CN109806823A - Continuous photochemical reaction unit and system - Google Patents
Continuous photochemical reaction unit and system Download PDFInfo
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- CN109806823A CN109806823A CN201910195168.5A CN201910195168A CN109806823A CN 109806823 A CN109806823 A CN 109806823A CN 201910195168 A CN201910195168 A CN 201910195168A CN 109806823 A CN109806823 A CN 109806823A
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Abstract
The present invention provides a kind of continuous photochemical reaction unit and systems.The continuous photochemical reaction unit includes reaction member, and reaction member includes: transparent coil reactor；Transparent rack, transparent coil reactor are spirally coiled on transparent rack；Inner light source, inner light source extend along the coiling extending direction of transparent coil reactor, and transparent coil reactor is arranged around inner light source；Outer light source, outer light source are area source and the outside that transparent coil reactor is arranged in.Transparent coil reactor internal diameter is greatly reduced relative to traditional tank reactor, therefore the utilization rate of light source is higher, and then improves photochemical reaction efficiency, shortens the photochemical reaction time；The amount that the Gaseous materials of reaction are participated in unit time greatly reduces, and security risk is greatly reduced, it is easy to accomplish amplification production.Transparent coil reactor is individually supported using transparent rack, is conducive to the quantity between transparent coil reactor, inner light source and outer light source and the flexible setting of position.
Description
Technical field
The present invention relates to photochemical reaction technical fields, in particular to a kind of continuous photochemical reaction unit and are
System
Background technique
Current existing photochemical reaction technology mostly uses greatly tank reactor, easily due to gases such as ethylene, acetylene, hydrogen
Combustion explosion, the high requirements on the equipment, photochemical reaction is carried out in traditional still reaction, and there are great security risks, uncomfortable
In industrialized production.
Moreover, traditional autoclave photochemistry technological reaction time is long, because the light efficiency of lamp source unit light-emitting area is big
Big to weaken, reaction is completed to generally require more than ten hour even several days, and production efficiency is lower.
In addition, mercury lamp or hernia lamp etc. that traditional photochemical reactor uses luminescence band range wider mostly, then cooperate
Filter carries out photochemical reaction, and not only structure is complicated for this mode, and wastes the luminous efficiency of lamp source significantly；While by
It is high to radiating capacity of equipment requirement in quantity of heat production height, it is lower compared with the universal light intensity of LED lamp source under same electric power conditions；And due to
The defect service life of itself lamp source is also shorter, causes the raising of photochemical reaction equipment investment and equipment operating cost.
Summary of the invention
The main purpose of the present invention is to provide a kind of continuous photochemical reaction unit and systems, to solve in the prior art
Photochemical reaction equipment when being used for gas reaction safety it is low and the problem of be not easy industrial applications.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of continuous photochemical reaction unit, packet
Reaction member is included, reaction member includes: transparent coil reactor；Transparent rack, transparent coil reactor are spirally coiled in transparent
On bracket；Inner light source, inner light source extend along the coiling extending direction of transparent coil reactor, and transparent coil reactor is around interior light
Source setting；Outer light source, outer light source are area source and the outside that transparent coil reactor is arranged in.
Further, above-mentioned transparent coil reactor is projected as ring in the plane vertical with the extending direction of inner light source
Shape structure, ring structure include that two are opposite and parallel straightway and two curved sections, curved section replace connection with straightway,
The corresponding transparent coil reactor side of each straightway of ring structure is planar side.
Further, above-mentioned outer light source includes two planar light sources, and each planar side is provided with a planar light source, and flat
Area source is arranged in parallel with planar side, and the area of preferred planar light source and the area of plane of planar side are equal.
Further, above-mentioned transparent rack has multiple, the transparent rack spaced set of planar side, and preferably clear bracket is
Hollow stent, further preferred hollow stent are connected to cold source.
Further, above-mentioned transparent coil reactor is FEP tubular reactor or quartz tube reactor.
Further, above-mentioned inner light source and outer light source are UVLED light source.
Further, above-mentioned continuous photochemical reaction unit further includes temperature regulating device, and reaction member is arranged in temperature regulating device
In, preferably temperature regulating device is air cooling device.
