CN105833815A - Low/normal temperature photoreactor - Google Patents

Low/normal temperature photoreactor Download PDF

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Publication number
CN105833815A
CN105833815A CN201510020992.9A CN201510020992A CN105833815A CN 105833815 A CN105833815 A CN 105833815A CN 201510020992 A CN201510020992 A CN 201510020992A CN 105833815 A CN105833815 A CN 105833815A
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China
Prior art keywords
photoreactor
heat radiation
photoreaction
integral type
reaction
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Pending
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CN201510020992.9A
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Chinese (zh)
Inventor
冯科
吴骊珠
陈彬
张丽萍
佟振合
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Technical Institute of Physics and Chemistry of CAS
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Technical Institute of Physics and Chemistry of CAS
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Priority to CN201510020992.9A priority Critical patent/CN105833815A/en
Publication of CN105833815A publication Critical patent/CN105833815A/en
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Abstract

The invention belongs to the technical field of photoreaction, and particularly relates to a low/normal temperature photoreactor, which comprises: the integrated supporting and radiating module comprises a liquid cooling module and is used for carrying out liquid cooling radiation on the LED light source; the stirring and adjusting device is used for adjusting the light intensity of the LED light source; the light reaction container is arranged above the stirring and adjusting device through the integrated supporting and heat dissipation module; the light reaction container performs light reaction under the irradiation of the LED light source, and the reaction temperature is adjusted through the liquid cooling module. The low/normal temperature photoreactor of the invention is widely suitable for small-dose photochemical synthesis reaction.

Description

A kind of low/normal-temperature light reactor
Technical field
The present invention relates to a kind of Photoreactor, particularly relate to one and be widely used in low dose of photochemical Learn synthetic reaction and the low/normal-temperature light reactor of high flux screening.
Background technology
Photochemical syntheses reaction directly utilizes light radiation as energy source, overcomes reaction gesture Build, generate product via excited state species;Different from thermal chemical reaction, photochemical reaction is direct Construct target compound structure, it is possible to be greatly simplified synthetic reaction step, embody efficient, former Subeconomy and eco-friendly modern concepts, become what current Synthetic Organic Chemistry was enlivened the most One of research field.
At present, photochemical syntheses reaction mainly uses with relatively large lamps such as halogen lamp, mercury lamp, xenon lamps Has the Photoreactor as light source, owing to needing to use the radiator structure of transparent material, these light Structure of reactor is complicated, relatively costly and is only applicable to heavy dose of photochemical syntheses reaction, There is presently no the Photoreactor being specifically designed to the reaction of laboratory small photochemical syntheses.
Summary of the invention
The present invention provides a kind of Photoreactor, the most applicable to solve Photoreactor of the prior art Technical problem in heavy dose of photochemical syntheses reaction.
For solving above-mentioned technical problem, the present invention provides a kind of low/normal-temperature light reactor, including: LED light source, integral type support heat radiation module, stirring and adjusting means and photoreaction container, Described integral type supports heat radiation module and includes liquid cooled module, for carrying out described LED light source Liquid-cooling heat radiation;Described stirring and adjusting means are for regulating the light intensity of described LED light source;Institute State photoreaction container and be arranged on described stirring and regulation by described integral type support heat radiation module The top of device;Described photoreaction container carries out photoreaction under the irradiation of described LED light source, And regulate reaction temperature by described liquid cooled module, carry out low-temp reaction and/or normal-temperature reaction; Described Photoreactor uses when low-temp reaction and the identical replaceable light of normal-temperature reaction Reaction vessel.
Further, described integral type supports heat radiation module by rustless steel, copper, aluminum manufacture.
Further, described liquid cooled module includes condensed fluid inlet hole, condensed fluid flow pipe and cold Lime set is portalled, and described liquid cooled module portals cold with outer loop by condensed fluid inlet hole and condensed fluid Solidifying device is connected.
Further, described integral type supports heat radiation module and includes guiding groove, and described photoreaction is held Device is inserted by described guiding groove and supports heat radiation module with described integral type and fits tightly.
Further, described photoreaction container includes seal washer, for holding in described photoreaction When device inserts described integral type support heat radiation module, the steam in air is stoped to enter described one Formula supports heat radiation module and condenses therein.
Further, described photoreaction container is partially coated with shading more than described seal washer Japanning.
Further, described LED light source includes LED array and connects with described LED array The driving power supply connect, described LED array is arranged on described integral type and supports in heat radiation module.
Further, described LED array is vertical LED array or horizontal LED array.
Further, described stirring and adjusting means use magnetic agitation or machinery concussion.
Further, the photoreaction that described photoreaction container is carried out is low-temp reaction and/or often Temperature reaction.Therefore, the present invention is directed to the light for the reaction of laboratory small photochemical syntheses Reactor, to meet the core demand of photochemical syntheses repercussion study the following aspects: the highest Flux: permutation and combination or a series of condition to numerous reactants are screened, and need to enter simultaneously The multiple parallel reactions of row;2. low dose of: simultaneously the most cost-effective during screening;The highest light intensity: Improve photoreaction speed, save the response time;4. Single wavelength: use the light of specific wavelength to select Property excite specific photosensitizer, reduce side reaction.
Accompanying drawing explanation
Fig. 1: embodiment of the present invention Photoreactor structural representation;
Fig. 2: embodiment of the present invention integral type supports heat radiation module cut-away view;
Fig. 3: embodiment of the present invention photoreaction container supports the installation on heat radiation module in integral type Schematic diagram;
Wherein, 1, integral type supports heat radiation module;1a, guiding groove;1b, condensed fluid portal; 1c, condensed fluid inlet hole;2, stirring and adjusting means;2a, switch;2b, display lamp;2c、 Adjusting knob;3, photoreaction container;3a, seal washer;3b, japanning shading light part;3c、 Standard interface;4, LED chip.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below will knot Close the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, Be fully described by, it is clear that described embodiment be a part of embodiment of the present invention rather than Whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having Make the every other embodiment obtained under creative work premise, broadly fall into present invention protection Scope.
Seeing Fig. 1, the embodiment of the present invention provides a kind of Photoreactor, including: LED light source, Integral type supports heat radiation module 1, stirring and adjusting means 2 and photoreaction container 3, integral type Support heat radiation module 1 and include liquid cooled module, for LED light source is carried out liquid-cooling heat radiation;Stir Mix and adjusting means 2 is for regulating the light intensity of LED light source and stirring or impact strength;Light is anti- Answer container 3 to support heat radiation module 1 by integral type and be arranged on the upper of stirring and adjusting means 2 Side;Photoreaction container 3 carries out photoreaction under the irradiation of LED light source, and by liquid chill Block regulation reaction temperature, carries out low-temp reaction and/or normal-temperature reaction;Described Photoreactor exists Use and normal-temperature reaction identical replaceable photoreaction container during low-temp reaction.
In embodiments of the present invention, the low-temp reaction temperature range of Photoreactor is at-80 DEG C~4 DEG C Between, normal-temperature reaction is typically at 23 DEG C ± about 5 DEG C.
Wherein, integral type support heat radiation module 1 can be had heat radiation by rustless steel, copper, aluminum etc. The metal material of performance is made, and preferably can use aluminium manufacture, although the aluminum alloy heat coefficient of expansion Relatively big, but heat conduction is good, it is easy to processing, relative low price, it is highly suitable as support and dissipates Hot material.Form as in figure 2 it is shown, integral type supports heat radiation module 1 by multiple block combiner, interior Portion leaves wiring groove and installing hole.Integral type supports the liquid cooled module internal structure of heat radiation module 1 Have condensed fluid flow pipe, by condensed fluid portal 1b and condensed fluid inlet hole 1c cold with outer loop Solidifying device is connected, and this condenser system, on the one hand for the heat radiation of LED light source, on the other hand also may be used From outside regulation and control photoreaction container 3 temperature, operation interval be 80 DEG C to room temperature.Further, liquid Chill block can select different condensed fluid according to different reaction conditions with reaction temperature.Often Can adopt during temperature reaction and use water as condensed fluid, the aqueous solution of alcohol or alcohol during low-temp reaction, can be used to make For condensed fluid.Therefore, the photoreaction container in the embodiment of the present invention can be widely used in low temperature And/or under normal temperature condition.
As it is shown on figure 3, integral type supports heat radiation module 1 may be configured with perforation and guiding groove 1a, many Individual interchangeable photoreaction container 3 can be inserted by guiding groove 1a and support with integral type dissipating Thermal module 1 fits tightly so that therebetween can heat-shift to greatest extent.It addition, Integral type is supported and can be engaged by seal washer 3a between heat radiation module 1 and photoreaction container 3, So can effectively stop the steam in air to enter integral type and support heat radiation module internal condensation, Avoid LED light source short circuit.It addition, photoreaction container 3 can in the part of more than seal washer 3a To scribble shading japanning, form japanning shading light part 3b, to avoid photoreaction container 3 using During cause light pollution.
LED light source can include LED array and the driving power supply being connected with LED array, LED chip 4 in LED array can be arranged on integral type and support in heat radiation module 1, by electricity Line is connected formation loop with stirring and adjusting means 2.It is arranged on integral type in LED chip 4 to support Time on heat radiation module 1, will also pass through waterproof package simultaneously and process, to improve the resistance to of Photoreactor Degree for a long time.LED chip 4 in the LED array of the embodiment of the present invention can use vertical or horizontal battle array Row.In vertical LED array, integral type supports heat radiation module 1 and aluminium can be preferably used, In horizontal LED array integral type support heat radiation module 1 can be preferably used steel and with stirring and The upper surface (upper surface is support system) of adjusting means 2 blends.The embodiment of the present invention Drive power supply different because of the connection quantity of LED chip, use current control mode, exchange input Support 110~220V, 50~60Hz civil power, the integral waterproofing standard of the embodiment of the present invention meets IP65 degree of protection.
Stirring and adjusting means 2 can use magnetic agitation or machinery concussion, can by switch 2a, Display lamp 2b, adjusting knob 2c switch, indicate, regulate mixing speed, and pass through current intensity Regulate and control the luminous intensity of LED chip 4.
The photoreaction container 3 of the embodiment of the present invention can use Pyrex glass or quartz to make, can For having the standard interface 3c such as #14/20, #19/22, #24/29, #24/40, screw socket, smallmouth Straight type test tube.
In magnetic agitation mode, according to the arrangement principle of symmetrical expression photoreaction container 3, for vertical Photoreaction container 3 arrangement of formula LED array optimum can be 1,2 × 1,2 × 2,4 × 1,4 × 2; Horizontal LED array is set according to the effective coverage of magnetic agitation and the symmetry of photoreaction container 3 Putting, the arrangement of peak optimization reaction container can be 4 multi pack modes, 7 multi pack modes, or 12 multi packs Etc. mode.In machinery concussion mode, the arrangement of photoreaction container 3 can be m × n rectangle Array, and match with horizontal LED array.Plastic lens can be installed additional for horizontal LED array Sheet optically focused module (can promote light utilization efficiency about 10~15%).
The embodiment of the present invention uses high-power LED light source to tie with stirring and adjusting means 2 phase Close, it is adaptable to the photochemical syntheses reaction of low dose of type and high flux screening, its cost is relatively low, Easy heat radiation, taking up room little, and the embodiment of the present invention is further introduced into liquid-cooling heat radiation mode, In many aspects there is important improvement:
The most open global design without casing, ultimate attainment miniaturization, portable, save space.This Photoreactor size involved by invention is far smaller than the most various commercially available Photoreactor, such as Fig. 1 Shown in, model machine a size of 20cm × 15cm × 16cm (L × W × H), and including Portion is fully integrated required power supply and adapter, connects civil power and can use, if selected further Select the greater compactness of commercially available magnetic stirring apparatus of size, can miniaturization further.
2. using modular unitary design, meet technical grade standard, integrated level is high, becomes This is low.Wherein, integral type support heat radiation module 1 be industrial processes aluminium sheet radiator, stir and Adjusting means 2 has been further introduced into LED on the basis of commercially available small magnetic agitator and has controlled electricity Source, photoreaction container 3 is the straight type test tube with standard interface, and LED chip 4 is commercially available Gao Gong Rate LED sheet, contains ultraviolet, visible, the various wavelength of near-infrared, and all parts all can be according to Industrial standard carries out waterproof and dampproof process.
3. for photochemical syntheses repercussion study small, high flux, high light intensity, unicast Long core demand.Use multiple straight type test tube parallel reaction, can be simultaneously to numerous reactants Permutation and combination or a series of condition are screened;The cumulative volume of type reaction solution is 5~20 ML, saves reagent cost;Unit volume reaction solution by optical energy density high (seeing table 1), Photoreaction speed is fast, saves the response time;Specific wavelength LED can be chosen and used up during illumination Quick dose of coupling, farthest reduces the generation of side reaction.
4. make the straight type test tube of apparatus standard interface as replaceable photoreaction container, low cost Honest and clean, and conveniently carry out various chemosynthesis standard operations or the process such as anhydrous, anaerobic.
5. support housing liquid cold temperature control design so that low-temp reaction as normal-temperature reaction, Identical replaceable photoreaction container can be used, it is not necessary to use custom-designed sandwich Transparent reaction container, enters light intensity simultaneously and keeps constant, so can be substantially reduced low-temp reaction Cost, simplification operating procedure;Overcome in existing cryogenic technique and can only enter light from bottom or middle part, Realize high intensity of illumination;The design using waterproof guiding groove to match with seal washer, successfully solves The problem that certainly under open environment, steam easily condenses on low-temperature components.
6. support heat radiation module and have employed totally enclosed unitary design, photoreaction container part Outer surface has carried out japanning shading treatment, has carried out global optimization, make in terms of preventing light pollution Obtain Photoreactor can use in open environment easily.
A kind of use for laboratory miniaturization LED involved in the present invention is low/normal-temperature light reactor with make Comparing with the Photoreactor of halogen lamp, mercury lamp, xenon lamp etc., comprehensive advantage is obvious;At a class acyl group Transport reaction (reaction 1, Org.Lett.2014,16,5968), a class intersection dehydrogenation coupling reaction (reaction 2, J.Am.Chem.Soc.2013,135,19052) and class Photocatalyzed Hydrogen Production reaction are (anti- Answer 3, J.Am.Chem.Soc.2014,136,8261) comparative result in is as shown in table 1.This LED light reactor light intensity under the conditions of Single wavelength is much larger than solar simulator AM 1.5 (100mW/cm2) standard, the optical energy density that unit volume reaction solution accepts is big, it is possible to big Shorten greatly the response time.Photosensitizer is obvious with selected optical source wavelength matching effect, as in reaction 3 In using CdTe quantum as photosensitizer time, to absorb spectral coverage reaction efficiency high, in weak suction strong Receive spectral coverage reaction efficiency low, even do not react, show rational wavelength dependency.
The LED light reactor of table 1. present invention and halogen lamp, mercury lamp, the comparison of xenon lamp reactor:
Remarks:[1]Newport company Model 842-PE portable light energy meter is used to measure;[2]Typical case is anti- The cumulative volume answering solution is 10mL;[3]Series of parallel experiment reaches the result of same reaction degree.
The above is only the preferred embodiment of the present invention, it is noted that lead for this technology For the those of ordinary skill in territory, on the premise of without departing from the technology of the present invention principle, it is also possible to Making some improvement and replacement, these improve and replace and also should be regarded as protection scope of the present invention.

Claims (9)

1. a Photoreactor, it is characterised in that including: LED light source, integral type support Heat radiation module, stirring and adjusting means and photoreaction container, described integral type supports heat radiation module Including liquid cooled module, for described LED light source is carried out liquid-cooling heat radiation;Described stirring and tune Regulating device is for regulating the light intensity of described LED light source;Described photoreaction container passes through described one Body formula supports heat radiation module and is arranged on the top of described stirring and adjusting means;Described photoreaction is held Device carries out photoreaction under the irradiation of described LED light source, and is regulated by described liquid cooled module Reaction temperature, carries out low-temp reaction and/or normal-temperature reaction;Described Photoreactor is anti-at low temperature Seasonable use and the identical replaceable photoreaction container of normal-temperature reaction.
2. Photoreactor as claimed in claim 1, it is characterised in that described integral type is propped up Support heat radiation module is by rustless steel, copper, aluminum manufacture.
3. Photoreactor as claimed in claim 1, it is characterised in that described liquid cooled module Portalling including condensed fluid inlet hole, condensed fluid flow pipe and condensed fluid, described liquid cooled module passes through Condensed fluid inlet hole is portalled with condensed fluid and is connected with outer loop condensing unit.
4. Photoreactor as claimed in claim 1, it is characterised in that described integral type is propped up Support heat radiation module include guiding groove, described photoreaction container inserted by described guiding groove and with institute State integral type support heat radiation module to fit tightly.
5. Photoreactor as claimed in claim 1, it is characterised in that described photoreaction is held Device includes seal washer, supports heat radiation mould for inserting described integral type at described photoreaction container During group, stop the steam in air to enter described integral type and support heat radiation module and coagulate therein Knot.
6. Photoreactor as claimed in claim 5, it is characterised in that described photoreaction is held The device shading that is partially coated with more than described seal washer is painted.
7. Photoreactor as claimed in claim 1, it is characterised in that described LED light source Including LED array and the driving power supply that is connected with described LED array, described LED array It is arranged on described integral type to support in heat radiation module.
8. Photoreactor as claimed in claim 7, it is characterised in that described LED array For vertical LED array or horizontal LED array.
9. Photoreactor as claimed in claim 1, it is characterised in that described stirring and tune Regulating device uses magnetic agitation or machinery concussion.
CN201510020992.9A 2015-01-15 2015-01-15 Low/normal temperature photoreactor Pending CN105833815A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108126640A (en) * 2018-01-23 2018-06-08 北京缔森科技发展有限公司 A kind of bottom illuminated high temperature and pressure photochemical reaction kettle
WO2022127926A1 (en) * 2020-12-19 2022-06-23 北京大学 Liquid phase synthesis assisted system

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Publication number Priority date Publication date Assignee Title
JP4905856B2 (en) * 2007-03-29 2012-03-28 東京電力株式会社 Photocatalytic reactor
CN202188707U (en) * 2011-05-24 2012-04-11 石页 Water-filling type wavy ice box
CN202709589U (en) * 2012-03-28 2013-01-30 王文斌 Novel ice box
CN203148138U (en) * 2013-03-07 2013-08-21 戴仁德 Wave ice box
CN103357364A (en) * 2012-03-27 2013-10-23 中国科学院理化技术研究所 Photoreactor
CN103752360A (en) * 2013-12-30 2014-04-30 西安天隆科技有限公司 Thermal module for biochemical reaction
CN204522959U (en) * 2015-01-15 2015-08-05 中国科学院理化技术研究所 Low/normal temperature photoreactor

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4905856B2 (en) * 2007-03-29 2012-03-28 東京電力株式会社 Photocatalytic reactor
CN202188707U (en) * 2011-05-24 2012-04-11 石页 Water-filling type wavy ice box
CN103357364A (en) * 2012-03-27 2013-10-23 中国科学院理化技术研究所 Photoreactor
CN202709589U (en) * 2012-03-28 2013-01-30 王文斌 Novel ice box
CN203148138U (en) * 2013-03-07 2013-08-21 戴仁德 Wave ice box
CN103752360A (en) * 2013-12-30 2014-04-30 西安天隆科技有限公司 Thermal module for biochemical reaction
CN204522959U (en) * 2015-01-15 2015-08-05 中国科学院理化技术研究所 Low/normal temperature photoreactor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108126640A (en) * 2018-01-23 2018-06-08 北京缔森科技发展有限公司 A kind of bottom illuminated high temperature and pressure photochemical reaction kettle
WO2022127926A1 (en) * 2020-12-19 2022-06-23 北京大学 Liquid phase synthesis assisted system

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