CN109758995A - A kind of Universal fluorescence fluid photochemistry microreactor part and its 3D printing manufacturing method - Google Patents
A kind of Universal fluorescence fluid photochemistry microreactor part and its 3D printing manufacturing method Download PDFInfo
- Publication number
- CN109758995A CN109758995A CN201910161945.4A CN201910161945A CN109758995A CN 109758995 A CN109758995 A CN 109758995A CN 201910161945 A CN201910161945 A CN 201910161945A CN 109758995 A CN109758995 A CN 109758995A
- Authority
- CN
- China
- Prior art keywords
- photochemistry
- fluid
- channel
- microreactor
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A kind of Universal fluorescence fluid photochemistry microreactor part and its 3D printing manufacturing method, belong to photochemical reactor studying technological domain.Ability is constructed using the powerful space of transparent photosensitive resin and 3D printing, is prepared for the photochemistry microreactor part simultaneously with collection optical channel and reaction channel.Collection stimulative substance is introduced into optical channel with fluid form, both the effect of light harvesting and wavelength convert can have been played, solve the matched problem of traditional photochemical reactor light source, collection stimulative substance can be replaced flexibly again to meet different photochemically reactive demands in reaction channel, greatly extend the application range of reactor.Being simple to manufacture, quickly for photochemistry microreactor of the present invention, can be mass-produced, and provide convenience for quick screening, the optimization of reaction condition and the reaction mechanism etc. of research reaction.Solar collector material used is recyclable to be recycled, and reduces material cost, and free from environmental pollution.
Description
Technical field
The invention belongs to photochemical reactor studying technological domains, are related to the micro- reaction of 3D printing fluorescent fluid photochemistry
Device.More particularly to using transparent photo-cured resin 3D printing manufacture to have the function of wavelength convert, it is anti-to can be applied to different photochemistry
The method for the microreactor answered.
Background technique
Photochemical reaction refers to the chemical reaction process occurred under the irradiation of external light source.Photochemical reactor conduct
The place that photochemical reaction carries out, performance superiority and inferiority have highly important effect for photochemical reaction.In photochemical reactor
Mutual alignment is the pass for directly affecting photochemical reactor performance between light source type, reactor geometries and reactor and light source
Key factor.Nearly this year carrys out microreactor since the mass transfer and diabatic process of reaction system are greatly improved, and can make to chemically react
Process obtains higher conversion ratio and yield and receives significant attention.Microreactor typically refers to its internal fluid channels or dispersion
Micro-structure chemical reactor of the space scale in micron dimension.Light is prepared in conjunction with additional radiation source using light transmission microreactor
Chemical microreactor can effectively promote photochemically reactive conversion ratio and selectivity.However in photochemical reaction, due to
By the restriction of fundamental principles of quantum mechanics, whether the progress of reaction directly with the wavelength of extraneous radiation source it is related (especially
The chemical reaction of excited by visible light), therefore different radiation sources is generally required for different photochemical reactions.And reality
In, the light source of some special wavelengths is more difficult to get or expensive, this significantly limits the application of photochemistry microreactor.
Fluorescent dye and quantum dot often have wider absorption band and relatively narrow emission band.These substances can lead to
The a certain stronger transmitting light of wavelength of exciting light generation for collecting different wave length is crossed, to play the function of light harvesting and wavelength convert.
Using this feature, people can use the broad-spectrum light sources such as cheap LED light source even daylight to cause photochemical reaction.At present
Using it is more be that fluorescence light harvesting declines reactor, i.e., fluorescent material is distributed in transparent medium, then uses the side of overmolded
Method constructs microchannel inside it, forms microreactor after cured.In the reactor, fluorescent material absorbs the light of additional light source
And the fluorescence of wavelength needed for emitting.The fluorescence emitted can be in the mode in transparent medium with optical waveguide transmits and focuses on
The microchannel set, to promote the photochemically reactive progress in microchannel.This kind of reactor very good solution photochemistry is anti-
Wavelength matched problem during answering.But there are the following problems for this kind of reactor: firstly, since fluorescent dye is at the beginning
It is just doped in reactor matrix, can not separate, therefore this kind of reactor is only applicable to a certain specific light reaction；Secondly, glimmering
The replacement and recycling of photoinitiator dye are difficult to realize；Finally, many and diverse using overmolded method preparation reactor process, time-consuming, and difficult
To design more complicated space structure.These factors are to causing fluorescence light harvesting formula photochemistry microreactor manufacturing cost high, general
Adaptive is low, and application range is very restricted.Therefore develop it is a kind of prepare simple and a variety of photochemical reactions can be general
It is very important for light harvesting formula photochemistry microreactor.
