CN213611314U - Reaction device of covalent organic framework composite material based on photoinitiation - Google Patents
Reaction device of covalent organic framework composite material based on photoinitiation Download PDFInfo
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- CN213611314U CN213611314U CN202022338655.3U CN202022338655U CN213611314U CN 213611314 U CN213611314 U CN 213611314U CN 202022338655 U CN202022338655 U CN 202022338655U CN 213611314 U CN213611314 U CN 213611314U
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Abstract
The utility model provides a reaction device of covalent organic framework composite material based on photoinitiation, which comprises a covalent organic framework reaction unit, a photoinitiator storage tank, an organic polymerization monomer storage tank and a photochemical reactor communicated with the covalent organic framework reaction unit, the photoinitiator storage tank and the organic polymerization monomer storage tank; wherein, photochemical reactor includes the inner chamber, sets up in the inner chamber including base, LED light band pipe and spiral reaction channel, and at least one LED light band pipe sets up on the base, and spiral reaction channel is even spiral arrangement along LED light band pipe outer wall, and spiral reaction channel one end communicates with photochemical reactor's pan feeding mouth, and the other end communicates photochemical reactor's discharge gate. The device can prepare the covalent organic framework composite material by adding the photoinitiator and the organic polymerization monomer to carry out continuous reaction under the LED illumination condition in the synthesis process of the covalent organic framework composite material.
Description
Technical Field
The utility model belongs to covalence organic frame combined material preparation facilities field, concretely relates to covalence organic frame combined material's reaction unit based on photoinitiation.
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.
It is now shown in the prior art that photoinitiated polymerization, as a polymerization means distinguished from thermally initiated polymerization, has many advantages and practicality due to the controllability of light intensity and wavelength. The wide application of the high-efficiency photoinitiation system in the fields of holographic recording, laser direct plate making, photocuring, laser stereolithography and the like has been receiving wide attention. In recent years, the formation of covalent organic composites by the complex reaction of photoinitiators and covalent organic materials has become a focus of research, wherein the use of Light Emitting Diodes (LEDs) as new light sources is attracting more and more attention. Compared with the traditional existing lamp, the LED has better light output, higher working efficiency and lower cost, and shows huge application potential. Therefore, a reaction device based on photoinitiated covalent organic framework composite materials is provided, and the preparation of the covalent organic framework composite materials on a large scale through LED illumination reaction is necessary.
SUMMERY OF THE UTILITY MODEL
To the above defect or the improvement demand of prior art, the utility model provides a covalence organic frame combined material's reaction unit based on light initiation, this device carries out continuous reaction under LED illumination condition through adding photoinitiator and organic polymerization monomer in covalence organic frame combined material's the synthetic process, uses this device can prepare out covalence organic frame combined material.
In order to achieve the above object, according to the present invention, a photo-initiation-based covalent organic framework composite material reaction device is provided, which comprises a covalent organic framework reaction unit, a photo-initiation agent storage tank, an organic polymerization monomer storage tank, and a photochemical reactor communicated with the covalent organic framework reaction unit, the photo-initiation agent storage tank, the organic polymerization monomer storage tank, and the photochemical reactor;
the covalent organic framework reaction unit comprises a first ligand storage tank, a second ligand storage tank, a mixing reactor, a scrubber and a reaction collector which are connected with each other; the discharge ports of the first ligand storage tank and the second ligand storage tank are respectively communicated with a feed inlet at the top end of the mixing reactor, the discharge port at the bottom end of the mixing reactor is communicated with a feed inlet of a washer, and the discharge port at the bottom end of the washer is communicated with a feed inlet of a reaction collector; the discharge port pipeline of the reaction collector is converged and communicated with the discharge port pipelines of the photoinitiator storage tank and the organic polymerization monomer storage tank and is communicated with the feed port of the photochemical reactor;
the photochemical reactor comprises an inner cavity, the inner cavity is internally provided with a base, an LED light band tube and a spiral reaction channel, at least one LED light band tube is arranged on the base, the spiral reaction channel is arranged along the outer wall of the LED light band tube in an even spiral manner, one end of the spiral reaction channel is communicated with a feeding port of the photochemical reactor, and the other end of the spiral reaction channel is communicated with a discharging port of the photochemical reactor.
