CN213253867U - Preparation facilities of covalence organic frame complex film - Google Patents
Preparation facilities of covalence organic frame complex film Download PDFInfo
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- CN213253867U CN213253867U CN202021785844.9U CN202021785844U CN213253867U CN 213253867 U CN213253867 U CN 213253867U CN 202021785844 U CN202021785844 U CN 202021785844U CN 213253867 U CN213253867 U CN 213253867U
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Abstract
The utility model belongs to the field of covalent organic framework material preparation devices, and discloses a preparation device of a covalent organic framework composite membrane, which comprises a first storage tank, a second storage tank, a third storage tank, a reaction kettle, a collector, a washing dryer, an activation kettle, a PVDP melting kettle, a hollow wire drawing grinding tool and a cooling box which are connected in sequence; wherein, cavity wire drawing grinding apparatus includes feeding track, sprays the mouth and cavity wire drawing device, feeding track one end and feed inlet, and the other end is connected with cavity wire drawing device, sprays the mouth and sets up in feeding track top and communicate with the feed inlet. The feeding proportion of two feed inlets is invariable in the device, and continuous stable operation under normal production state, ammonia modified covalent organic frame solution through mix according to certain proportion with PVDP material, compound at abundant contact in-process, make the reaction fully go on, more homogeneous, abundant at the device reaction technology, easy operation.
Description
Technical Field
The utility model belongs to covalence organic framework material preparation facilities field, concretely relates to covalence organic frame composite film's preparation facilities.
Background
Covalent Organic Frameworks (COFs) are a class of crystalline organic porous materials synthesized by Omar m.yaghi et al in 2005 that are completely linked by covalent bonds of light elements (C, H, O, N, B, etc.). The covalent organic framework material takes organic micromolecules as a secondary construction unit, and is connected in a covalent bond mode through a framework chemical theory to construct a high molecular framework network. It has the characteristics of small density, large specific surface area, porosity, crystallinity and the like. In addition, the structure and the function of the covalent organic framework material can be regulated and controlled by designing the structure and the function of the organic micromolecule.
In addition, the film material can be used in the fields of separation, photoelectricity, sensing, energy storage and the like, and has important application value. However, conventional membrane materials, which are mostly polymers or ceramics, generally have a broad pore size distribution, have a problem of inaccurate separation. Linear polymers have strong flexibility and are easy to form films, and have been widely applied to the preparation of composite film materials, for example, polymers are compounded with Covalent Organic Frameworks (COFs) to prepare a good mixed mechanism film material, and the material has the properties of both polymers and COFs, including good crystallinity, high porosity and strong machinability. The research on the preparation process, particularly the preparation process flow device suitable for industrial popularization, becomes a research hotspot in the field.
At present, a device suitable for large-scale production of covalent organic framework composite membranes does not exist, and on one hand, the device needs to meet the requirement of reaction synthesis uniformity in industrialization and on the other hand, the device needs to overcome the defect that the doping proportion of the process flow is not easy to control.
SUMMERY OF THE UTILITY MODEL
To overcome the above defects or improve the requirements of the prior art, the utility model provides a preparation device of a covalent organic framework composite membrane, which is used for generating a COF (covalent organic framework) composite hollow-structure membrane silk material. The process flow of the device comprises the steps of preparing a covalent organic framework material through a synthesis reaction, modifying a basic functional group on the covalent organic framework, extracting a certain amount of ammonia-modified covalent organic framework according to a reaction proportion, washing, dissolving in a certain amount of solvent, melting PVDP, putting into a hollow wire-drawing grinding tool, spraying ammonia-modified covalent organic framework solution in the wire-drawing process, loading the covalent organic framework on the surface of the PVDP material through an ammonia group, cooling and washing to form the covalent organic framework composite membrane material.
In order to achieve the purpose, the utility model provides a preparation device of a covalent organic framework composite film, which comprises a first storage tank, a second storage tank, a third storage tank, a reaction kettle, a collector, a washing dryer, an activation kettle, a PVDP melting kettle, a hollow wire drawing grinding tool and a cooling tank which are connected in sequence;
wherein, the feed inlet of first storage tank and second storage tank bottom with feed inlet intercommunication on the reation kettle lateral wall, the third storage tank with the second feed inlet intercommunication on reation kettle top, the feed inlet is provided with spray set, the discharge gate of reation kettle bottom with the collection mouth intercommunication on collector top, the discharge gate of collector bottom through first pump with the feed inlet intercommunication on scrubbing dryer top, scrubbing dryer discharge gate through the second pump with the feed inlet intercommunication on activation cauldron top, the activation cauldron discharge gate with the feed inlet intercommunication on cavity wire drawing grinding apparatus top, PVDP melts the discharge gate of cauldron bottom with the feed inlet intercommunication of cavity wire drawing grinding apparatus lateral wall end, the discharge gate and the cooler bin discharge gate of cavity wire drawing grinding apparatus opposite lateral wall end pass through the track intercommunication.
Further, the cavity wire drawing grinding apparatus includes feeding track, sprays the mouth and cavity wire drawing device, feeding track one end with the feed inlet of cavity wire drawing grinding apparatus lateral wall end is connected, the other end with cavity wire drawing device is connected, spray the mouth set up in feeding track top and with the feed inlet intercommunication on cavity wire drawing grinding apparatus top.
Further, the hollow wire drawing grinding tool comprises a temperature sensor, a temperature control device and a display interface, the temperature sensor is arranged on the side wall of the inner cavity of the hollow wire drawing grinding tool, the output end of the temperature sensor is connected with the temperature control device, the temperature control device is electrically connected with the display interface, and the display interface is arranged on the outer wall of the hollow wire drawing grinding tool.
Furthermore, a filter membrane transmission crawler belt is arranged in the cooling box, and at least one cooling spraying device is arranged above the filter membrane transmission crawler belt.
Further, a vibration device is arranged on the filter membrane conveying crawler.
Further, the device also comprises a waste liquid treatment pool; and a waste liquid port of the washing dryer is communicated with a feeding port of the waste liquid treatment pool.
Further, a temperature controller and a pressure controller are arranged in the reaction kettle and the PVDP melting kettle.
Further, stirring devices are arranged in the reaction kettle, the activation kettle and the PVDP melting kettle.
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 preparation facilities of covalence organic frame complex film, the adoption has cavity wire drawing grinding apparatus, cavity wire drawing grinding apparatus includes the feeding track, spray mouthful and hollow wire drawing device, the feeding track in the PVDP input cavity wire drawing grinding apparatus after the high temperature melts, the covalence organic frame that ammonia was decorated sprays to PVDP carries out the load reaction to make covalence organic frame pass through ammonia functional group load on PVDP, form the compound PVDP material of covalence organic frame, the feeding proportion of two feed inlets is invariable. The continuous stable operation under normal production state, ammonia modified covalent organic framework solution through with PVDP material according to certain proportion mixture, compound at abundant contact in-process, make the reaction fully go on, the device reaction technology is more homogeneous, abundant, easy operation.
2. The utility model provides a preparation facilities of covalence organic frame complex film, the preparation of covalence organic frame that ammonia was decorated adopts reation kettle, and this reactor includes temperature controller and pressure controller, the reaction condition of effective control composite reaction on the one hand, and on the other hand passes through pressure adjustment and guarantees the pressure balance of response device, prevents to burst, production accidents such as product refluence, reactant overflow and produces.
3. The utility model provides a preparation facilities of covalence organic frame complex film can be suitable for COF (covalence organic frame) compound hollow structure's the scale production of membrane silk material. The composite reaction process can regulate and control the reaction proportion and the doping amount, and the washed wastewater is treated by designing a wastewater collecting and treating device, so that the reaction process is simple and controllable, and the environment is friendly.
Drawings
Fig. 1 is a schematic view of the overall structure of a device for preparing a covalent organic framework composite membrane according to the present invention;
fig. 2 is a detailed schematic diagram of an activation kettle, a PVDP melting kettle, a hollow wire drawing grinding tool and a cooling box 10 of a preparation apparatus for a covalent organic framework composite membrane 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 first storage tank-1, a second storage tank-2, a third storage tank-3, a reaction kettle-4, a collector-5, a washing dryer-6, an activation kettle-7, a PVDP melting kettle-8, a hollow wire drawing grinding tool-9, a cooling box-10, a stirring device-701 of the activation kettle, a feeding hole-901 at the top end of the hollow wire drawing grinding tool, a feeding hole-902 at one side wall end of the hollow wire drawing grinding tool and a temperature sensor-903.