Due to fluorescent material is entered in reactor media using doping way and causing it to be fixed cannot replace, if will
Fluorescent material is introduced into inside microreactor with fluid form, then is expected to solve the above problems.3D printing is a kind of emerging increasing
Material manufacturing technology can construct the object with Complicated Spatial Structure by layer-by-layer printing, and with rapid shaping
Feature.Ability is constructed by means of the powerful space of 3D printing technique, while there is the continuous flow of collection optical channel and reactant channel
Photochemistry microreactor can be processed manufacture, form the replaceable universal optical chemical microreactor part of fluorescent material.
Summary of the invention
Universal fluorescence fluid light is prepared using 3D printing technique combination fluorescent material the object of the present invention is to provide a kind of
The method of chemical microreactor.
Technical solution of the present invention:
A kind of Universal fluorescence fluid photochemistry microreactor part, including the outlet of optical channel 2, reaction channel 1, optical channel,
Optical channel entrance, reaction channel outlet and reaction channel entrance；Fluorescent fluid is full of inside the optical channel 2, two-port is close
Envelope；Reaction solution is passed through inside the reaction channel 1, optical channel 2 is located at around reaction channel 1, it is ensured that it is photochemically reactive into
Row.
The reaction channel 1 and optical channel 2 is snakelike square tube, and optical channel 2 is two sets, is arranged in parallel in reaction respectively
The two sides up and down in channel 1.
The reaction channel 1 is linear type square tube, and the optical channel 2 is spiral shape round tube, is wound in reaction channel 1
Periphery.
The material of the Universal fluorescence fluid photochemistry microreactor part is transparent photosensitive resin 3.
Fluorescent material in the fluorescent fluid is fluorescent dye, fluorescence quantum or nanocrystalline, and solvent is water, second
Alcohol, isopropanol, acetonitrile, ethyl acetate, DMF, toluene or methylene chloride.
A kind of 3D printing manufacturing method of Universal fluorescence fluid photochemistry microreactor part, steps are as follows:
(1) model for being gone out microreactor part using Solidworks software design, is printed, optical channel with 3D printer
2 and reaction channel 1 characteristic size (i.e. caliber or section side length) be 0.5-1mm, material be transparent photosensitive resin 3.
(2) microreactor part is printed using ultraviolet light solidification 3D printer.
(3) microreactor part is cleaned with ethyl alcohol and isopropanol mixed liquor, and ensures to be subsequently placed in channel without resin residue
Solidify 2-10 hours under ultraviolet lamp.
(4) fluorescent material is dissolved in solvent, concentration is then injected into light using syringe and leads in 0.1-1000ppm
In road 2, and 2 both ends of optical channel are tamping.Universal fluorescence fluid photochemistry microreactor part is then prepared.
The layer printing precision that the 3D printer is selected is 0.025-0.1mm.
Beneficial effects of the present invention: the present invention prepares universal optical chemical microreactor using 3D printing technique, is photochemical
The research for learning reaction provides the apparatus being simple and efficient.One, the production of the micro- anti-device of photochemistry is very easy, at low cost.Two,
Fluorescent dye enters optical channel with fluid form, can easily recycle after reaction, avoids waste and the ring of fluorescent material
Border pollution, save the cost.Three, the demand according to differential responses in reaction channel to optical wavelength can be replaced flexibly in optical channel
The type of fluorescent material, has widened the type of the chemical reaction occurred in reactor significantly, and universality is stronger.
Detailed description of the invention
Fig. 1 is the schematic diagram of snakelike fluorescent fluid photochemistry microreactor.
Fig. 2 is the schematic diagram of spiral shape fluorescent fluid photochemistry microreactor.