Preferably, the photochemical reactor comprises a low-temperature control device, and the low-temperature control device is arranged on the outer wall of the photochemical reactor.
Preferably, the low-temperature control device is provided with two interfaces communicated with the outside for inputting/outputting cooling fluid.
Preferably, the photochemical reactor further comprises a temperature sensing device, and the temperature sensing device is arranged in the inner cavity of the photochemical reactor.
Preferably, the photochemical reactor is provided with one LED light band tube in the inner cavity.
Preferably, the LED light strip tube comprises a light strip tube housing and an LED light strip.
Preferably, the discharge port of the photochemical reactor is connected with a washing dryer, and the washing dryer is used for washing and drying the compounded product and then outputting the product.
Preferably, the scrubber and the scrubbing dryer are both provided with liquid outlets connected with a first waste liquid treatment pool, and a waste liquid outlet of the first waste liquid treatment pool is communicated with a water inlet of a second waste liquid treatment pool.
Preferably, flow control valves are arranged on discharge port pipelines of the reaction collector, the photoinitiator storage tank and the organic polymerization monomer storage tank.
Preferably, a stirring device is arranged in the mixing reactor.
Generally, through the utility model discloses above technical scheme who conceives compares with prior art, can gain following beneficial effect:
(one) the utility model provides a reaction unit based on covalently organic frame combined material of photoinitiation is provided with the photochemical reactor at synthetic in-process, mixes covalently organic frame material, photoinitiator and the organic polymeric ligand of collecting in the photochemical reactor and forms covalently organic frame combined material through continuous reaction under LED illumination condition with the three.
(II) the utility model provides a reaction unit based on organic frame combined material of covalence of photoinitiation is provided with the spiral reaction pipeline in the photochemical reactor, and organic frame combined material of covalence, photoinitiator and organic polymeric ligand mix under the illumination condition in the spiral reaction pipeline and pass through continuous reaction.
(III) the utility model provides a reaction unit of covalence organic frame combined material based on photoinitiation can be suitable for the scale production of covalence organic frame combined material. The systematic device replaces manual experiment operation, so that the workload is reduced, and the process is more automatic.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a photo-initiated covalent organic framework composite-based reaction apparatus, implemented in accordance with the present invention;
FIG. 2 is a detailed schematic diagram of a photochemical reactor of a photo-initiated covalent organic framework composite based reaction apparatus, implemented in accordance with 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 ligand storage tank-1, a second ligand storage tank-2, a mixing reactor-3, a washer-4, a reaction collector-5, a photoinitiator storage tank-6, an organic polymerization monomer storage tank-7, a photochemical reactor-8, a washing dryer-9, a first waste liquid treatment tank-10, a second waste liquid treatment tank-11, an inner cavity-801, a base-802, an LED light band tube-803, a spiral reaction channel-804, a low-temperature control device-805 and a temperature sensing device-806.
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 specific embodiment of the present invention, there is provided a reaction apparatus for preparing a covalent organic framework composite material based on photoinitiation, comprising a photochemical reactor, wherein the synthesis process comprises: firstly, preparing a covalent organic framework material, and collecting the covalent organic framework material after washing; then mixing the collected covalent organic framework material, the photoinitiator and the organic polymeric ligand in a photochemical reactor and forming the covalent organic framework composite material through continuous reaction under the condition of LED illumination; and washing and drying the covalent organic framework composite material to finally form the covalent organic framework composite material.