According to another aspect of the present invention, a kind of continuous photochemical reaction system is provided, comprising: feeding device；One
Or any of the above-described kind of continuous photochemical reaction unit of multiple parallel connections；
Product reception device, feeding device, the transparent coil reactor of continuous photochemical reaction unit and product, which receive, to be filled
It sets and is sequentially communicated.
Further, above-mentioned feeding device includes: gas raw material power supply unit；Liquid charging stock power supply unit；Air and liquid mixer, with
Gas raw material power supply unit is connected to liquid charging stock power supply unit, and the outlet of air and liquid mixer is connected to transparent coil reactor.
Further, gas flow control is provided on the pipeline between above-mentioned gas raw material supply device and air and liquid mixer
Device is provided with liquid pump on the pipeline between liquid charging stock power supply unit and air and liquid mixer, and continuous photochemical reaction system also wraps
PLC control device is included, PLC control device and gas flow controller, liquid pump and the anti-of continuous photochemical answer the inner light source of device
It is electrically connected with outer light source.
It applies the technical scheme of the present invention, the reactor of continuous photochemical reaction unit is transparent coil reactor, therefore
Its internal diameter is greatly reduced relative to traditional tank reactor, therefore can obtain sufficient illumination, light in reactant wherein
The utilization rate in source is higher, and then photochemical reaction efficiency can be improved, and shortens the photochemical reaction time；In addition, when due to unit
The amount of the interior Gaseous materials for participating in reaction greatly reduces, and security risk is greatly reduced；And reaction scale can not be by
The limitation of reactor size, for example multiple continuous photochemical reaction units are carried out in parallel while being reacted, and then are easily achieved
Amplification production.Simultaneously as individually being supported using transparent rack to transparent coil reactor, therefore be conducive to transparent coil pipe
The flexible setting of quantity and position between reactor, inner light source and outer light source, and transparent coil reactor amplifies design
When not will receive the limitation of inner light source, therefore can satisfy the needs of more kinds of continuous photochemical reaction units.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the continuous photochemical reaction unit side view provided according to an embodiment of the present；
Fig. 2 shows the top views of continuous photochemical reaction unit shown in FIG. 1；And
Fig. 3 shows the continuous photochemical reaction system structural schematic diagram provided according to an embodiment of the present invention.
Wherein, the above drawings include the following reference numerals:
11, transparent coil reactor；12, transparent rack；13, inner light source；14, outer light source；
01, feeding device；011, gas raw material power supply unit；012, liquid charging stock power supply unit；013, air and liquid mixer；014,
Gas flow controller；015, liquid pump；02, continuous photochemical reaction unit；03, product reception device；04, PLC control dress
It sets.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
Carrying out photochemical reaction as the application background technique is analyzed, in traditional still reaction of the prior art, there are poles
Big security risk, is unsuitable for industrialized production.In order to solve this problem, this application provides a kind of reactions of continuous photochemical
Apparatus and system.
In a kind of typical embodiment of the application, a kind of continuous photochemical reaction unit is provided, such as Fig. 1 and 2 institute
Show, which includes reaction member, reaction member include transparent coil reactor 11, transparent rack 12,
Inner light source 13 and outer light source 14, transparent coil reactor 11 are spirally coiled on transparent rack 12；Inner light source 13 is along transparent coil pipe
The coiling extending direction of reactor 11 extends, and transparent coil reactor 11 is arranged around inner light source 13；Outer light source 14 is area source
And the outside of transparent coil reactor 11 is set.
The reactor of the continuous photochemical reaction unit of the application be transparent coil reactor 11, therefore its internal diameter relative to
Traditional tank reactor greatly reduces, therefore can obtain sufficient illumination in reactant wherein, the utilization rate of light source compared with
Height, and then photochemical reaction efficiency can be improved, shorten the photochemical reaction time；In addition, due to participating in reaction in the unit time
The amounts of Gaseous materials greatly reduce, security risk is greatly reduced；And reaction scale can not be limited by reactor size
System, for example multiple continuous photochemical reaction units are carried out in parallel while being reacted, and then are easily achieved amplification production.Together
When, due to individually being supported using transparent rack 12 to transparent coil reactor 11, be conducive to transparent coil reactor
11, the flexible setting of the quantity between inner light source 13 and outer light source 14 and position, and transparent coil reactor 11 is amplified and is set
Timing not will receive the limitation of inner light source 13, therefore can satisfy the needs of more kinds of continuous photochemical reaction units.