In figure: 1 reaction channel；2 optical channels；3 transparent photosensitive resins.
Specific embodiment
With reference to the accompanying drawing and technical solution, further the present invention is described in detail.
A method of Universal fluorescence fluid photochemistry microreactor being prepared using 3D printing technique, specific steps are such as
Under:
Embodiment 1 (snakelike microreactor)
(1) SolidWorks software design microreactor model is used, light microchannel and microchannel are snakelike side
Pipe, pipeline side length are long 8.2cm, wide 3cm, high 1.5cm having a size of 1mm, passage length 105mm, reactor overall dimensions.
(2) microreactor is printed using ultraviolet light solidification 3D printer, material is transparent photosensitive resin.
(3) print after the completion of, reactor is removed from workbench, be put into the mixed solution of ethyl alcohol and isopropanol into
Row cleaning especially pays attention to cleaning inside microchannels, guarantees without resin residue.It is subsequently placed to solidify 4h under ultraviolet lamp.
(4) fluorescent dye Lumogen F Red 305 is dissolved in ethanol solution, concentration 200ppm uses syringe
It is injected into optical channel.
(5) the fluorescent fluid photochemistry microreactor part is placed in the cylindrical cone of inner wrap blue LED lamp band
It is interior, form final photochemical reaction device.It, can be by reactant diphenylanthrancene and light for reacting the catalysis oxidation of diphenylanthrancene
Catalyst methylene blue is injected separately into reaction channel, and the conversion rate of oxidation of diphenylanthrancene is simple under the action of fluorescent fluid
3 times under blue light.
Embodiment 2 (spiral shape microreactor)
(1) SolidWorks software design microreactor model is used.Light microchannel is spiral shape round tube, pipe diameter
For 1mm, passage length 105mm.Reaction channel is linear type square tube, a length of 1 password of ducting side, passage length 56mm.Instead
Answering device overall dimensions is long 7cm, wide 3.5cm, high 1.5cm.
(2) microreactor is printed using ultraviolet light solidification 3D printer, material is transparent photosensitive resin.
(3) print after the completion of, reactor is removed from workbench, be put into the mixed solution of ethyl alcohol and isopropanol into
Row cleaning especially pays attention to cleaning inside microchannels, guarantees without resin residue.It is subsequently placed to solidify 4h under ultraviolet lamp.
(4) fluorescent dye fluorescein isothiocynate (FITC) is dissolved in ethanol solution, concentration 400ppm uses injection
Device is injected into optical channel.
(5) the fluorescent fluid photochemistry microreactor part is placed in the cylindrical cone of inner wrap blue LED lamp band
It is interior, form final photochemical reaction device.It, can be by reactant to methylbenzene phenyl-sulfhydrate for reacting the oxidation to methylbenzene phenyl-sulfhydrate
Red Y is affixed one's name to photochemical catalyst and is injected separately into reaction channel, and reaction conversion ratio is under simple blue light under the action of fluorescent fluid
1.8 again.
Claims (8)
1. a kind of Universal fluorescence fluid photochemistry microreactor part, which is characterized in that including optical channel (2), reaction channel
(1), optical channel outlet, the outlet of optical channel entrance, reaction channel and reaction channel entrance；It is full of inside the optical channel (2)
Fluorescent fluid, two-port sealing；It is passed through reaction solution inside the reaction channel (1), optical channel (2) is located at reaction channel (1)
Around, it is ensured that photochemically reactive progress.
2. a kind of Universal fluorescence fluid photochemistry microreactor part according to claim 1, which is characterized in that described
Reaction channel (1) and optical channel (2) are snakelike square tube, and optical channel (2) is two sets, are arranged in parallel in reaction channel (1) respectively
Two sides up and down.
3. a kind of Universal fluorescence fluid photochemistry microreactor part according to claim 1, which is characterized in that described
Reaction channel (1) is linear type square tube, and the optical channel (2) is spiral shape round tube, is wound in reaction channel (1) periphery.
4. a kind of Universal fluorescence fluid photochemistry microreactor part according to claim 1,2 or 3, which is characterized in that
The material of the Universal fluorescence fluid photochemistry microreactor part is transparent photosensitive resin (3).
