CN108786687A - Photochemical reaction system based on micro- Chemical Engineering Technology - Google Patents

Photochemical reaction system based on micro- Chemical Engineering Technology Download PDF

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Publication number
CN108786687A
CN108786687A CN201710301252.1A CN201710301252A CN108786687A CN 108786687 A CN108786687 A CN 108786687A CN 201710301252 A CN201710301252 A CN 201710301252A CN 108786687 A CN108786687 A CN 108786687A
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China
Prior art keywords
micro
chemical engineering
engineering technology
reaction channel
reaction system
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Pending
Application number
CN201710301252.1A
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Chinese (zh)
Inventor
苏远海
李光晓
徐文华
商敏静
路庆华
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Priority to CN201710301252.1A priority Critical patent/CN108786687A/en
Publication of CN108786687A publication Critical patent/CN108786687A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/123Ultraviolet light
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/127Sunlight; Visible light
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00788Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • B01J2219/00792One or more tube-shaped elements
    • B01J2219/00797Concentric tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00873Heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871Heating or cooling of the reactor

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A kind of photochemical reaction system based on micro- Chemical Engineering Technology of photochemistry applied technical field, including:Multichannel microreactor and LED light strip, wherein:Multichannel microreactor is equipped with reaction channel group, and reaction channel group one end is connected with mixing chamber, the other end is connected with collecting chamber, and reaction channel group's outer helical is wound with LED light strip;The reaction channel group is made of the reaction channel of several annular arrays.The present invention can obtain uniform illumination, improve the yield and degree of purity of product during photochemical transformation in conjunction with the characteristics of photochemical transformation and micro- Chemical Engineering Technology, while reaching higher thermal matter transfer performance inside reaction channel.