The transparent coil reactor 11 of the application can be conventional round screw thread coil reactor, in order to improve heat dissipation effect
Rate, preferably as shown in Fig. 2, projection of the above-mentioned transparent coil reactor 11 in the plane vertical with the extending direction of inner light source 13
For ring structure, ring structure includes that two opposite and parallel straightway and two curved sections, curved section replace with straightway
Connection, corresponding transparent 11 side of coil reactor of each straightway of ring structure are planar side.Pass through setting straightway and song
Line segment, so that the coil pipe relative distribution of transparent coil reactor 11, is conducive to conduct heat away.
It is preferably as illustrated in fig. 1 and 2, above-mentioned in order to further increase the reaction efficiency of material in transparent coil reactor 11
Outer light source 14 includes two planar light sources, and each planar side is provided with a planar light source, and planar light source is parallel with planar side
Setting, the area of preferred planar light source and the area of plane of planar side are equal.Using planar light source to transparent coil reactor 11
Planar side in material irradiated, enable wherein material equably receive more luminous energy, and then improve the reaction of material
Efficiency.Above-mentioned inner light source 13 may be set to be multiple, i.e., can increase and decrease inner light source number according to reaction requirement；What reaction needed
Light intensity is stronger/close, and inner light source is more；Multiple inner light sources need distribution as uniform as possible, to guarantee transparent plate tube reaction as far as possible
The light intensity of device relative position irradiation is identical.
The above-mentioned transparent rack 12 of the application makes it relative to inner light source primarily to support transparent coil reactor 11
13 and outer light source 14 it is relatively fixed, it is as illustrated in fig. 1 and 2, preferably above-mentioned in order to improve the stability of transparent coil reactor 11
Bright bracket 12 has multiple, 12 spaced set of transparent rack of planar side.In addition to light transmittance is further increased, preferably clear
Bracket 12 is hollow stent, simultaneously because the hollow setting of transparent rack 12, which can be attached with cold source, from
And transparent rack 12 is made to realize heat transfer effect, improve the emission efficiency of reaction heat.Using the hollow setting of transparent rack 12, can incite somebody to action
It avoids and cooling jacket is arranged between lamp source and coil pipe as temperature regulating device, and then avoids cooling jacket and cause lamp source
Light intensity decreasing.
In order to improve the translucency of transparent coil reactor 11, preferably above-mentioned transparent coil reactor 11 is FEP (perfluor second
Allyl alkene copolymer) tubular reactor or quartz tube reactor.Above-mentioned FEP tubular reactor or quartz tube reactor, knot
Structure has more lightweight performance, and light transmission is high, and can high temperature resistant and higher pressure.
Preferably, above-mentioned inner light source 13 and outer light source 14 can be medium pressure mercury lamp, high-pressure sodium lamp, preferably UVLED light source.
Above-mentioned UVLED light source light-emitting efficiency is high, quantity of heat production is low, the service life is long.
In a kind of embodiment of the application, above-mentioned continuous photochemical reaction unit further includes temperature regulating device, and reaction member is set
It sets in temperature regulating device, preferably temperature regulating device is air cooling device.Using set temperature regulating device to transparent coil reactor 11
Temperature regulated and controled, improve the stability and reaction efficiency of its internal-response.
In another typical embodiment of the application, a kind of continuous photochemical reaction system is provided, such as Fig. 3 institute
Show, which includes feeding device 01, one or more any of the above-described kind of continuous photochemicals in parallel
Reaction unit 02 and product reception device 03, the transparent coil reactor 11 of feeding device 01, continuous photochemical reaction unit 02
It is sequentially communicated with product reception device 03.