5. a kind of Universal fluorescence fluid photochemistry microreactor part according to claim 1,2 or 3, which is characterized in that
Fluorescent material in the fluorescent fluid is fluorescent dye, fluorescence quantum or nanocrystalline, solvent be water, ethyl alcohol, isopropanol,
Acetonitrile, ethyl acetate, DMF, toluene or methylene chloride.
6. a kind of Universal fluorescence fluid photochemistry microreactor part according to claim 4, which is characterized in that described
Fluorescent material in fluorescent fluid is fluorescent dye, fluorescence quantum or nanocrystalline, solvent be water, ethyl alcohol, isopropanol, acetonitrile,
Ethyl acetate, DMF, toluene or methylene chloride.
7. a kind of 3D printing manufacturing method of Universal fluorescence fluid photochemistry microreactor part, which is characterized in that steps are as follows:
(1) model for being gone out microreactor part using Solidworks software design, is printed, optical channel (2) with 3D printer
Caliber or section side length with reaction channel (1) are 0.5-1mm, and material is transparent photosensitive resin (3)；
(2) microreactor part is printed using ultraviolet light solidification 3D printer；
(3) microreactor part is cleaned with ethyl alcohol and isopropanol mixed liquor, and ensures to be subsequently placed at ultraviolet in channel without resin residue
Solidify 2-10 hours under lamp；
(4) fluorescent material is dissolved in solvent, concentration is then injected into optical channel (2) using syringe in 0.1-1000ppm
In, and optical channel (2) both ends are tamping；Universal fluorescence fluid photochemistry microreactor part is then prepared.
8. a kind of 3D printing manufacturing method of Universal fluorescence fluid photochemistry microreactor part according to claim 7,
It is characterized in that, the layer printing precision that the 3D printer is selected is 0.025-0.1mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910161945.4A CN109758995B (en) | 2019-03-05 | 2019-03-05 | Universal fluorescent fluid photochemical microreactor part and 3D printing manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910161945.4A CN109758995B (en) | 2019-03-05 | 2019-03-05 | Universal fluorescent fluid photochemical microreactor part and 3D printing manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109758995A true CN109758995A (en) | 2019-05-17 |
| CN109758995B CN109758995B (en) | 2020-12-11 |
Family
ID=66456646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910161945.4A Active CN109758995B (en) | 2019-03-05 | 2019-03-05 | Universal fluorescent fluid photochemical microreactor part and 3D printing manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109758995B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110813211A (en) * | 2019-12-03 | 2020-02-21 | 广东省新材料研究所 | Micro-reactor and manufacturing method thereof |
| CN111266069A (en) * | 2020-01-17 | 2020-06-12 | 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 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070183933A1 (en) * | 2004-02-18 | 2007-08-09 | Hitachi Chemical Co., Ltd | Supporting unit for microfluid system |
| JP2010132597A (en) * | 2008-12-04 | 2010-06-17 | Mitsui Eng & Shipbuild Co Ltd | Apparatus and method for carrying out oxidation treatment of toluene |
| CN104028188A (en) * | 2014-01-20 | 2014-09-10 | 南京工业大学 | Ultraviolet light micro-channel reactor |
| CN104888874A (en) * | 2015-05-27 | 2015-09-09 | 上海交通大学 | Preparation method and application of micro-fluidic chip based on 3D printing technique |
| CN207401491U (en) * | 2017-08-28 | 2018-05-25 | 重庆中控欧玛仪表研究院有限公司 | For the micro-fluidic chemical luminous chip of cell tests |
| CN108786687A (en) * | 2017-05-02 | 2018-11-13 | 上海交通大学 | Photochemical reaction system based on micro- Chemical Engineering Technology |
| CN208194370U (en) * | 2018-04-13 | 2018-12-07 | 中国平煤神马能源化工集团有限责任公司 | A kind of photocatalysis microchannel processing unit of caprolactam rearrangement reaction waste liquid |
-
2019
- 2019-03-05 CN CN201910161945.4A patent/CN109758995B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070183933A1 (en) * | 2004-02-18 | 2007-08-09 | Hitachi Chemical Co., Ltd | Supporting unit for microfluid system |