Description

Photochemical reaction system based on micro- Chemical Engineering Technology
Technical field
It is specifically a kind of based on the photochemical of micro- Chemical Engineering Technology the present invention relates to a kind of technology in photochemical reaction field Learn reaction system.
Background technology
Photochemical transformation because its with it is environmental-friendly, compare thermal chemical reaction with relatively mild reaction condition, can realize The features such as reaction process that some thermochemical studies are difficult to realize, worldwide obtains extensive since the 1970s Concern.
But inside reactor uneven illumination is even in existing light reaction technology, easily causes side reaction, thus reaction selectivity It is low, seriously affect production efficiency;On the other hand, capacity usage ratio is low, effective temperature control of light source and reaction system is difficult and Reaction process amplification is also the problem for restricting photochemical transformation and realizing extensive commercial application.
Invention content
The present invention is directed to deficiencies of the prior art, it is proposed that a kind of photochemical reaction based on micro- Chemical Engineering Technology System can improve photochemical in conjunction with the characteristics of photochemical transformation and micro- Chemical Engineering Technology, while reaching higher thermal matter transfer performance Learn the yield and degree of purity of product in conversion process.
The present invention is achieved by the following technical solutions:
The present invention includes:Multichannel microreactor and LED light strip, wherein:Multichannel microreactor is equipped with reaction channel group, Reaction channel group one end is connected with mixing chamber, the other end is connected with collecting chamber, and reaction channel group's outer helical is wound with LED light Band;
The reaction channel group is made of the reaction channel of several annular arrays.
The reaction channel is capillary;Preferably, capillary inner diameter is 0.25~3mm.
The mixing chamber is equipped with several feed inlets and capillary discharge port, capillary discharge port quantity and reaction channel Quantity is identical, position and reaction channel correspond.
The LED light strip by several annular arrays light source fixed rod support, it is good inside reaction channel to ensure Light distribution improves yield;The both ends of the light source fixed link are fixedly connected with mixing chamber, collecting chamber respectively.
The light source fixed link quantity is no less than 3.
The light source of the LED light strip be 200~400nm of wave-length coverage 400~760nm of ultraviolet light or wave-length coverage can It is light-exposed;Light source can be replaced according to the requirement of differential responses system.
The material of the reaction channel is the thermoplastic polymer material with translucency such as FEP, PFA, ETFE, ECTFE;Its Remaining structure material can be inorganic material, such as stainless steel, copper, zinc, aluminium, silicon carbide or organic glass;It is different according to each component It is welding or pressure fastening that the corresponding mode that is fixedly connected, which can be selected, in material.
Preferably, the LED light strip outer cover is equipped with heat exchange sleeve, enhances heat exchange efficiency, removes light source luminescent in time The heat that process generates, further increases the service life of light source and the yield of photochemical transformation process.
Heat transferring medium in the heat exchange sleeve is one or more mixed in Cryogenic air, low temperature nitrogen and low temperature argon gas Close gas.
Technique effect
Compared with prior art, present invention combination photochemical transformation and the characteristics of micro- Chemical Engineering Technology, reaches higher mass transfer, biography While hot rate, the good light distribution of reaction channel, efficient electricity conversion and larger flux behaviour are realized Make, improve yield, the degree of purity of product during photochemical transformation, reduce energy consumption, is suitable for a variety of photochemical reaction systems;Together When this system internal structure it is simple, each component independently installed can be dismantled, convenient processing and manufacture.
Description of the drawings
Fig. 1 is the overall structure front view that the present invention is equipped with heat exchange sleeve;
Fig. 2 is the structure front view that the present invention does not install heat exchange sleeve;
Fig. 3 is internal structure front view of the present invention without heat exchange sleeve and LED light strip;
Fig. 4 is A-A sectional views in Fig. 2;
In figure:Mixing chamber 1, collecting chamber 2, heat exchange sleeve 3, LED light strip 4, reaction channel 5, light source fixed link 6.
Specific implementation mode
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation Example.
Embodiment 1
As shown in Figure 1, Figure 2 and Figure 3, the present embodiment includes:Multichannel microreactor and LED light strip 4, wherein:Multichannel Microreactor is equipped with reaction channel group, and reaction channel group one end is connected with mixing chamber 1, the other end is connected with collecting chamber 2, and reaction is logical Road group's outer helical is wound with LED light strip 4, and 4 outside of LED light strip is equipped with heat exchange sleeve 3;
As shown in figure 4, the reaction channel group is made of the reaction channel 5 of 25 annular arrays.
The reaction channel 5 is capillary;Preferably, capillary inner diameter 0.75mm, length 2.5m, material are PFA。
The mixing chamber 1 is set there are two feed inlet and 25 capillary discharge ports.
Preferably, the LED light strip 4 is supported by the light source fixed link 6 of 3 annular arrays, the light source fixed link 6 Both ends are fixedly connected with mixing chamber 1, collecting chamber 2 respectively.
The LED light strip 4 emits the visible light that characteristic wavelength is 530nm, power 60W.
Preferably, the heat transferring medium in the heat exchange sleeve 3 is Cryogenic air.
The present embodiment carries out benzenethiol light-catalyzed reaction using above system:Using oxygen as gas phase, containing benzenethiol, tetramethyl Ethylenediamine and the methanol solution in Yihong are liquid phase, reaction time 90s, the product diphenyl disulfide being collected into, yield It is 90%.
Embodiment 2
As shown in Figures 2 and 3, the present embodiment includes:Multichannel microreactor and LED light strip 4, wherein:Multichannel is micro- anti- Device is answered to be equipped with reaction channel group, reaction channel group one end is connected with mixing chamber 1, the other end is connected with collecting chamber 2, reaction channel group Outer helical is wound with LED light strip 4;
As shown in figure 4, the reaction channel group is made of the reaction channel 5 of 25 annular arrays.
The reaction channel 5 is capillary;Preferably, capillary inner diameter 1.59mm, length 4.1m, material are FEP。
The mixing chamber 1 is set there are two feed inlet and 25 capillary discharge ports.
Preferably, the LED light strip 4 is supported by the light source fixed link 6 of 3 annular arrays;The light source fixed link 6 Both ends are fixedly connected with mixing chamber 1, collecting chamber 2 respectively.
4 launch wavelength of the LED light strip is the ultraviolet light of 365nm, power 300W.
The present embodiment carries out maleic anhydride photocatalysis dimerization reaction using above system:Gas phase is nitrogen, and liquid phase is quality The maleic anhydride solution of score 5%, solvent are ethyl acetate, and reaction time 19.1min is collected into product cyclobutane Tetracarboxylic acid dianhydride, yield 30%.
Embodiment 3
As shown in Figure 1, Figure 2 and Figure 3, the present embodiment includes:Multichannel microreactor and LED light strip 4, wherein:Multichannel Microreactor is equipped with reaction channel group, and reaction channel group one end is connected with mixing chamber 1, the other end is connected with collecting chamber 2, and reaction is logical Road group's outer helical is wound with LED light strip 4, and 4 outside of LED light strip is equipped with heat exchange sleeve 3;
As shown in figure 4, the reaction channel group is made of the reaction channel 5 of 25 annular arrays.
The reaction channel 5 is capillary;Preferably, capillary inner diameter 1.59mm, length 4.1m, capillary tubes Matter is FEP.
The mixing chamber 1 is set there are two feed inlet and 25 capillary discharge ports.
Preferably, the LED light strip 4 is supported by the light source fixed link 6 of 3 annular arrays;The light source fixed link 6 Both ends are fixedly connected with mixing chamber 1, collecting chamber 2 respectively.
The LED light strip 4 emits the ultraviolet light that characteristic wavelength is 365nm, power 300W.
Preferably, the heat transferring medium in the heat exchange sleeve 3 is low temperature nitrogen.
The present embodiment carries out maleic anhydride photocatalysis dimerization reaction using above system:Gas phase is nitrogen, and liquid phase is quality The maleic anhydride solution of score 5%, solvent are ethyl acetate, and reaction time 19.1min is collected into product cyclobutane Tetracarboxylic acid dianhydride, yield 42%;
High-pressure sodium lamp is usually set to the center of tank reactor as light source in the prior art:To be in equilateral triangle cloth The high-pressure sodium lamp of 3 200W set is arranged in the central area of tank reactor, the ultraviolet light that transmitting characteristic wavelength is 365nm, Under the same reaction conditions, it is exchanged heat using low temperature nitrogen, heat exchange amount is 2 times of the present embodiment, and yield is only 20%;If single high The power ascension of pressure mercury lamp to 600W, reaction light application time need to increase to 1 hour, and yield is only 10%.

Claims (9)

1. a kind of photochemical reaction system based on micro- Chemical Engineering Technology, which is characterized in that including:Multichannel microreactor and LED Light belt, wherein:Multichannel microreactor is equipped with reaction channel group, and reaction channel group one end is connected with mixing chamber, other end connection There are collecting chamber, reaction channel group's outer helical to be wound with LED light strip;
The reaction channel group is made of the reaction channel of several annular arrays.
2. the photochemical reaction system according to claim 1 based on micro- Chemical Engineering Technology, characterized in that the reaction is logical Road is capillary, and capillary inner diameter is 0.25~3mm.
3. the photochemical reaction system according to claim 2 based on micro- Chemical Engineering Technology, characterized in that the reaction channel Material be the thermoplastic polymer material with translucency such as FEP, PFA, ETFE, ECTFE.
4. the photochemical reaction system according to claim 2 based on micro- Chemical Engineering Technology, characterized in that the mixing chamber Equipped with several feed inlets and capillary discharge port, capillary discharge port quantity is identical as reaction channel quantity, position with react Channel corresponds.
5. the photochemical reaction system according to claim 1 based on micro- Chemical Engineering Technology, characterized in that the LED light Band by the light source fixed rod support of several annular arrays, fix with mixing chamber, collecting chamber respectively by the both ends of the light source fixed link Connection.
6. the photochemical reaction system according to claim 5 based on micro- Chemical Engineering Technology, characterized in that the light source is solid Fixed pole quantity is no less than 3.
7. the photochemical reaction system according to claim 5 based on micro- Chemical Engineering Technology, characterized in that the LED light The visible light of 400~760nm of ultraviolet light or wave-length coverage with 200~400nm of launch wavelength range.
8. the photochemical reaction system according to claim 5 based on micro- Chemical Engineering Technology, characterized in that the LED light Band outer cover is equipped with heat exchange sleeve.
9. the photochemical reaction system according to claim 8 based on micro- Chemical Engineering Technology, characterized in that the heat exchange sleeve In heat transferring medium be Cryogenic air, low temperature nitrogen and low temperature argon gas in one or more mixed gas.
CN201710301252.1A 2017-05-02 2017-05-02 Photochemical reaction system based on micro- Chemical Engineering Technology Pending CN108786687A (en)

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Application Number Priority Date Filing Date Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109758995A (en) * 2019-03-05 2019-05-17 大连理工大学 A kind of Universal fluorescence fluid photochemistry microreactor part and its 3D printing manufacturing method
CN110773089A (en) * 2019-11-05 2020-02-11 山东奇谱创能生物科技有限公司 Multi-channel chemical micro-reaction equipment based on single light beam
CN111790335A (en) * 2019-04-08 2020-10-20 上海交通大学 Ultraviolet photochemical reactor device based on continuous flow technology
CN114195620A (en) * 2021-12-23 2022-03-18 上海交通大学 Method for synthesizing phenol by photo-oxidation benzene continuous flow based on micro-reactor
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1911498A (en) * 2006-08-01 2007-02-14 华东师范大学 Capillary tube array photo catalysis reactor and its preparation and application
CN201147688Y (en) * 2007-12-17 2008-11-12 天津理工大学 Actinic chemistry reactor using LED as light source
CN203392892U (en) * 2013-08-15 2014-01-15 陕西理工学院 Photocatalytic magnetic inorganic adsorption electroplating wastewater treatment device
CN105344299A (en) * 2015-11-16 2016-02-24 北京中教金源科技有限公司 LED light source photochemical reaction instrument

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1911498A (en) * 2006-08-01 2007-02-14 华东师范大学 Capillary tube array photo catalysis reactor and its preparation and application
CN201147688Y (en) * 2007-12-17 2008-11-12 天津理工大学 Actinic chemistry reactor using LED as light source
CN203392892U (en) * 2013-08-15 2014-01-15 陕西理工学院 Photocatalytic magnetic inorganic adsorption electroplating wastewater treatment device
CN105344299A (en) * 2015-11-16 2016-02-24 北京中教金源科技有限公司 LED light source photochemical reaction instrument

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109758995A (en) * 2019-03-05 2019-05-17 大连理工大学 A kind of Universal fluorescence fluid photochemistry microreactor part 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
CN111790335A (en) * 2019-04-08 2020-10-20 上海交通大学 Ultraviolet photochemical reactor device based on continuous flow technology
CN110773089A (en) * 2019-11-05 2020-02-11 山东奇谱创能生物科技有限公司 Multi-channel chemical micro-reaction equipment based on single light beam
CN114195620A (en) * 2021-12-23 2022-03-18 上海交通大学 Method for synthesizing phenol by photo-oxidation benzene continuous flow based on micro-reactor

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Application publication date: 20181113

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