101 is created.
The cover 8 is disposed on one end of the upper chamber 101, and covers one end of the upper chamber 101. The upper chamber 101 is used for accommodating reactants (metal salts, organic ligands) and providing an environmental atmosphere. The first funnel 13 is disposed at an end of the upper cavity 101 away from the case cover 8, and is accommodated in the upper cavity 101. The mouth of the first funnel 13 faces the box cover 8, and the fourth valve 4 is arranged on the funnel mouth of the first funnel 13.
The first liquid path comprises a pipeline and a first valve 1, and the first valve 1 is arranged on the pipeline. One end of the pipeline penetrates through the box cover 8 and then enters the upper cavity 101. In this embodiment, the pipe is made of glass. Wherein a solvent (water, ethanol, acetone, etc.) is added into the upper chamber 101 through the first liquid path.
The suction filtration mechanism comprises a lower cavity 102, a second funnel 14, a filter membrane 11, a fifth valve 5 and a third air path, wherein the lower cavity 102 is cylindrical, and the opening of the lower cavity faces the first funnel 13. The second funnel 14 is disposed in the lower cavity 102, and opens toward a junction 103 formed between the upper cavity 101 and the lower cavity 102. The fifth valve 5 is arranged on the mouth of the second funnel 14. The edge of the filter membrane 11 is attached to the inner wall of the lower chamber 102 and it is arranged on the second funnel 14. The third air passage comprises a third air pipe and a sixth valve 6, one end of the third air pipe penetrates through the ultrasonic heating mechanism 12 and the lower cavity 102 and then extends into the lower cavity 102, and the other end of the third air pipe is connected to the vacuum pump. The sixth valve 6 is provided on the third air pipe. In this embodiment, the third air pipe is located below the second hopper 14; the lower cavity 102 and a part of the upper cavity 101 are contained in the ultrasonic heating mechanism 12, and the ultrasonic heating mechanism 12 has a heating function.
The second liquid path comprises a stainless steel pipe and a seventh valve 7, one end of the stainless steel pipe extends into the lower cavity 102, and the seventh valve 7 is arranged on the stainless steel pipe. The second fluid path is used for discharging waste fluid generated in the lower chamber 102.
In the present embodiment, the filter membrane 11 is made of stainless steel; the first air pipe, the second air pipe and the third air pipe are all made of stainless steel materials; the cavity 10 is made of metal material; the parts of the synthesis equipment which need to be contacted with the reactants do not react with the reactants, and the parts in the cavity 10 are all high temperature resistant and low pressure resistant (0-300 ℃, 0-0.1 MPa).
The reactant is heated by the ultrasonic heating mechanism 12 in the upper chamber 101 and starts to react, a product generated by the reaction enters the lower chamber 102 through the fourth valve 4, and a solvent is added into the upper chamber 101 through the first liquid path, so that the upper chamber 101 is ultrasonically cleaned. The filter membrane 11 filters the reaction product, and simultaneously the third gas path is used for vacuumizing the lower cavity 102 to quickly filter the solvent in the reaction product and impurities dissolved in the solvent. Finally, the ultrasonic heating mechanism 12 heats the synthesized metal organic framework material, so that the metal organic framework material is vacuum-dried, and the dried metal organic framework material is taken out to complete the synthesis of the metal organic framework material.
The multifunctional synthesis equipment suitable for the metal organic framework material provided by the invention has the capability of independently finishing the whole synthesis process of the metal organic framework material, so that the synthesis process of the metal organic framework material can avoid the repeated use of a plurality of instruments and the repeated transfer of samples, the workload of operators is reduced, the yield of the metal organic framework material is improved, and the mass production of the metal organic framework material becomes possible. In addition, the upper cavity and the lower cavity of the synthesis equipment are respectively provided with an air path, so that the cavity can meet the experimental requirements of various gas atmospheres including air, flowing air, inert gas, vacuum and the like; meanwhile, a metal filter membrane and a vacuum pump are added in the lower cavity, so that the metal organic framework material, soluble impurities and a solvent can be quickly separated, the filtering time is reduced, and the purification and drying processes of the metal organic framework material are quicker.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. A multifunctional synthesis equipment suitable for metal organic framework materials is characterized in that:
the synthesis equipment comprises a gas replacement mechanism, a suction filtration mechanism, an ultrasonic heating mechanism (12), a first liquid path (9) and a second liquid path, wherein the gas replacement mechanism is detachably connected to the suction filtration mechanism, and the suction filtration mechanism and part of the gas replacement mechanism are accommodated in the ultrasonic heating mechanism (12); the first liquid path (9) and the second liquid path are respectively arranged on the gas displacement mechanism and the suction filtration mechanism;
adding a solvent into the gas displacement mechanism through the first liquid path (9); the gas displacement mechanism is used for accommodating reactants and providing corresponding atmosphere for the reaction of the reactants, and a synthetic product obtained after the reaction of the reactants is transmitted to the suction filtration mechanism; the suction filtration mechanism is used for separating and drying the metal organic framework material of the synthesized product, soluble impurities and a solvent; the second liquid channel is used for discharging waste liquid in the suction filtration mechanism; the ultrasonic heating mechanism (12) mixes reactants through ultrasonic vibration and is also used for heating the suction filtration mechanism to dry the metal organic framework material;
the gas replacement mechanism comprises a first gas path, a second gas path, an upper cavity (101) and a first funnel (13), wherein the first gas path and the second gas path are respectively arranged on the upper cavity (101); the upper cavity (101) is cylindrical, and the first funnel (13) is arranged in the upper cavity (101) and is positioned at the opening end of the upper cavity (101); the first gas path is connected with the gas cylinder, and predetermined gas is introduced into the upper cavity (101) through the first gas path to create a reaction atmosphere required by the reaction of reactants; the second air path is connected to a vacuum pump, and the upper cavity (101) is vacuumized through the vacuum pump and the second air path.
2. The multifunctional synthesis apparatus for metal-organic framework materials according to claim 1, characterized in that: and after the synthetic product enters the suction filtration mechanism from the gas replacement mechanism, liquid is added into the gas replacement mechanism through the first liquid path (9), and then the ultrasonic heating mechanism (12) performs ultrasonic cleaning on the gas replacement mechanism.
3. The multifunctional synthesis apparatus for metal-organic framework materials according to claim 1, characterized in that: the gas replacement mechanism further comprises a fourth valve (4), and the fourth valve (4) is arranged on the funnel mouth of the first funnel (13).
4. The multifunctional synthesis apparatus for metal-organic framework materials according to claim 1, characterized in that: the gas replacement mechanism further comprises a box cover (8), the box cover (8) is detachably arranged at one end, far away from the suction filtration mechanism, of the upper cavity (101), and the first liquid path is arranged on the box cover (8).
5. The multifunctional synthesis apparatus for metal-organic framework materials according to any of claims 1 to 4, characterized in that: the suction filtration mechanism comprises a second funnel (14), a lower cavity (102) and a third gas path, wherein the second funnel (14) is arranged in the lower cavity (102), and the third gas path is arranged on the lower cavity (102) and is positioned between the second funnel (14) and the second liquid path; and the third air path is connected to a vacuum pump.
6. The multifunctional synthesis apparatus for metal-organic framework materials according to claim 5, characterized in that: the suction filtration mechanism further comprises a filter membrane (11), wherein the filter membrane (11) is arranged on the second funnel (14) and is used for filtering out solvent and soluble impurities in the synthesized product.
7. The multifunctional synthesis apparatus for metal-organic framework materials according to claim 6, characterized in that: the filter membrane (11) is made of stainless steel.
8. The multifunctional synthesis apparatus for metal-organic framework materials according to any of claims 1 to 4, characterized in that: the second liquid path comprises a stainless steel tube and a seventh valve (7), one end of the stainless steel tube extends into the suction filtration mechanism, and the seventh valve (7) is arranged on the stainless steel tube.
9. The multifunctional synthesis apparatus for metal-organic framework materials according to any of claims 1 to 4, characterized in that: the first liquid path (9) comprises a pipeline and a first valve (1), and the first valve (1) is arranged on the pipeline; one end of the pipeline extends into the gas replacement mechanism; the pipe is made of glass.
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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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