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.
As shown in fig. 1, according to a preferred embodiment of the present invention, there is provided a manufacturing apparatus of a covalent organic framework composite membrane for forming a COF (covalent organic framework) composite hollow structure membrane wire material. Therefore, the process flow using the device comprises the following steps: firstly, preparing a covalent organic framework material through a synthetic reaction, spraying and soaking the covalent organic framework material through a high-concentration alkaline solution, modifying an alkaline functional group on the covalent organic framework, collecting an ammonia-modified covalent organic framework product, extracting a certain amount of ammonia-modified covalent organic framework according to a reaction proportion, washing the ammonia-modified covalent organic framework product, dissolving the ammonia-modified covalent organic framework product in a certain amount of solvent, melting PVDP, putting the molten PVDP into a hollow wire-drawing grinding tool, spraying the ammonia-modified covalent organic framework solution in a wire-drawing process, loading the covalent organic framework on the surface of the PVDP material through an ammonia group, controlling the reaction temperature in the hollow wire-drawing process, and recently cooling and washing the membrane material to form the covalent organic framework composite membrane material.
In this embodiment, the device for preparing the covalent organic framework composite membrane comprises a first storage tank 1, a second storage tank 2, a third storage tank 3, a reaction kettle 4, a collector 5, a washing dryer 6, an activation kettle 7, a PVDP melting kettle 8, a hollow wire drawing grinding tool 9 and a cooling tank 10 which are connected in sequence;
wherein, the feed inlet of first storage tank 1 and the feed inlet on the 2 bottoms of second storage tank communicate with the feed inlet on the 4 lateral walls of reation kettle, third storage tank 3 communicates with the second feed inlet on the 4 tops of reation kettle, the feed inlet is provided with spray set, the discharge gate of 4 bottoms of reation kettle communicates with the collection mouth on 5 tops of collector, the discharge gate of 5 bottoms of collector communicates with the feed inlet on 6 tops of scrubbing-and-drying ware through the first pump, the discharge gate of scrubbing-and-drying ware 6 communicates with the feed inlet on 7 tops of activation kettle through the second pump, the discharge gate of activation kettle 7 communicates with the feed inlet 901 on cavity wire drawing grinding apparatus top, PVDP melts the discharge gate of 8 bottoms and the feed inlet 902 intercommunication of a lateral wall end of cavity wire drawing grinding apparatus, the discharge gate of the other lateral wall end of cavity wire drawing grinding apparatus 9 passes.
More preferably, the reaction vessel 4 is used for preparing a covalent organic framework, the preparation of the covalent organic framework comprises two ligands, the first storage tank 1 and the second storage tank 2 are respectively used for storing a first ligand and a second ligand, the first ligand comprises at least one of mesitylene-benzaldehyde, terephthalaldehyde, tetrakis (4-formylbenzene) methane, tetra-aldehyde phenyl porphyrin, 3',5,5' -tetra-aldehyde biphenyl, 2 '-bipyridine-5, 5' -dicarboxaldehyde, 2, 5-dihydroxy terephthalaldehyde, 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.
More preferably, the third storage tank 3 is used for storing a high-concentration alkaline solution, and after the covalent organic framework is prepared and formed in the reaction kettle 4, the high-concentration alkaline solution is sprayed sufficiently to soak the covalent organic framework in the alkaline solution, so as to modify the alkaline functional groups on the covalent organic framework, wherein the alkaline solution 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, and the like.
More preferably, the covalent organic framework material modified by ammonia is generated by the reaction in the reaction kettle 4 and then collected by the collector 5, and a certain amount of the covalent organic framework modified by ammonia is extracted from the collector 5 according to the subsequent reaction proportion and then enters the washing dryer 6 for washing and drying.
More preferably, the washing dryer 6 is used to spray the solvent used for washing onto the reaction product, and then discharge the reaction waste liquid through a waste liquid port by means of a filtering device. The solvent used for washing includes, but is not limited to, preferably deionized water, absolute methanol, absolute ethanol, acetone, N-hexane, ethyl acetate, N-dimethylformamide, N-diethylformamide, dichloromethane, trichloromethane, tetrachloromethane, petroleum ether, tetrahydrofuran, pyridine, pyrrole, acetonitrile, toluene, 1, 4-dioxane, and the like.
More preferably, the activation kettle 7 is used for dispersing the washed ammonia modified covalent organic framework material by sufficient stirring, the activation kettle 7 includes a stirring device 701 therein, the dispersed ammonia modified covalent organic framework is sprayed into the cavity of the hollow wire-drawing grinding tool 9 through the feed inlet 901, and the solvent used for dispersion includes: anhydrous ethanol, anhydrous methanol, water, ethyl acetate, acetone, petroleum ether, dichloromethane, chloroform, tetrachloromethane, acetonitrile, N-dimethylformamide, N-diethylformamide, and the like, but is not limited thereto.
More preferably, the PVDP melter 8 is used for melting PVDP (polyvinylidene fluoride) at high temperatures, which has good chemical resistance, processability, and fatigue and creep resistance, and is one of the best materials for pumps, valves, pipes, piping fittings, tanks, and heat exchangers in the fluid treatment system of chemical plants, as a whole or lining. After melting the PVDP at a high temperature, the molten PVDP is fed into the hollow wire-drawing grinding tool 9 through the feed inlet 902.
As shown in fig. 2, the hollow wire drawing grinding tool 9 includes a feeding track, a spraying port and a hollow wire drawing device, one end of the feeding track is connected to the feeding port 902, the other end of the feeding track is connected to the hollow wire drawing device, and the spraying port is disposed above the feeding track and is communicated with the feeding port 901.
More preferably, after melting at high temperature, PVDP is fed into a feeding caterpillar in the hollow wire drawing grinding tool 9 through a feeding hole 902, an ammonia-modified covalent organic framework is sprayed to PVDP through a feeding hole 901 for carrying out a loading reaction, the feeding ratio of the two feeding holes is constant, the covalent organic framework is loaded on PVDP through an ammonia functional group to form a covalent organic framework composite PVDP material, and the material passes through a hollow wire drawing device to form a hollow membrane wire material, and is output for cooling and washing.
Preferably, the hollow wire-drawing grinding tool 9 comprises a temperature sensor 903, a temperature control device and a display interface, wherein the temperature sensor 903 is arranged on the side wall of the inner cavity of the hollow wire-drawing grinding tool 9, the output end of the temperature sensor 903 is connected with the temperature control device, the temperature control device is electrically connected with the display interface, and the display interface is arranged on the outer wall of the hollow wire-drawing grinding tool 9.
More preferably, the temperature sensor 903 collects the reaction wire drawing temperature in the hollow wire drawing grinding tool 9 and transmits temperature data to the temperature control device, the temperature control device controls the temperature according to the set temperature and displays the current temperature through the display interface, and the display interface is arranged on the outer wall of the hollow wire drawing grinding tool 9, so that human-computer interaction can be performed, and the temperature setting and the current temperature display can be performed.
Preferably, a filter membrane conveying crawler is arranged in the cooling box 10, and at least one cooling spraying device is arranged above the filter membrane conveying crawler.
More preferably, the cooling tank 10 is provided with a filter membrane conveying crawler belt to convey the product, and the product is cooled and washed by an upper cooling spraying device, and finally output.
Preferably, the filter membrane conveying crawler is provided with a vibration device. For uniform dispersion of the product.
Preferably, the device also comprises a waste liquid treatment tank 11; the waste liquid port of the washing dryer 6 is communicated with the feeding port of the waste liquid treatment tank 11. The method is used for collecting and treating waste liquid, and can recycle or degrade the treated product into a standard capable of being discharged.
Preferably, a temperature controller and a pressure controller are arranged in the reaction kettle 4 and the PVDP melting kettle 8. The method is used for controlling the reaction temperature and pressure, so that the reaction is carried out under the optimal condition on one hand, the pressure of the reaction process is balanced on the other hand, and process accidents such as explosion caused by overlarge reaction pressure or backflow of an intermediate product caused by undersize pressure are avoided.
Preferably, stirring devices are arranged in the reaction kettle 4, the activation kettle 7 and the PVDP melting kettle 8. For the reaction to proceed sufficiently.
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, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included within the scope of the present invention.
Claims (8)
1. The preparation device of the covalent organic framework composite membrane is characterized by comprising a first storage tank (1), a second storage tank (2), a third storage tank (3), a reaction kettle (4), a collector (5), a washing dryer (6), an activation kettle (7), a PVDP melting kettle (8), a hollow wire drawing grinding tool (9) and a cooling box (10) which are sequentially connected;
wherein the feed inlets at the bottom ends of the first storage tank (1) and the second storage tank (2) are communicated with the feed inlet on the side wall of the reaction kettle (4), the third storage tank (3) is communicated with the second feed inlet at the top end of the reaction kettle (4), the feed inlets are provided with spray devices, the discharge outlet at the bottom end of the reaction kettle (4) is communicated with the collection port at the top end of the collector (5), the discharge outlet at the bottom end of the collector (5) is communicated with the feed inlet at the top end of the washing dryer (6) through a first pump, the discharge outlet of the washing dryer (6) is communicated with the feed inlet at the top end of the activation kettle (7) through a second pump, the discharge outlet of the activation kettle (7) is communicated with the feed inlet (901) at the top end of the hollow wire drawing grinding tool, the discharge outlet at the bottom end of the PVDP melting kettle (8) is communicated with the feed inlet (902, and a discharge hole at the other side wall end of the hollow wire drawing grinding tool (9) is communicated with a discharge hole of the cooling box (10) through a crawler belt.
2. The preparation device of the covalent organic framework composite membrane according to claim 1, wherein the hollow wire-drawing grinding tool (9) comprises a feeding crawler, a spraying port and a hollow wire-drawing device, one end of the feeding crawler is connected with a feeding port (902) at one side wall end of the hollow wire-drawing grinding tool, the other end of the feeding crawler is connected with the hollow wire-drawing device, and the spraying port is arranged above the feeding crawler and is communicated with a feeding port (901) at the top end of the hollow wire-drawing grinding tool.
3. The preparation device of the covalent organic framework composite membrane according to claim 1, wherein the hollow wire-drawing grinding tool (9) comprises a temperature sensor (903), a temperature control device and a display interface, the temperature sensor (903) is arranged on the side wall of the inner cavity of the hollow wire-drawing grinding tool (9), the output end of the temperature sensor (903) is connected with the temperature control device, the temperature control device is electrically connected with the display interface, and the display interface is arranged on the outer wall of the hollow wire-drawing grinding tool (9).
4. The apparatus for preparing covalent organic framework composite membrane according to claim 1, wherein the cooling tank (10) is provided with a filter membrane conveying crawler belt, and at least one cooling spray device is arranged above the filter membrane conveying crawler belt.
5. The apparatus for preparing covalent organic framework composite membrane according to claim 4, wherein the filter membrane transmission track is provided with a vibration device.
6. The apparatus for preparing a covalent organic framework composite membrane according to claim 1, further comprising a waste liquid treatment tank (11); and a waste liquid port of the washing dryer (6) is communicated with a feeding port of the waste liquid treatment pool (11).
7. The apparatus for preparing covalent organic framework composite membrane according to claim 1, wherein a temperature controller and a pressure controller are arranged in the reaction kettle (4) and the PVDP melting kettle (8).
8. The apparatus for preparing covalent organic framework composite membrane according to claim 1, wherein stirring devices are arranged in the reaction kettle (4), the activation kettle (7) and the PVDP melting kettle (8).
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| CN202021785844.9U CN213253867U (en) | 2020-08-24 | 2020-08-24 | Preparation facilities of covalence organic frame complex film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114497724A (en) * | 2022-01-20 | 2022-05-13 | 苏州大学张家港工业技术研究院 | Solid electrolyte and preparation method and application thereof |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114497724A (en) * | 2022-01-20 | 2022-05-13 | 苏州大学张家港工业技术研究院 | Solid electrolyte and preparation method and application thereof |
| CN114497724B (en) * | 2022-01-20 | 2023-05-23 | 苏州大学张家港工业技术研究院 | Solid electrolyte and preparation method and application thereof |
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