| JP2010132597A (en) * | 2008-12-04 | 2010-06-17 | Mitsui Eng & Shipbuild Co Ltd | Apparatus and method for carrying out oxidation treatment of toluene |
| CN104028188A (en) * | 2014-01-20 | 2014-09-10 | 南京工业大学 | Ultraviolet light micro-channel reactor |
| CN104888874A (en) * | 2015-05-27 | 2015-09-09 | 上海交通大学 | Preparation method and application of micro-fluidic chip based on 3D printing technique |
| CN108786687A (en) * | 2017-05-02 | 2018-11-13 | 上海交通大学 | Photochemical reaction system based on micro- Chemical Engineering Technology |
| CN207401491U (en) * | 2017-08-28 | 2018-05-25 | 重庆中控欧玛仪表研究院有限公司 | For the micro-fluidic chemical luminous chip of cell tests |
| CN208194370U (en) * | 2018-04-13 | 2018-12-07 | 中国平煤神马能源化工集团有限责任公司 | A kind of photocatalysis microchannel processing unit of caprolactam rearrangement reaction waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 荣国斌编著: "《高等有机化学基础》", 31 May 2009, 上海：华东理工大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110813211A (en) * | 2019-12-03 | 2020-02-21 | 广东省新材料研究所 | Micro-reactor and manufacturing method thereof |
| CN111266069A (en) * | 2020-01-17 | 2020-06-12 | 山东清创化工有限公司 | Photochemical synthesis system and method with customizable light source |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109758995B (en) | 2020-12-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109758995A (en) | A kind of Universal fluorescence fluid photochemistry microreactor part and its 3D printing manufacturing method | |
| Bonfield et al. | Photons as a 21st century reagent | |
| Noël | A personal perspective on the future of flow photochemistry | |
| Aillet et al. | Accurate measurement of the photon flux received inside two continuous flow microphotoreactors by actinometry | |
| Van Gerven et al. | A review of intensification of photocatalytic processes | |
| Sohrabi et al. | A review on the design and development of photocatalyst synthesis and application in microfluidic reactors: Challenges and opportunities | |
| Carofiglio et al. | Fullerene‐promoted singlet‐oxygen photochemical oxygenations in glass‐polymer microstructured reactors | |
| JPH09225295A (en) | Photocatalyst-containing device and photocatalyst utilizing reactor | |
| Burek et al. | Completely integrated wirelessly-powered photocatalyst-coated spheres as a novel means to perform heterogeneous photocatalytic reactions | |
| US10258957B2 (en) | Flow reactor for photochemical reactions | |
| CN104028188A (en) | Ultraviolet light micro-channel reactor | |
| CN103239987B (en) | Methane conversion device | |
| US11872556B2 (en) | General-purpose fluorescent fluid photochemical microreactor and manufacturing method therefor by 3D printing | |
| Zhao et al. | Reactor optimization and process intensification of photocatalysis for capillary-based PMMA LSC-photomicroreactors | |
| CN202099089U (en) | Portable photocatalytic reactor for organic wastewater treatment | |
| JP5349930B2 (en) | Method for oxidizing toluene | |
| CN110396107A (en) | A kind of Yellow luminous chiral nano silver clustered materials of high stable and its application in white light LEDs | |
| CN111266069B (en) | Photochemical synthesis system and method with customizable light source | |
| CN201147688Y (en) | Actinic chemistry reactor using LED as light source | |
| Usami et al. | Photocatalytic degradation of 4-chlorophenol in a photochemical reactor with an interconnected microchannel and a light guide network | |
| JP2007075682A (en) | Continuous flow photochemical reaction apparatus and method for producing photochemical reaction product by using the same | |
| CN112191203A (en) | LED light source photocatalysis tubular reactor and application thereof | |
| CN111790335A (en) | Ultraviolet photochemical reactor device based on continuous flow technology | |
| CN101337174B (en) | Strengthened photochemical reactor | |
| CN113019266B (en) | Continuous photocatalytic pipe reactor and method for carrying out trifluoromethylation reaction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |