CN104028188A - Ultraviolet light micro-channel reactor - Google Patents
Ultraviolet light micro-channel reactor Download PDFInfo
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- CN104028188A CN104028188A CN201410025852.6A CN201410025852A CN104028188A CN 104028188 A CN104028188 A CN 104028188A CN 201410025852 A CN201410025852 A CN 201410025852A CN 104028188 A CN104028188 A CN 104028188A
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Abstract
本发明公开一种紫外光微通道反应器，其特征在于，包括透紫外光管、设置在透紫外光管内的紫外光发生器、和反应微通道；所述的反应微通道设置在透紫外光管的管壁外或管壁中。透紫外光管密封并设置有换热流体进口和换热流体出口。透紫外光管上设置有密封件以密封该透紫外光管，密封件可以避免换热流体的外流，提高换热效率。具体而言，本发明的技术方案可分为将反应微通道设置的与透紫外光管的管壁中和管壁外的两种技术方案实本发明提供了一种提高反应效率的光化学反应器；解决了紫外光发生器在于微反应器结合时紫外光发生器产生的热量干扰微反应器反应的技术问题。
The invention discloses an ultraviolet light microchannel reactor, which is characterized in that it comprises an ultraviolet light transmission tube, an ultraviolet light generator arranged in the ultraviolet light transmission tube, and a reaction microchannel; the reaction microchannel is arranged in the ultraviolet light transmission tube outside or in the pipe wall. The ultraviolet light-transmitting tube is sealed and provided with a heat exchange fluid inlet and a heat exchange fluid outlet. The ultraviolet light-transmitting tube is provided with a seal to seal the ultraviolet-transmitting tube. The seal can prevent the outflow of the heat exchange fluid and improve the heat exchange efficiency. Specifically, the technical scheme of the present invention can be divided into two technical schemes that the reaction microchannel is arranged and the tube wall of the ultraviolet light-transmitting tube and outside the tube wall. The present invention provides a photochemical reactor that improves reaction efficiency. ; The technical problem that the heat generated by the ultraviolet light generator interferes with the reaction of the microreactor when the ultraviolet light generator is combined with the microreactor is solved.
Description
Technical field
The present invention relates to a kind of ultraviolet light micro passage reaction, specifically belong to photocatalysis micro passage reaction field.
Background technology
Photochemistry is the chemical subdiscipline of the caused permanent chemical effect of research light-matter interaction, and value generally produces chemical reaction under the irradiation of visible ray or ultraviolet light.Photochemical reaction, is mainly manifested in than there being many different places from general reacting phase: heating makes molecule activation, and in system, Boltzmann's distribution is obeyed in the distribution of molecular energy; And molecule is while being subject to photoactivation, can accomplish in principle selective excitation, the distribution of the molecular energy in system belongs to non-equilibrium distribution.So photochemically reactive approach is often different with ground state thermal chemical reaction from product, as long as light wavelength is applicable to, can be absorbed by material, at very low temperature, photochemical reaction still can be carried out in time.
Micro passage reaction can replace various functions and the method for conventional chemical laboratory, and integration is high, automatically controls, accurately response parameter.The microfabricated chemical reactor carrying out in microchannel, because specific area is large, heat and mass is rapid, conversion ratio is obviously improved, and to the control of reaction be selectively also that popular response cannot be reached, so both combinations can be made the most of the advantage mutually, strengthening reaction, Reaction time shorten improves reaction efficiency.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of ultraviolet light micro passage reaction micro passage reaction for ultraviolet catalytic reaction and the manufacture method of saturating ultraviolet light pipe wherein.
This ultraviolet light micro passage reaction, can apply to the reaction in photocatalysis field widely, significant for accurately obtaining of reaction process condition, and the application that can carry out the fields such as fine chemistry industry and medicine be synthetic.
Technical scheme: a kind of micro passage reaction for ultraviolet catalytic reaction of the present invention, comprises ultraviolet light pipe, is arranged on ultraviolet light generator and microchannel in ultraviolet light pipe; Microchannel is arranged in the outer or tube wall of the tube wall of ultraviolet light pipe.Ultraviolet light pipe of the present invention is the pipeline that can make by ultraviolet material, can be that quartz ampoule or other those skilled in the art will know that to can be used to manufacture and can see through ultraviolet ray and can be used as the pipeline that in the present invention, ultraviolet light pipe is used thoroughly.Further, the saturating ultraviolet light seal of tube is also provided with heat exchanging fluid import and heat exchanging fluid outlet, like this, can heat or cooling ultraviolet light generator by heat exchanging fluid, controls better the temperature of microchannel place reaction system.Further, thoroughly on ultraviolet light pipe, be provided with seal to seal this saturating ultraviolet light pipe, seal can be avoided the outflow of heat exchanging fluid, improves heat exchange efficiency.Heat exchanging fluid can be gas or liquid, uses the gas can simplification device as heat exchanging fluid, uses liquid can improve heat exchange efficiency as heat exchanging fluid.Each interface of ultraviolet light micro passage reaction connects by ferrule fitting.
Particularly, technical scheme of the present invention can be divided into two kinds of technical schemes in that arrange and tube wall saturating ultraviolet light pipe and outside tube wall by microchannel and realizes:
Scheme one, microchannel is arranged on outside the tube wall of ultraviolet light pipe, and microchannel is comprised of the flexible duct for being wrapped in outside ultraviolet light tube wall.Flexible duct is that internal diameter is the polyfluortetraethylene pipe of 0.2～3mm.
Scheme two, microchannel is arranged in the tube wall of ultraviolet light pipe, and the width of microchannel is 0.2～3mm, and the degree of depth is 0.2～1mm, and the shape of this microchannel is helical structure.
On the basis of scheme one and scheme two, further, selecting ultraviolet light pipe is quartz ampoule, and microchannel (3) import department is provided with micro-mixer and precision syringe.
Further, ultraviolet light micro passage reaction also comprises the constant temperature heat-conducting layer being wrapped in outside microchannel, and constant temperature heat-conducting layer is connected to keep constant temperature or take protection for the electric heating layer arranging with oil bath or water bath device be micro-reaction channel place constant temperature; Further, ultraviolet light micro passage reaction also comprises the light shield layer being coated on outside microchannel.Constant temperature heat-conducting layer should be sentenced the reaction temperature of controlling microchannel place in order to be arranged at as much as possible near microchannel, therefore should light shield layer be arranged at outside constant temperature heat-conducting layer as far as possible, but light shield layer is arranged between constant temperature heat-conducting layer and microchannel and also can't affects realization of the present invention.Light shield layer can prevent that external light source from producing and disturbing photochemical reaction in microchannel.
Further, the ultraviolet light emission spectrum peak that ultraviolet light generator excites is 254 nanometers or 365 nanometers.
Further, thoroughly ultraviolet light pipe adopts following manufacture method processing to obtain being arranged on the microchannel (3) in the tube wall of ultraviolet light pipe (2):
(1) at saturating ultraviolet light pipe outer wall, be etched or machined into the microchannel (3) described in type;
(2) another saturating ultraviolet light pipe interference fit is enclosed within on the saturating ultraviolet light pipe outer wall that step (1) obtains;
(3) product that high-temperature calcination step (2) obtains, is integrated the melting of two-layer ultraviolet light pipe, forms airtight microchannel (3).
The situation that it is quartz ampoule that this manufacture method is particularly suitable for when saturating ultraviolet light pipe.
The invention provides a kind of micro passage reaction for ultraviolet catalytic reaction, this reactor is comprised of microchannel and ultraviolet generator and heat exchange unit, efficient mini blender and precise injection pump.This microreactor agent structure is multilayer system, and inside is ultraviolet light generator, and coaxial middle part is quartz ampoule, and quartz ampoule outside is micro passage reaction, and outermost layer can be set to heat tape.Ultraviolet light generator can selection type ultraviolet light generator for 254nm or 365nm wavelength; Microchannel is the microchannel of transparent polyfluortetraethylene pipe or quartzy upper etching, can see through ultraviolet light, and under ultraviolet light conditions, carry out chemical reaction.Heat tape can be reaction corresponding energy, the process of accelerated reaction is provided.In quartz ampoule, can pass into gas or liquid, for heating or cooling.Import department is furnished with efficient mini blender and precise injection pump.
Compared with prior art, its beneficial effect is in the present invention: a kind of photochemical reactor that improves reaction efficiency is provided.The saturating ultraviolet light seal of tube of internal layer of the present invention and be provided with heat exchanging fluid import and heat exchanging fluid outlet in can pass into required gas or liquid carries out cooling or heating, prevent that the heat that ultraviolet light generator produces from disturbing microreactor to react, driving a reaction carries out.Feeding system adopts the junction with micro passage reaction, and the efficient micro-mixer of connect can mix material in millisecond, one side material contact fully, react.Feeding system adopts accurate syringe pump, and the supply of material is accurately controlled.All pipelines of the present invention connect employing ferrule fitting, detachable, easy to maintenance, with low cost.The micro passage reaction of ultraviolet catalytic reaction provided by the present invention, simple in structure, easy to operate, adopt micro-mixer and micro passage reaction structure, make inside reactor specific area large, fully improve the reaction contact area of material, promoted greatly heat transfer, mass transfer and reaction.
Accompanying drawing explanation
Fig. 1 is the ultraviolet light micro passage reaction embodiment 1 device schematic diagram in the present invention;
Fig. 2 is the ultraviolet light micro passage reaction embodiment 2 device schematic diagrames in the present invention.
The specific embodiment
Below technical solution of the present invention is elaborated, but protection scope of the present invention is not limited to embodiment.
Embodiment 1:
Ultraviolet light micro passage reaction in the present embodiment, is characterized in that, comprises ultraviolet light pipe 2, is arranged on ultraviolet light generator 1 and microchannel 3 in ultraviolet light pipe 2; Microchannel 3 is arranged in the outer or tube wall of the tube wall of ultraviolet light pipe 2.Saturating ultraviolet light pipe 2 in the present embodiment seals and is provided with heat exchanging fluid import 6 and heat exchanging fluid outlet 7.Specifically by being thoroughly provided with seal 8 to seal this saturating ultraviolet light pipe 2 on ultraviolet light pipe 2.Each interface of ultraviolet light micro passage reaction connects by ferrule fitting.
Microchannel 3 in the present embodiment is arranged on outside the tube wall of ultraviolet light pipe 2, and this microchannel 3 is for being wrapped in the flexible duct outside ultraviolet light pipe 2 tube walls.
Flexible duct in the present embodiment is that internal diameter is the polyfluortetraethylene pipe of 0.2mm.
Saturating ultraviolet light pipe in the present embodiment is quartz ampoule, and microchannel 3 import departments are provided with micro-mixer 9 and precision syringe.
Ultraviolet light micro passage reaction in the present embodiment also comprises the constant temperature heat-conducting layer 5 being wrapped in outside microchannel 3, constant temperature heat-conducting layer is for being connected heat-insulation layer with oil bath or water bath device, but also can be set to electric heating layer, can play equally the effect that constant temperature is provided for reaction; Ultraviolet light micro passage reaction also comprises the light shield layer 4 being coated on outside microchannel 3, to avoid the interference effect of external light source light reflex.
Ultraviolet light generator in the present embodiment is ultraviolet light pipe, and the ultraviolet light emission spectrum peak that it excites is 254 nanometers.Ultraviolet light generator also can adopt UV-light luminous semiconductor, but UV-light luminous semiconductor also has the inferior position of the less and non-uniform light of luminous power, can select according to on-the-spot actual needs.In addition the ultraviolet light generator that, adopts ultraviolet light emission spectrum peak-to-peak value why to be worth in concrete actual enforcement can be chosen according to photochemically reactive needs.
Embodiment 2
Other arranges same embodiment 1, but wherein the internal diameter of flexible duct is 3mm.
Embodiment 3
Ultraviolet light micro passage reaction in the present embodiment comprises ultraviolet light pipe 2, is arranged on ultraviolet light generator 1 and microchannel 3 in ultraviolet light pipe 2; Microchannel 3 is arranged in the outer or tube wall of the tube wall of ultraviolet light pipe 2.
The saturating ultraviolet light pipe 2 of the present embodiment medium ultraviolet micro passage reaction seals and is provided with heat exchanging fluid import 6 and heat exchanging fluid outlet 7, thoroughly on ultraviolet light pipe 2, is provided with seal 8 to seal this saturating ultraviolet light pipe 2.Each interface of ultraviolet light micro passage reaction connects by ferrule fitting.
The microchannel 3 of the present embodiment medium ultraviolet micro passage reaction is arranged in the tube wall of ultraviolet light pipe 2, and the width of microchannel 3 is 0.2mm, and the degree of depth is 0.2mm, and the shape of this microchannel 3 is helical structure.
Saturating ultraviolet light pipe in the present embodiment is quartz ampoule, and microchannel 3 import departments are provided with micro-mixer 9 and precision syringe.
Ultraviolet light micro passage reaction in the present embodiment also comprises the constant temperature heat-conducting layer 5 being wrapped in outside microchannel 3, and constant temperature heat-conducting layer is electric heating layer, and ultraviolet light micro passage reaction also comprises the light shield layer 4 being coated on outside microchannel 3.
The present embodiment medium ultraviolet optical generator is UV-light luminous semiconductor, and the ultraviolet light emission spectrum peak that it excites is 365 nanometers.
Embodiment 4
Other arranges same embodiment 3, but wherein microchannel width is 3mm, and the degree of depth is 1mm.
Embodiment 5
The present embodiment is the manufacture method of the saturating ultraviolet light pipe in the ultraviolet micro passage reaction in the embodiment of the present invention 2, and this saturating ultraviolet light pipe 2 is quartz ampoule, by following steps, is made:
(1) at quartz ampoule outer wall, be etched or machined into type microchannel 3;
(2) another quartz ampoule interference fit is enclosed within on the quartz ampoule outer wall that step (1) obtains;
(3) product that high-temperature calcination step (2) obtains, is integrated two-layer quartz ampoule melting, forms airtight microchannel 3.
Obtain the saturating ultraviolet light pipe using in embodiment 2.
Embodiment 6
At the vapour Bark of 100ml, dye in green and add 0.5g nano-TiO
2, through irradiations such as ultraviolets, 60min, percent of decolourization can reach 92.5%.
Same solution, through the micro passage reaction of syringe pump injection embodiment 3, through ultraviolet catalytic, when bleaching time is 60s, percent of decolourization reaches 96.2%; When bleaching time is 240s, percent of decolourization reaches 99.5%.
Embodiment 7
In the direct scarlet dyestuff of 100ml, add 0.5g nano-TiO
2, through irradiations such as ultraviolets, 60min, percent of decolourization can reach 83.5%.
Same solution, through the micro passage reaction of syringe pump injection embodiment 3, through ultraviolet catalytic, when bleaching time is 60s, percent of decolourization reaches 93.2%; When bleaching time is 240s, percent of decolourization reaches 97.5%.
Embodiment 8
The oxidative degradation of UV/Fenton method to MTBE in polluted-water, at ambient temperature, works as H
2o
2for 10mM, Fe
2+for 2mM, pH is 2.4 o'clock, and the MTBE that initial concentration is 1mM can remove 99% through in 30min.
Same solution, through the micro passage reaction of syringe pump injection embodiment 3, through ultraviolet catalytic, bleaching time 5min, percent of decolourization reaches 99%.
Embodiment 9
At UV/H
2o
2method is in the oxidative degradation experimental study of MTBE in polluted-water, when ultraviolet wavelength is 254nm, and H
2o
2for 15mM, pH is 3.0 o'clock, the MTBE that initial concentration is 1mM, and in 60min, MTBE clearance can reach 97.6%.
Same solution, through the micro passage reaction of syringe pump injection embodiment 1, through ultraviolet catalytic, bleaching time 240s, percent of decolourization reaches 99%.
Embodiment 10
UV/TiO
2the oxidative degradation of method to MTBE in polluted-water, is that 254nm and MTBE initial concentration are under 1mM condition at ultraviolet wavelength, TiO
2concentration 2.0g/L, pH is that MTBE clearance can reach in 80%, 120min and can reach 99% in 3,60min.
Same solution, through the micro passage reaction of syringe pump injection embodiment 2, through ultraviolet catalytic, bleaching time 240s, percent of decolourization reaches 92%.
As mentioned above, although represented and explained the present invention with reference to specific preferred embodiment, it shall not be construed as the restriction to the present invention self.Not departing under the spirit and scope of the present invention prerequisite of claims definition, can make in the form and details various variations to it.
Claims (10)
1. a ultraviolet light micro passage reaction, is characterized in that, comprises ultraviolet light pipe (2), is arranged on ultraviolet light generator (1) and microchannel (3) in ultraviolet light pipe (2); Described microchannel (3) is arranged in the outer or tube wall of the tube wall of ultraviolet light pipe (2).
2. a kind of ultraviolet light micro passage reaction according to claim 1, is characterized in that, described saturating ultraviolet light pipe (2) seals and be provided with heat exchanging fluid import (6) and heat exchanging fluid outlet (7).
3. a kind of ultraviolet light micro passage reaction according to claim 2, it is characterized in that, on described saturating ultraviolet light pipe (2), be provided with seal (8) to seal this saturating ultraviolet light pipe (2), described each interface of ultraviolet light micro passage reaction connects by ferrule fitting.
4. a kind of ultraviolet light micro passage reaction according to claim 1, it is characterized in that, described microchannel (3) is arranged on outside the tube wall of ultraviolet light pipe (2), and described microchannel (3) is for being wrapped in the flexible duct outside ultraviolet light pipe (2) tube wall.
5. a kind of ultraviolet light micro passage reaction according to claim 4, is characterized in that, described flexible duct is that internal diameter is the polyfluortetraethylene pipe of 0.2～3mm.
6. a kind of ultraviolet light micro passage reaction according to claim 1, is characterized in that, described microchannel (3) is arranged in the tube wall of ultraviolet light pipe (2), and the width of described microchannel (3) is 0.2～3mm, and the degree of depth is 0.2～1mm.
7. according to a kind of ultraviolet light micro passage reaction described in claim 1,2,3,4,5 or 6, it is characterized in that, described saturating ultraviolet light pipe is quartz ampoule, and described microchannel (3) import department is provided with micro-mixer (9) and precise injection pump.
8. according to a kind of ultraviolet light micro passage reaction described in claim 1,2,3,4,5 or 6, it is characterized in that, described ultraviolet light micro passage reaction also comprises and is wrapped in the outer constant temperature heat-conducting layer (5) of microchannel (3), and described constant temperature heat-conducting layer is electric heating layer or the heat-insulation layer that is connected with oil bath or water bath device; Described ultraviolet light micro passage reaction also comprises the light shield layer (4) being coated on outside microchannel (3).
9. according to a kind of ultraviolet light micro passage reaction described in claim 1,2,3,4,5 or 6, it is characterized in that, the ultraviolet light emission spectrum peak that described ultraviolet light generator excites is 254 or 365nm.
10. a kind of ultraviolet light micro passage reaction according to claim 6, is characterized in that, adopts the processing of following manufacture method to obtain being arranged on the microchannel (3) in the tube wall of ultraviolet light pipe (2):
(1) at saturating ultraviolet light pipe outer wall, be etched or machined into the microchannel (3) described in type;
(2) another saturating ultraviolet light pipe interference fit is enclosed within on the saturating ultraviolet light pipe outer wall that step (1) obtains;
(3) product that high-temperature calcination step (2) obtains, is integrated the melting of two-layer ultraviolet light pipe, forms airtight microchannel (3).
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| CN201410025852.6A CN104028188A (en) | 2014-01-20 | 2014-01-20 | Ultraviolet light micro-channel reactor |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107645970A (en) * | 2015-03-26 | 2018-01-30 | 康宁股份有限公司 | Flow Reactors for Photochemical Reactions |
| CN109225095A (en) * | 2018-11-28 | 2019-01-18 | 内蒙古三爱富万豪氟化工有限公司 | Optical chlorinating reaction device and the method for preparing difluoromono-chloroethane |
| CN109758995A (en) * | 2019-03-05 | 2019-05-17 | 大连理工大学 | A universal fluorescent fluid photochemical microreaction device and its 3D printing manufacturing method |
| CN109999747A (en) * | 2019-04-23 | 2019-07-12 | 浙江工业大学 | A kind of device and preparation method thereof of serialization preparation adjacent nitro benzyl bromine |
| CN111138651A (en) * | 2019-12-31 | 2020-05-12 | 浙江巨化技术中心有限公司 | A kind of synthetic method of perfluoropolyether peroxide |
| WO2020177065A1 (en) * | 2019-03-05 | 2020-09-10 | 大连理工大学 | General-purpose fluorescent fluidic photochemical microreactor and manufacturing method therefor by 3d printing |
| CN111790335A (en) * | 2019-04-08 | 2020-10-20 | 上海交通大学 | UV light photochemical reactor device based on continuous flow technology |
| CN112961128A (en) * | 2021-02-19 | 2021-06-15 | 上海昶法新材料有限公司 | Novel production process device for preparing ASA |
| CN113003850A (en) * | 2020-11-13 | 2021-06-22 | 四川全息生态环境技术产业有限公司 | Advanced oxidation method and device |
| CN113307713A (en) * | 2021-06-29 | 2021-08-27 | 南京工程学院 | Method for preparing long-chain alkane by micro-channel-photocatalysis coupling |
| WO2025044587A1 (en) * | 2023-09-01 | 2025-03-06 | 浙江大学杭州国际科创中心 | Liquid core waveguide photoreactor and liquid core waveguide illumination method |
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| CN107645970A (en) * | 2015-03-26 | 2018-01-30 | 康宁股份有限公司 | Flow Reactors for Photochemical Reactions |
| CN107645970B (en) * | 2015-03-26 | 2021-08-06 | 康宁股份有限公司 | Flow Reactors for Photochemical Reactions |
| CN109225095A (en) * | 2018-11-28 | 2019-01-18 | 内蒙古三爱富万豪氟化工有限公司 | Optical chlorinating reaction device and the method for preparing difluoromono-chloroethane |
| CN109758995A (en) * | 2019-03-05 | 2019-05-17 | 大连理工大学 | A universal fluorescent fluid photochemical microreaction device and its 3D printing manufacturing method |
| US11872556B2 (en) | 2019-03-05 | 2024-01-16 | Dalian University Of Technology | General-purpose fluorescent fluid photochemical microreactor and manufacturing method therefor by 3D printing |
| WO2020177065A1 (en) * | 2019-03-05 | 2020-09-10 | 大连理工大学 | General-purpose fluorescent fluidic photochemical microreactor and manufacturing method therefor by 3d printing |
| CN111790335A (en) * | 2019-04-08 | 2020-10-20 | 上海交通大学 | UV light photochemical reactor device based on continuous flow technology |
| CN109999747A (en) * | 2019-04-23 | 2019-07-12 | 浙江工业大学 | A kind of device and preparation method thereof of serialization preparation adjacent nitro benzyl bromine |
| CN111138651A (en) * | 2019-12-31 | 2020-05-12 | 浙江巨化技术中心有限公司 | A kind of synthetic method of perfluoropolyether peroxide |
| CN113003850A (en) * | 2020-11-13 | 2021-06-22 | 四川全息生态环境技术产业有限公司 | Advanced oxidation method and device |
| CN112961128A (en) * | 2021-02-19 | 2021-06-15 | 上海昶法新材料有限公司 | Novel production process device for preparing ASA |
| CN112961128B (en) * | 2021-02-19 | 2023-05-16 | 上海昶法新材料有限公司 | Novel production process device for preparing ASA |
| CN113307713A (en) * | 2021-06-29 | 2021-08-27 | 南京工程学院 | Method for preparing long-chain alkane by micro-channel-photocatalysis coupling |
| WO2025044587A1 (en) * | 2023-09-01 | 2025-03-06 | 浙江大学杭州国际科创中心 | Liquid core waveguide photoreactor and liquid core waveguide illumination method |
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Application publication date: 20140910 |