CN213160759U - Preparation facilities of yolk-shell structure covalence organic framework material - Google Patents

Preparation facilities of yolk-shell structure covalence organic framework material Download PDF

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CN213160759U
CN213160759U CN202021494332.7U CN202021494332U CN213160759U CN 213160759 U CN213160759 U CN 213160759U CN 202021494332 U CN202021494332 U CN 202021494332U CN 213160759 U CN213160759 U CN 213160759U
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spray
organic framework
framework material
yolk
covalent organic
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禹杰
李�瑞
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Suzhou Shifuan Material Technology Co ltd
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Suzhou Shifuan Material Technology Co ltd
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Abstract

The utility model discloses a yolk-shell structure covalent organic framework material preparation device, which comprises a covalent organic framework material preparation device and a spray transmission device which are connected in sequence, wherein the spray transmission device comprises a plurality of spray areas separated by a plurality of spray transmission chamber clapboards, and each spray area is provided with a corresponding spray head; the spray header is communicated with the multi-type spray reagent pipeline, and the multi-type spray reagent pipeline comprises an acidic reagent pipeline, an alkaline reagent pipeline and a washing reagent pipeline which are communicated with the multi-type spray reagent pipeline. According to the utility model discloses the preparation facilities who realizes, the utility model provides a preparation facilities utilizes the conveyer to bring the transmission of carrying out corresponding reactant to use the baffle to form a plurality of spray rooms, and be filtration membrane preparation at the conveyer belt, can realize the more abundant sculpture of silica structure, make the result more excellent.

Description

Preparation facilities of yolk-shell structure covalence organic framework material
Technical Field
The utility model belongs to covalence organic framework material preparation facilities field, concretely relates to yolk-shell structure covalence organic framework material's preparation facilities.
Background
Covalent Organic Frameworks (COFs) are porous materials which are connected by building units through reversible covalent bonds, and are novel porous crystalline materials with ordered pore channel structures. The porous crystalline material has potential application value in the fields of gas storage, chemical sensing, drug release, heterogeneous catalysis and photoelectricity. In the past decade, many two-dimensional or three-dimensional COFs have been obtained by selecting various building blocks, and the structural synthesis thereof focuses on the selection of building elements and the design of structures, which are also important factors for determining the performance of COF materials. However, the structural units for synthesizing COFs are mainly concentrated on organic structural units, which limits the structural and functional diversity of COFs to some extent. Therefore, the development of the multi-metal composite construction unit has important significance for enriching the structure and the function of the COFs material.
At present, a silica-based COF material with a yolk-shell structure nanotube decoration hollow structure becomes a hot point of research, on one hand, a covalent organic framework material with a yolk-shell structure has high catalytic activity, and on the other hand, silica (SiO2) becomes one of the most researched materials due to cost effectiveness, nontoxicity, high thermal stability and high chemical stability. However, no device suitable for large-scale production of the material exists at present, and the device needs to meet the requirements of industrialization, uniform etching reaction and no influence on product appearance, and simultaneously needs to overcome the defect that the etching amount of weak acid or weak base in the process flow is not easy to control.
SUMMERY OF THE UTILITY MODEL
To the above defect or improvement demand of prior art, the utility model provides a yolk-shell structure covalence organic framework material's preparation facilities uses this device can prepare the covalence organic framework material who has yolk-shell structure, and this material surface multi-stage functionalization possesses high catalytic activity.
The utility model provides a yolk-shell structure covalent organic framework material preparation device, which comprises a covalent organic framework material preparation device and a spraying and conveying device;
the spraying and conveying device comprises a plurality of spraying and conveying chamber partition plates, the spraying and conveying chamber partition plates divide the spraying and conveying device into a plurality of spraying areas, and each spraying area is provided with a corresponding spraying head;
the spray header is communicated with the multi-type spray reagent pipeline, and the multi-type spray reagent pipeline comprises an acidic reagent pipeline, an alkaline reagent pipeline and a washing reagent pipeline.
Preferably, a conveyor belt made of a filter membrane material is arranged inside the washing and drying chamber, and the conveyor belt divides the plurality of spraying areas into a spraying cavity and a filtrate cavity.
Preferably, the discharge port of the covalent organic framework material preparation device is communicated with the feeding conveying end of a conveying belt in the spraying conveying device, and the conveying belt drives the reaction product to pass through a plurality of spraying areas, so that the reaction product is alternately sprayed by the acidic reagent, the alkaline reagent and the washing reagent in the plurality of spraying areas.
Preferably, the conveyor belt is provided with a conveying vibration roller.
Preferably, a liquid outlet of a filtrate cavity of the spraying and conveying device is communicated with a waste liquid treatment device, and the waste liquid treatment device is at least a three-stage waste liquid treatment device.
Preferably, the device also comprises a washing and drying chamber, and the discharge hole of the spraying conveying device is connected with the feed hole of the washing and drying chamber through a conveying belt.
Preferably, a filter membrane conveyor belt is arranged in the washing and drying chamber.
Preferably, the liquid outlet of the washing and drying chamber is communicated with a waste liquid treatment device.
Generally, through the utility model discloses above technical scheme who conceives compares with prior art, has following beneficial effect:
1. the utility model provides a yolk-shell structure covalent organic framework material preparation device, which is applicable to large-scale production, and fully contacts spray etching reaction in a conveyor belt mode, so that the reaction product result is more excellent;
2. the utility model provides a yolk-shell structure covalent organic framework material preparation device, wherein the preparation material of the conveyor belt is mainly a filter membrane, so that the spraying reaction contact of solid-phase reactants can be more sufficient, and the spraying contact of a larger area can be realized;
3. the utility model provides a novel device for preparing a yolk-shell structure covalent organic framework material, wherein a vibration conveying roller is arranged on the filtering and conveying device, so that a solid phase aggregate on a filtering membrane does not generate large-particle aggregation of the yolk-shell structure covalent organic framework as much as possible;
4. this real preparation facilities with novel covalent organic framework material of a yolk-shell structure that provides, this spray conveyer's filtrating chamber liquid outlet and waste liquid treatment device intercommunication, waste liquid treatment device is at least tertiary waste liquid treatment device, can in time collect the waste liquid, prevents that the waste liquid from highly passing the conveyer belt, makes the result take place secondary pollution.
Drawings
FIG. 1 is a schematic diagram of the structure of a device for preparing a yolk-shell structure covalent organic framework material according to the present invention;
the same reference numbers will be used throughout the drawings to refer to the same or like elements or structures, wherein:
the device comprises a covalent organic framework material preparation device-1, a spray conveying device-2, a conveying belt-3, a spray head-4, a spray conveying chamber partition-5, a spray reagent pipeline-6, a conveying vibration roller-7, a first waste liquid treatment device-8, a second waste liquid treatment device-9, a third waste liquid treatment device-10 and a washing and drying chamber-11.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in 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. Furthermore, the technical features mentioned in the embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
It should be noted that the term "first/second" in the present invention is used only for distinguishing similar objects, and does not represent a specific ordering for the objects, and it should be understood that "first/second" may be interchanged with a specific order or sequence if allowed. It should be understood that "first \ second" distinct objects may be interchanged under appropriate circumstances such that embodiments of the invention described herein may be practiced in sequences other than those described or illustrated herein.
According to the utility model relates to a specific embodiment provides a preparation facilities of yolk-shell structure covalence organic framework material for the preparation needs carry out the covalence organic framework material of acid/alkali sculpture, is used for preparing the covalence organic framework material of yolk-shell structure, and this material is preferred to use silicon dioxide as the core, and the organic framework material of cladding covalence, and the rethread weak acid or weak base spray in turn, form the covalence organic framework material of yolk-shell structure. Therefore, the process flow using the device comprises the following steps: firstly, preparing covalent organic framework material with silicon dioxide as nucleus, after alternatively spraying by weak acid or weak base, washing and drying to obtain the corresponding product.
As shown in fig. 1, the utility model discloses a yolk-shell structure covalence organic framework material's preparation facilities, it is including setting up the conveying device 2 that sprays behind covalence organic framework material preparation facilities 1, and in an embodiment wherein, above-mentioned spraying device includes a plurality of spray zone that are separated by a plurality of spray conveying room baffles 5, and every spray zone all is provided with corresponding shower head 4.
The preparation device also comprises a spray pipeline 6 which is communicated with the multi-stage spray header 4 and mainly comprises an acidic spray pipeline, an alkaline spray pipeline and a washing solvent spray pipeline, and is used for spraying corresponding washing reagent to the inner cavity separated by the partition board of the transfer chamber through the spray header, wherein in one embodiment, the pipeline can be a conveying pipeline, and the multi-stage spray pipeline can also be arranged according to the type and the condition of the sprayed reagent.
Wherein the acidic spray reagent comprises: hydrobromic acid, hydrogen iodide, hydrofluoric acid, polyphosphoric acid, phosphorous acid, phosphoric acid, phosphomolybdic acid, hypophosphorous acid, iodic acid, dilute hydrochloric acid, dilute sulfuric acid, boric acid, tungstic acid, metaphosphoric acid, perrhenic acid, silicotungstic acid, hydrate sulfonic acid, phosphotungstic acid, selenic acid, iodoacetic anhydride, hydrogen bromide, and acetic acid.
Wherein the alkaline spray reagent comprises: sodium carbonate, potassium carbonate, sodium acetate, potassium acetate, sodium bicarbonate, sodium phenolate, potassium bicarbonate, sodium hydroxide, potassium hydrogen phosphate, potassium dihydrogen phosphate, trimethyl ammonium hydroxide, triethyl ammonium hydroxide, triethylamine or a mixture thereof.
Wherein the washing reagent mainly comprises: one or more of absolute ethyl alcohol, absolute methanol, water, ethyl acetate, acetone, petroleum ether, dichloromethane, trichloromethane, tetrachloromethane, acetonitrile, N, N-dimethylformamide, N, N-diethylformamide and the like.
Further, the spraying manner of the spraying reagent is an alternate spraying manner, namely spraying is performed in different spraying chambers separated by partition plates, after the reagent is sprayed and then washed by the washing reagent, then spraying is performed by the alkaline spraying reagent, and then washing is performed by the washing reagent, so that spraying is performed alternately.
Further, a conveyor belt 3 made of a filter membrane material is arranged inside the spraying and conveying device 2, and the conveyor belt 3 divides the plurality of spraying areas into a spraying cavity and a filtrate cavity.
Furthermore, the discharge port of the covalent organic framework material preparation device 1 is communicated with the feeding conveying end of a conveying belt 3 in a spraying conveying device 2, and the conveying belt 3 drives the reaction products to pass through a plurality of spraying areas, so that the reaction products are alternately sprayed by the acidic reagent, the alkaline reagent and the washing reagent in the plurality of spraying areas. The covalent organic framework material preparation device 1 prepares covalent organic framework products taking silicon dioxide as a core through reaction, and the products form the yolk-shell structure covalent organic framework material after being alternately etched by acid and alkali through a plurality of spraying areas by a conveyor belt 3.
Furthermore, the covalent organic framework material preparation device 1 is used for preparing a core-shell structure which takes silicon dioxide as a core to coat the covalent organic framework, the main method is that silicon dioxide, two ligand solutions and a solvent are input through a feed inlet and react in the covalent organic framework material preparation device 1, the covalent organic framework material preparation device 1 is of a reaction kettle structure and is provided with a heating device and a pressure regulation device, and the reaction can be set at the optimal reaction condition. After the reaction is finished, the reaction product enters a spraying and conveying device 2 to be sprayed and washed firstly, and then acid and alkali are alternately sprayed.
Further, the covalent organic skeleton may be prepared by including two kinds of ligands, and the first ligand may include at least one of trimesic aldehyde, terephthalaldehyde, tetrakis (4-formylbenzene) methane, tetraaldehyde phenylporphyrin, 3',5,5' -tetraaldehyde biphenyl, 2 '-bipyridine-5, 5' -dicarboxaldehyde, 2, 5-dihydroxyterephthalaldehyde, 2, 5-dimethoxybenzene-1, 4-dicarboxaldehyde, 2, 5-diformylfuran, 1,3, 5-trialdehyde phloroglucinol, and the like, but is not limited thereto. The second ligand includes, but is not limited to, at least one of p-phenylenediamine, melem, biphenyldiamine, 5,15- (aminophenyl) -10, 20-phenylporphyrin, tetrakis (4-aminophenyl) methane, tris (4-aminophenyl) amine, 5 '-diamino-2, 2' -bipyridine, 2,4, 6-tris (4-aminophenoxy) -1,3, 5-triazine, 1,3, 5-tris (4-aminophenyl) benzene, and the like.
Furthermore, a conveyor belt with a conveying vibration roller 7 is arranged in the spraying conveying device 2, the material of the conveyor belt mainly comprises a filtering membrane, so that solid-phase filtered substances can be in more sufficient contact with sprayed reagents on the conveying membrane, and in order to generate aggregation of large particles with resistance, the conveyor belt avoids the generation of the large particles in a mode of conveying the vibration roller 6.
Further, at least 3 levels of waste liquid treatment devices 8,9 and 10 are arranged inside the spray conveying device 2, wherein the liquid in the liquid storage space after the filtration membrane is required to penetrate through the spray conveying device 2 cannot exceed the standard, so that a multi-level waste liquid treatment device is required to be arranged later, wherein the devices are not only arranged in three levels, and at least three levels are communicated for better treating the waste liquid. Multistage waste liquid treatment device can effectively communicate and prevent that the waste liquid from submerging conveyer belt 3 or flowing backwards, carries out secondary pollution to the product to realize the processing of synthesizing.
Further, the device also comprises a washing and drying chamber 11, and a discharge port of the spraying conveying device 2 is connected with the washing and drying chamber 11 through a conveying belt.
Further, a filtering membrane conveyor belt is arranged in the cavity of the washing and drying chamber 11.
Further, the liquid outlet of the washing and drying chamber 11 is communicated with the waste liquid treatment devices 8,9 and 10.
It will be understood by those skilled in the art that the foregoing is merely a preferred embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.

Claims (8)

1. A yolk-shell structure covalent organic framework material preparation device, which is characterized by comprising a covalent organic framework material preparation device (1) and a spray conveying device (2);
the spraying and conveying device (2) comprises a plurality of spraying and conveying chamber partition plates (5), the spraying and conveying chamber partition plates (5) divide the spraying and conveying device (2) into a plurality of spraying areas, and each spraying area is provided with a corresponding spraying head (4);
the spray header (4) is communicated with the multi-type spray reagent pipeline (6), and the multi-type spray reagent pipeline (6) comprises an acidic reagent pipeline, an alkaline reagent pipeline and a washing reagent pipeline.
2. Apparatus for the preparation of yolk-shell structured covalent organic framework material as claimed in claim 1, characterized in that the spray conveyor (2) is internally provided with a conveyor belt (3) made of filter membrane material, said conveyor belt (3) dividing a plurality of said spray zones into spray and filtrate chambers.
3. The apparatus for preparing yolk-shell structural covalent organic framework material as claimed in claim 2, wherein the discharge port of said apparatus (1) for preparing covalent organic framework material is connected with the feed conveying end of the conveyor belt (3) in said spray conveyor (2), said conveyor belt (3) drives the reaction product through a plurality of said spray zones, so that said reaction product is alternately sprayed with acidic reagent, alkaline reagent and washing reagent in said plurality of said spray zones.
4. Apparatus for the preparation of yolk-shell structured covalent organic framework material as claimed in claim 2, wherein said conveyor belt is provided with a conveyor vibrating roller (7).
5. Apparatus for the preparation of yolk-shell structured covalent organic framework material as claimed in claim 2, wherein the filtrate chamber outlet of said spray conveyor (2) is in communication with a waste liquid treatment apparatus (8-10), said waste liquid treatment apparatus (8-10) being at least a three-stage waste liquid treatment apparatus.
6. The apparatus for preparing yolk-shell structural covalent organic framework material as claimed in claim 1, wherein the apparatus further comprises a washing and drying chamber (11), and the outlet of the spray conveyor (2) is connected with the inlet of the washing and drying chamber (11) by a conveyor belt.
7. Apparatus for the preparation of yolk-shell structured covalent organic framework material as claimed in claim 6, wherein a filter membrane conveyor belt is arranged inside the washing and drying chamber (11).
8. Apparatus for the preparation of yolk-shell structured covalent organic framework material as claimed in claim 6, wherein the outlet of said washing and drying chamber (11) is connected to a waste liquid treatment apparatus (8-10).
CN202021494332.7U 2020-07-25 2020-07-25 Preparation facilities of yolk-shell structure covalence organic framework material Active CN213160759U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113504274A (en) * 2021-07-20 2021-10-15 郑州轻工业大学 Covalent organic framework material, preparation method and application thereof, aptamer sensor and preparation method thereof
CN114931924A (en) * 2022-06-20 2022-08-23 珠海天威飞马打印耗材有限公司 Chlorine dioxide preparation equipment and preparation method thereof
CN114984894A (en) * 2022-06-20 2022-09-02 珠海天威飞马打印耗材有限公司 Chlorine dioxide preparation equipment and preparation method thereof
CN116078431A (en) * 2022-12-13 2023-05-09 湘潭大学 Au-based catalytic material based on hollow TTI-COF and application of Au-based catalytic material in catalyzing reduction of 4-nitrophenol

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113504274A (en) * 2021-07-20 2021-10-15 郑州轻工业大学 Covalent organic framework material, preparation method and application thereof, aptamer sensor and preparation method thereof
CN113504274B (en) * 2021-07-20 2023-11-21 郑州轻工业大学 Covalent organic framework material, preparation method and application thereof, aptamer sensor and preparation method thereof
CN114931924A (en) * 2022-06-20 2022-08-23 珠海天威飞马打印耗材有限公司 Chlorine dioxide preparation equipment and preparation method thereof
CN114984894A (en) * 2022-06-20 2022-09-02 珠海天威飞马打印耗材有限公司 Chlorine dioxide preparation equipment and preparation method thereof
CN114931924B (en) * 2022-06-20 2024-07-05 珠海天威飞马打印耗材有限公司 Chlorine dioxide preparation equipment and preparation method thereof
CN114984894B (en) * 2022-06-20 2024-07-12 珠海天威飞马打印耗材有限公司 Chlorine dioxide preparation equipment and preparation method thereof
CN116078431A (en) * 2022-12-13 2023-05-09 湘潭大学 Au-based catalytic material based on hollow TTI-COF and application of Au-based catalytic material in catalyzing reduction of 4-nitrophenol

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