CN109758995B - Universal fluorescent fluid photochemical microreactor part and 3D printing manufacturing method thereof - Google Patents
Universal fluorescent fluid photochemical microreactor part and 3D printing manufacturing method thereof Download PDFInfo
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- CN109758995B CN109758995B CN201910161945.4A CN201910161945A CN109758995B CN 109758995 B CN109758995 B CN 109758995B CN 201910161945 A CN201910161945 A CN 201910161945A CN 109758995 B CN109758995 B CN 109758995B
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000007639 printing Methods 0.000 claims description 12
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000002096 quantum dot Substances 0.000 claims description 3
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 claims description 2
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- OURODNXVJUWPMZ-UHFFFAOYSA-N 1,2-diphenylanthracene Chemical compound C1=CC=CC=C1C1=CC=C(C=C2C(C=CC=C2)=C2)C2=C1C1=CC=CC=C1 OURODNXVJUWPMZ-UHFFFAOYSA-N 0.000 description 3
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- ORFSSYGWXNGVFB-UHFFFAOYSA-N sodium 4-amino-6-[[4-[4-[(8-amino-1-hydroxy-5,7-disulfonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-5-hydroxynaphthalene-1,3-disulfonic acid Chemical compound COC1=C(C=CC(=C1)C2=CC(=C(C=C2)N=NC3=C(C4=C(C=C3)C(=CC(=C4N)S(=O)(=O)O)S(=O)(=O)O)O)OC)N=NC5=C(C6=C(C=C5)C(=CC(=C6N)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] ORFSSYGWXNGVFB-UHFFFAOYSA-N 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
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Abstract
A universal fluorescent fluid photochemical microreactor part and a 3D printing manufacturing method thereof belong to the technical field of photochemical reactor research. The photochemical microreactor part with a light collecting channel and a reaction channel is prepared by utilizing the transparent photosensitive resin and the strong space construction capability of 3D printing. Light-collecting substances are introduced into the optical channel in a fluid form, so that the effects of light collection and wavelength conversion can be achieved, the problem of light source matching of the traditional photochemical reactor is solved, the light-collecting substances can be flexibly replaced to meet the requirements of different photochemical reactions in the reaction channel, and the application range of the reactor is greatly expanded. The photochemical microreactor is simple and rapid to manufacture, can be produced in a large scale, and provides convenience for researching rapid screening of reaction, optimization of reaction conditions, reaction mechanism and the like. The used light collecting material can be recycled, the material cost is reduced, and the environment is not polluted.
Description
Technical Field
The invention belongs to the technical field of photochemical reactor research, and relates to a 3D printing fluorescent fluid photochemical microreactor. In particular to a method for manufacturing a micro-reactor which has a wavelength conversion function and can be applied to different photochemical reactions by using transparent light-cured resin 3D printing.
Background
The photochemical reaction refers to a chemical reaction process which occurs under the irradiation of an external light source. The photochemical reactor is used as a site for photochemical reaction, and the performance of the photochemical reactor is very important for the photochemical reaction. The type of light source in the photochemical reactor, the geometry of the reactor and the mutual position between the reactor and the light source are key factors that directly affect the performance of the photochemical reactor. In recent years, micro-reactors have attracted much attention because mass transfer and heat transfer processes of reaction systems are greatly improved, and higher conversion rate and yield can be obtained in chemical reaction processes. Microreactors generally refer to microstructured chemical reactors having internal fluidic channels or dispersion space dimensions on the order of micrometers. The photochemical microreactor is prepared by combining the light-transmitting microreactor with an external irradiation light source, so that the conversion rate and selectivity of photochemical reaction can be effectively improved. However, in the photochemical reaction, because of the restriction of the fundamental principle of quantum mechanics, whether the reaction is performed or not is directly related to the wavelength of the external irradiation light source (especially visible light excited chemical reaction), so different irradiation light sources are often required for different photochemical reactions. In reality, some light sources with special wavelengths are difficult to obtain or expensive, which greatly limits the application of photochemical microreactors.
Fluorescent dyes and quantum dots tend to have broader absorption bands and narrower emission bands. These materials can collect excitation light with different wavelengths to generate emission light with a strong wavelength, thereby performing the functions of light collection and wavelength conversion. By utilizing the characteristic, people can utilize cheap LED light sources, even sunlight and other broad-spectrum light sources to initiate photochemical reaction. At present, a fluorescence light-collecting micro-reactor is widely applied, namely, a fluorescent material is dispersed into a transparent medium, then a micro-channel is constructed in the micro-reactor by adopting a die-turning method, and the micro-reactor is formed after solidification. In the reactor, the fluorescent material absorbs light from an external light source and emits fluorescent light of a desired wavelength. The emitted fluorescence is transmitted in a transparent medium in a mode of an optical waveguide and is focused to the built-in micro-channel, so that the photochemical reaction in the micro-channel is promoted. The reactor well solves the problem of wavelength matching in the photochemical reaction process. However, such reactors suffer from several problems: firstly, since the fluorescent dye is doped into the substrate of the reactor at the beginning and cannot be separated, the reactor is only suitable for a specific photoreaction; secondly, the replacement and recycling of the fluorescent dye are difficult to realize; finally, the process of preparing the reactor by adopting the rollover method is complicated, takes long time and is difficult to design a more complex spatial structure. These factors lead to high manufacturing cost and low universality of the fluorescent light-collecting photochemical microreactor, and the application range is greatly limited. Therefore, it is very important to develop a light-collecting photochemical microreactor which is simple to prepare and can be used for various photochemical reactions.
The fluorescent material is fixed and can not be replaced due to the fact that the fluorescent material enters the medium of the reactor in a doping mode, and if the fluorescent material is introduced into the micro-reactor in a fluid mode, the problem is hopeful to be solved. The 3D printing is an emerging additive manufacturing technology, an object with a complex space structure can be constructed in a layer-by-layer printing mode, and the rapid prototyping characteristic is achieved. By means of the powerful space construction capability of the 3D printing technology, the continuous flow photochemical microreactor with the light collecting channel and the reactant channel can be processed and manufactured to form a replaceable general photochemical microreactor part made of fluorescent materials.
Disclosure of Invention
The invention aims to provide a method for preparing a universal fluorescent fluid photochemical microreactor by combining a 3D printing technology with a fluorescent material.
The technical scheme of the invention is as follows:
a universal fluorescent fluid photochemical microreactor part comprises an optical channel 2, a reaction channel 1, an optical channel outlet, an optical channel inlet, a reaction channel outlet and a reaction channel inlet; the light channel 2 is filled with fluorescent fluid, and two ports are sealed; reaction liquid is introduced into the reaction channel 1, and the optical channel 2 is positioned around the reaction channel 1 to ensure the photochemical reaction.
The reaction channel 1 and the optical channel 2 are both snakelike square tubes, and the optical channel 2 is provided with two sets which are respectively arranged on the upper side and the lower side of the reaction channel 1 in parallel.
The reaction channel 1 is a linear square tube, and the optical channel 2 is a spiral circular tube and is wound on the periphery of the reaction channel 1.
The universal fluorescent fluid photochemical microreactor is made of transparent photosensitive resin 3.
The fluorescent material in the fluorescent fluid is fluorescent dye, fluorescent quantum dots or nano-crystals, and the solvent is water, ethanol, isopropanol, acetonitrile, ethyl acetate, DMF, toluene or dichloromethane.
A3D printing manufacturing method of a universal fluorescent fluid photochemical microreactor part comprises the following steps:
(1) a model of a micro-reactor is designed by using Solidworks software, a 3D printer is used for printing, the characteristic size (namely the pipe diameter or the section side length) of an optical channel 2 and a reaction channel 1 is 0.5-1mm, and the material is transparent photosensitive resin 3.
(2) And printing the micro-reactor part by using an ultraviolet curing 3D printer.
(3) And (3) cleaning the microreactor part by using a mixed solution of ethanol and isopropanol, ensuring that no resin residue exists in the channel, and then curing for 2-10 hours under an ultraviolet lamp.
(4) The fluorescent material is dissolved in a solvent at a concentration of 0.1 to 1000ppm, and then injected into the light tunnel 2 using a syringe, and both ends of the light tunnel 2 are sealed. Then preparing the universal fluorescent fluid photochemical microreactor part.
The layer printing precision of the 3D printer is 0.025-0.1 mm.
The invention has the beneficial effects that: the invention adopts the 3D printing technology to prepare the universal photochemical microreactor and provides a simple and efficient equipment device for the research of photochemical reaction. First, the photochemical micro-reactor is very simple and convenient to manufacture and low in cost. And secondly, the fluorescent dye enters the optical channel in a fluid form, can be conveniently recycled after reaction, avoids the waste and environmental pollution of fluorescent materials, and saves the cost. And the types of fluorescent materials in the optical channel can be flexibly changed according to the requirements of different reactions in the reaction channel on the optical wavelength, so that the types of chemical reactions in the reactor are greatly widened, and the universality is stronger.
Drawings
FIG. 1 is a schematic diagram of a serpentine fluorescent fluid photochemical microreactor.
FIG. 2 is a schematic diagram of a spiral fluorescent fluidic photochemical microreactor.
In the figure: 1 a reaction channel; 2, an optical channel; 3 a transparent photosensitive resin.
Detailed Description
The invention is further described in detail below with reference to the drawings and technical solutions.
A method for preparing a universal fluorescent fluid photochemical microreactor by using a 3D printing technology comprises the following specific steps:
example 1 (Serpentine microreactor)
(1) A microreactor model is designed by using SolidWorks software, an optical microchannel and a reaction microchannel are both snakelike square tubes, the side length of each pipeline is 1mm, the length of each channel is 105mm, and the overall dimension of a reactor is 8.2cm in length, 3cm in width and 1.5cm in height.
(2) And printing the microreactor by using an ultraviolet curing 3D printer, wherein the microreactor is made of transparent photosensitive resin.
(3) After printing, the reactor is taken down from the working platform and is put into mixed solution of ethanol and isopropanol for cleaning, and particularly, the inside of the microchannel is cleaned by paying attention to ensure that no resin residue exists. Then placed under an ultraviolet lamp for curing for 4 h.
(4) The fluorescent dye Lumogen F Red 305 was dissolved in an ethanol solution at a concentration of 200ppm and injected into the light tunnel using a syringe.
(5) And placing the fluorescent fluid photochemical microreactor part in a cylindrical shading cylinder internally wound with a blue light LED lamp strip to form a final photochemical reaction device. For the catalytic oxidation of reaction diphenyl anthracene, reactant diphenyl anthracene and photocatalyst methylene blue can be respectively injected into a reaction channel, and the oxidation conversion rate of diphenyl anthracene is 3 times of that under pure blue light under the action of fluorescent fluid.
Example 2 (spiral microreactor)
(1) The microreactor model was designed using SolidWorks software. The optical micro-channel is a spiral circular tube, the diameter of the tube is 1mm, and the length of the channel is 105 mm. The reaction channel is a linear square tube, the side length of the pipeline is 1 code, and the length of the channel is 56 mm. The overall size of the reactor was 7cm in length, 3.5cm in width and 1.5cm in height.
(2) And printing the microreactor by using an ultraviolet curing 3D printer, wherein the microreactor is made of transparent photosensitive resin.
(3) After printing, the reactor is taken down from the working platform and is put into mixed solution of ethanol and isopropanol for cleaning, and particularly, the inside of the microchannel is cleaned by paying attention to ensure that no resin residue exists. Then placed under an ultraviolet lamp for curing for 4 h.
(4) The fluorescent dye Fluorescein Isothiocyanate (FITC) was dissolved in an ethanol solution at a concentration of 400ppm and injected into the optical channel using a syringe.
(5) And placing the fluorescent fluid photochemical microreactor part in a cylindrical shading cylinder internally wound with a blue light LED lamp strip to form a final photochemical reaction device. For the oxidation of p-methylthiophenol, the reactants p-methylthiophenol and photocatalyst Zuhong Y can be respectively injected into the reaction channel, and the reaction conversion rate under the action of fluorescent fluid is 1.8 times that under the action of pure blue light.
Claims (5)
1. A3D printing manufacturing method of a universal fluorescent fluid photochemical microreactor part is characterized in that the microreactor part comprises an optical channel (2), a reaction channel (1), an optical channel outlet, an optical channel inlet, a reaction channel outlet and a reaction channel inlet; the interior of the optical channel (2) is filled with fluorescent fluid, and two ports are sealed; reaction liquid is introduced into the reaction channel (1), and the optical channel (2) is positioned around the reaction channel (1) to ensure the photochemical reaction;
the 3D printing manufacturing method comprises the following steps:
(1) designing a model of a micro-reactor by using Solidworks software, wherein the pipe diameters or the section side lengths of the optical channel (2) and the reaction channel (1) are 0.5-1mm, and the material is transparent photosensitive resin (3);
(2) printing a micro-reactor piece by using an ultraviolet curing 3D printer;
(3) cleaning the microreactor part by using a mixed solution of ethanol and isopropanol, ensuring that no resin residue exists in a channel, and then curing for 2-10 hours under an ultraviolet lamp;
(4) dissolving the fluorescent material in a solvent to the concentration of 0.1-1000ppm, then injecting the fluorescent material into the light channel (2) by using a syringe, and sealing two ends of the light channel (2); then preparing the universal fluorescent fluid photochemical microreactor part.
2. The 3D printing manufacturing method of the universal type fluorescent fluid photochemical microreactor part according to claim 1, wherein the reaction channel (1) and the optical channel (2) are both S-shaped square tubes, and the optical channels (2) are arranged in two sets and are respectively arranged on the upper side and the lower side of the reaction channel (1) in parallel.
3. The 3D printing manufacturing method of the universal type fluorescent fluid photochemical microreactor part according to claim 1, wherein the reaction channel (1) is a linear square tube, and the optical channel (2) is a spiral circular tube wound around the periphery of the reaction channel (1).
4. The 3D printing method for manufacturing a universal fluorescent fluid photochemical microreactor component as claimed in claim 1, 2 or 3, wherein the fluorescent material in the fluorescent fluid is a fluorescent dye, a fluorescent quantum dot or a nanocrystal, and the solvent is water, ethanol, isopropanol, acetonitrile, ethyl acetate, DMF, toluene or dichloromethane.
5. The 3D printing manufacturing method of the universal fluorescent fluid photochemical microreactor part according to claim 1, wherein the 3D printer selects a layer printing precision of 0.025-0.1 mm.
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| CN110813211A (en) * | 2019-12-03 | 2020-02-21 | 广东省新材料研究所 | Micro-reactor and manufacturing method thereof |
| CN111266069B (en) * | 2020-01-17 | 2022-03-25 | 山东清创化工有限公司 | Photochemical synthesis system and method with customizable light source |
| CN115974554A (en) * | 2022-12-07 | 2023-04-18 | 之江实验室 | Transparent ceramic microreactor based on 3D printing integrated molding and preparation method thereof |
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| JP5349930B2 (en) * | 2008-12-04 | 2013-11-20 | 三井造船株式会社 | Method for oxidizing toluene |
| CN104028188A (en) * | 2014-01-20 | 2014-09-10 | 南京工业大学 | Ultraviolet light micro-channel reactor |
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