In this embodiment, a photo-initiation-based reaction apparatus for covalent organic framework composite materials includes a covalent organic framework reaction unit, a photo-initiation storage tank 6, an organic polymerization monomer storage tank 7, and a photochemical reactor 8 communicated with the above three;
further, the covalent organic framework reaction unit comprises a first ligand storage tank 1, a second ligand storage tank 2, a mixing reactor 3, a scrubber 4 and a reaction collector 5 which are connected with each other; the discharge ports of the first ligand storage tank 1 and the second ligand storage tank 2 are respectively communicated with the feed port at the top end of the mixing reactor 3, the discharge port at the bottom end of the mixing reactor 3 is communicated with the feed port of the washer 4, and the discharge port at the bottom end of the washer 4 is communicated with the feed port of the reaction collector 5; a discharge port pipeline of the reaction collector 5 is converged and communicated with a discharge port pipeline of the photoinitiator storage tank 6 and the organic polymerization monomer storage tank 7 and is communicated with a feed port of the photochemical reactor 8;
furthermore, the first ligand storage tank 1 and the second ligand storage tank 2 are respectively used for storing and preparing two ligand solutions. Wherein the first ligand includes at least one of trimesic aldehyde, terephthalaldehyde, tetra (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, 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, the discharge ports of the first ligand storage tank 1 and the second ligand storage tank 2 are respectively communicated with the feed port at the top end of the mixing reactor 3, and the two ligands are subjected to mixing reaction in the mixing reactor 3 to form a covalent organic framework. A stirring device is arranged in the mixing reactor 3.
Furthermore, the reaction process also comprises a solvent, and the solvent participating in the reaction comprises: methanol, ethanol, N-dimethylformamide solution, dichloromethane, dimethylsulfoxide, and the like, without being limited thereto. The solvent can dissolve the first ligand and the second ligand through the first ligand storage tank 1 and the second ligand storage tank 2 and flow into the mixing reactor 3, or flow in through a feeding port on the side wall of the mixing reactor 3.
Furthermore, a discharge port at the bottom end of the mixing reactor 3 is communicated with a feed port of the scrubber 4, a discharge port at the bottom end of the scrubber 4 is communicated with a feed port of the reaction collector 5, and the generated covalent organic framework material is collected by the reaction collector 5 after being washed.
In this embodiment, as shown in fig. 2, the photochemical reactor 8 includes an inner cavity 801, the inner cavity 801 includes a base 802, LED light strip tubes 803 and a spiral reaction channel 804, at least one LED light strip tube 803 is disposed on the base 802, the spiral reaction channel 804 is uniformly and spirally arranged along the outer wall of the LED light strip tube 803, one end of the spiral reaction channel 804 is communicated with a feeding port of the photochemical reactor 8, and the other end is communicated with a discharging port of the photochemical reactor 8.
Furthermore, the collected covalent organic framework material, the photoinitiator and the organic polymeric ligand are mixed in a photochemical reactor and continuously reacted under the condition of LED illumination to form the covalent organic framework composite material, and the three raw materials are input into the photochemical reactor 9 according to a certain proportion and can be mixed in advance in a feeding pipeline. The photoinitiator includes at least one of 2,4, 6-trimethyl benzoyl phosphonic acid ethyl ester, 2-methyl-1- [ 4-methylthiophenyl ] -2-morpholinyl-1-acetone, 2-isopropyl thioxanthone, 4-dimethylamino-ethyl benzoate, 1-hydroxy-cyclohexyl-phenyl ketone and the like, but is not limited thereto; the organic polymeric ligand includes [1,3, 5-trimethyl-2, 4, 6-tris (4 '-formylphenyl) ] benzene, 1, 1-diphenyl-2, 2-bis (4-formylphenyl) ethylene, 1, 2-bis (4' -formylphenyl) acetylene, 1,3, 5-tris (4 '-formyl [1,1' -biphenyl ] -4-yl) benzene, 1, 4-bis (4-formylphenyl) benzene, 1, 4-naphthalenedicarboxaldehyde, 1, 4-bis (4-aminophenoxy) benzene, 1, 6-bis (4-formylphenyl) -3, 8-bis (4-aminophenyl) pyrene, 2, 3-dihydroxynaphthalene-1, 4-diformyl, 2,4, 6-tris (4-formylphenoxy) -1,3, 5-triazine, 2,4, 6-trimethylbenzene-1, 3, 5-trimethylacyl, 2, 5-diheptyloxy-1, 4-terephthalaldehyde, 2',5' -dimethoxy- [1,1':4',1 "-triphenyl ] -4, 4" -dicarboxaldehyde, 2, 5-dichloroterephthalaldehyde, 2, 5-dialdimidine, 2, 5-dipentyloxy-1, 4-terephthalaldehyde, 2, 5-dibromobenzene-1, 4-dicarboxaldehyde, 2-fluoro-4-carboxalylbenzeneboronic acid, 2-hydroxy-1, 3, 5-benzenetricarboxylic acid, 2-hydroxy-5-methyl-1, 3-benzenedicarboxaldehyde, 2-hydroxyisophthalaldehyde, 3-formyl-4-hydroxybenzonitrile, 3-thiophen-3-ylphenylformaldehyde, 4,4- (cyclopenta-1-en-1, 2-ylidene) bis (5-methylthiophene-2-carbaldehyde), 4 '", 4" ", 4" "-methanetetraalkyltriamine (4-hydroxy- [1,1' -biphenyl ] -3-carbaldehyde), 4,4 '-dicarbaldehyde, 4,4' -oxydiphenylformaldehyde, 4, 7-bis (4-formylphenylethynyl) benzo [ c ] [1,2,5] thiadiazole, 4-hydroxyisophthalaldehyde, 4-ethynylbenzaldehyde, 5- ((4-formylphenyl) ethynyl) isophthalaldehyde, 5,5' - ((5' - (4- ((3- (tert-butyl) -5-formyl-4-hydroxyphenyl) ethynyl) phenyl) - [1,1': 3', 1 "-triphenyl ] -4, 4" -diyl) bis (acetylene-2, 1-diyl)) bis (3- (tert-butyl) -2-hydroxyphenylformaldehyde), 5,5' - (acetylene-1, 2-diyl) isophthalaldehyde, 5-o-vanillin, 5-hydroxyisophthalaldehyde, 5-vinyl-2-hydroxyphenylformaldehyde, pyridine-2, 6-dicarboxaldehyde, imidazole-2-carbaldehyde, tris (4-aldehydiphenyl) amine, tris (4-aldehydiphenyl) trisphenol, tetrakis (4-aldehydiphenyl) ethylene and the like, but is not limited thereto.
In the present embodiment, the photochemical reactor 8 includes a low-temperature control device 805, and the low-temperature control device 805 is disposed on an outer wall of the photochemical reactor 8.
Further, since the covalent organic framework material, the photoinitiator and the organic polymeric monomer react under the illumination and low temperature conditions, a corresponding low temperature control device 805 needs to be provided to ensure that the temperature in the photochemical reactor 9 is kept constant for a certain period of time. The reaction temperature is controlled between 45 and 150 ℃.
Further, the low temperature control device 805 is provided with two ports for communication with the outside for input/output of cooling fluid. The cooling fluid enters at the interface at the upper portion of the cryogenic control device 805 and exits at the interface at the lower portion of the cryogenic control device 805. The cooling fluid is preferably water.
Further, the photochemical reactor 8 further comprises a temperature sensing device 806, and the temperature sensing device 806 is disposed in the inner cavity 801 of the photochemical reactor 8. The apparatus further comprises a temperature control device, wherein the temperature sensing device 806 senses the temperature of the composite reaction and feeds the temperature back to the temperature control device, and the temperature control device controls the flow rate of the cooling fluid in the low temperature control device 805 according to the real-time temperature.
Further, the inner cavity of the photochemical reactor 8 is provided with 3-7 LED light band tubes 803. More preferably 5 LED light strip tubes 803. The LED light band tubes 803 are provided with spiral reaction channels 804, and the spiral reaction channels 804 on each LED light band tube 803 are connected in sequence and used for continuous reaction under the illumination condition.
In this embodiment, the discharge port of the photochemical reactor 8 is connected to the washing dryer 9, and the washing dryer 9 washes and dries the composite product and outputs the product. The washing dryer 9 is used for washing and drying the final product, and comprises a drying cavity and a filtrate cavity, and a filter membrane transmission device is arranged in the middle of the drying cavity and can transmit the washed and filtered product out from a discharge hole.
Further, the washer 4 and the washing dryer 9 are both provided with liquid outlets connected with the first waste liquid treatment tank 10, and a waste liquid outlet of the first waste liquid treatment tank 10 is communicated with a water inlet of the second waste liquid treatment tank 11. The first waste liquid treatment tank 10 is used for primary waste liquid treatment, and the second waste liquid treatment tank 11 is used for secondary waste liquid treatment.
In this embodiment, all the reaction apparatuses are made of a high-temperature-resistant and corrosion-resistant material, and stirring apparatuses are provided in the mixing reactor 3, the first waste liquid treatment tank 10, and the second waste liquid treatment tank 11, and are used for mixing reaction raw materials in the product reaction or waste liquid treatment.
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 (10)
1. The reaction device based on the covalent organic framework composite material initiated by light is characterized by comprising a covalent organic framework reaction unit, a photoinitiator storage tank (6), an organic polymerization monomer storage tank (7) and a photochemical reactor (8) communicated with the covalent organic framework reaction unit, the photoinitiator storage tank and the organic polymerization monomer storage tank;
the covalent organic framework reaction unit comprises a first ligand storage tank (1), a second ligand storage tank (2), a mixing reactor (3), a scrubber (4) and a reaction collector (5) which are connected with each other; the discharge ports of the first ligand storage tank (1) and the second ligand storage tank (2) are respectively communicated with a feed inlet at the top end of the mixing reactor (3), the discharge port at the bottom end of the mixing reactor (3) is communicated with a feed inlet of the scrubber (4), and the discharge port at the bottom end of the scrubber (4) is communicated with a feed inlet of the reaction collector (5); a discharge port pipeline of the reaction collector (5) is converged and communicated with a discharge port pipeline of the photoinitiator storage tank (6) and the organic polymerization monomer storage tank (7), and is communicated with a feed port of the photochemical reactor (8);
photochemical reactor (8) include inner chamber (801), set up in inner chamber (801) including base (802), LED light band pipe (803) and spiral reaction channel (804), at least one LED light band pipe (803) set up in on base (802), spiral reaction channel (804) are followed LED light band pipe (803) outer wall is even spiral and arranges, spiral reaction channel (804) one end with the pan feeding mouth intercommunication of photochemical reactor (8), the other end intercommunication the discharge gate of photochemical reactor (8).
2. The photo-initiated covalent organic framework composite-based reaction device according to claim 1, characterized in that the photochemical reactor (8) comprises a low-temperature control device (805), the low-temperature control device (805) being arranged at an outer wall of the photochemical reactor (8).
3. The photo-initiated covalent organic framework composite-based reaction device according to claim 2, characterized in that the low temperature control device (805) is provided with two interfaces to the outside for input/output of cooling fluid.
4. The photo-initiated covalent organic framework composite-based reaction device according to claim 2, characterized in that the photochemical reactor (8) further comprises a temperature sensing device (806), the temperature sensing device (806) being arranged in the lumen (801) of the photochemical reactor (8).
5. The photoinitiated covalent organic framework composite-based reaction device of claim 1 wherein 3-7 LED light strip tubes (803) are disposed in the inner cavity of the photochemical reactor (8).
6. The photoinitiated covalent organic framework composite-based reaction device of claim 1 wherein the LED light strip tube (803) comprises a light strip tube housing and an LED light strip.
7. The photo-induced covalent organic framework composite-based reaction device according to claim 1, wherein the discharge port of the photochemical reactor (8) is connected to a washing dryer (9), and the washing dryer (9) is used for washing and drying the compounded product and outputting the washed and dried product.
8. The photo-initiated covalent organic framework composite-based reaction device according to claim 1, wherein the scrubber (4) and the scrubber dryer (9) are both provided with liquid outlets connected to a first waste liquid treatment tank (10), and the waste liquid outlet of the first waste liquid treatment tank (10) is communicated with the water inlet of a second waste liquid treatment tank (11).
9. The photo-initiation based covalent organic framework composite reaction apparatus of claim 1, wherein the reaction collector (5), the photo-initiator storage tank (6) and the organic polymer monomer storage tank (7) are provided with flow control valves on the outlet pipelines.
10. Photo-initiated covalent organic framework composite-based reaction device according to claim 1, characterized in that a stirring device is provided inside the mixing reactor (3).
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| CN113501921A (en) * | 2021-08-03 | 2021-10-15 | 齐齐哈尔大学 | Covalent organic framework material and preparation method and application thereof |
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| CN113501921A (en) * | 2021-08-03 | 2021-10-15 | 齐齐哈尔大学 | Covalent organic framework material and preparation method and application thereof |
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