Since the reactor of the continuous photochemical reaction unit 02 of the application is transparent coil reactor 11, internal diameter
It is greatly reduced relative to traditional tank reactor, sufficient illumination, the utilization rate of light source can be obtained in reactant wherein
It is higher, and then photochemical reaction efficiency can be improved, shorten the photochemical reaction time；In addition, persistently being supplied using feeding device 01
Material, product reception device 03 persistently receive reaction product, therefore participate in reaction in the unit time in the state of successive reaction
The amount of Gaseous materials greatly reduces, and security risk is greatly reduced；And reaction scale can not be limited by reactor size,
For example multiple continuous photochemical reaction units 02 are carried out in parallel while being reacted, and then are easily achieved amplification production.Meanwhile
Due to individually being supported to transparent coil reactor 11 using transparent rack 12, be conducive to transparent coil reactor 11,
The flexible setting of quantity and position between inner light source 13 and outer light source 14 meets more kinds of continuous photochemical reaction units 02
It needs.
In a kind of embodiment of the application, above-mentioned feeding device 01 includes gas raw material power supply unit 011, liquid charging stock supply
Device 012 and air and liquid mixer 013, air and liquid mixer 013 are connected to gas raw material power supply unit 011 and liquid charging stock power supply unit 012,
And the outlet of air and liquid mixer 013 is connected to transparent coil reactor 11.Air and liquid mixer 013 makes gas raw material power supply unit 011
The reaction solution that the reaction gas and liquid charging stock power supply unit 012 of offer provide uniformly mixes, and the steady of reaction condition has been effectively ensured
It is qualitative.
In order to further increase reaction condition control accuracy, preferably as shown in figure 3, above-mentioned gas raw material supply device
Gas flow controller 014, liquid charging stock power supply unit 012 and gas-liquid are provided on pipeline between 011 and air and liquid mixer 013
Liquid pump 015 is provided on pipeline between mixer 013, continuous photochemical reaction system further includes PLC control device 04,
The inner light source 13 of PLC control device 04 and gas flow controller 014, liquid pump 015 and continuous photochemical reaction unit 02 and
Outer light source 14 is electrically connected.PLC control device 04 and gas flow controller 014, liquid pump 015 and continuous photochemical reaction unit
02 inner light source 13 is electrically connected with outer light source 14, adjusts gas in real time using gas flow controller 014 using PLC control device 04
The flow velocity of body raw material utilizes the flow velocity of the real-time adjustment liquid charging stock of liquid pump 015 simultaneously, and former according to gas raw material and liquid
The ratio of material is adjusted the intensity of illumination of inner light source 13 and outer light source 14, is guaranteed by the control to above-mentioned reaction condition anti-
The stability answered.
The beneficial effect of the application is further illustrated below with reference to embodiment and comparative example.
Embodiment 1
At room temperature, by compound AIt is dissolved in solvent acetonitrile after stirring clarification, with liquid pump 015 with 10mL/min's
Speed, while propylene alkene gas is driven into the speed of 200mL/min by gas-liquid mixed by gas flow controller 014 simultaneously
In device 013 (volume 200mL), the transparent coil reactor 11 of FEP material is accessed after air and liquid mixer 013 out (such as Fig. 1 institute
Show) receive illumination reaction, the bore of transparent coil reactor 11 is 4mm, and length of straigh line 30cm, curved section is arc,
Its radius is 5cm, and the total length of transparent coil reactor is 16m, and wherein inner light source 13 is a cylinder UVLED, and power exists
It is adjusted between 100~500W, outer light source 14 is two flat UVLED, the plane of respective area and transparent coil reactor
Lateral area is equal, and power is adjusted between 100~500W, controls in transparent coil reactor 11 temperature of charge at 30~60 DEG C,
Outlet sampling is analyzed using IPC-GC, product purity 98%, and the system of outflow obtains product in reduced under vacuum removing solvent
Yield 90%.
Embodiment 2
At room temperature, by compound AIt is dissolved in solvent acetonitrile after stirring clarification, with liquid pump 015 with 10mL/min's
Speed, while being squeezed into styrene (talan) liquid simultaneously with the speed of 200mL/min by gas flow controller 014
Into liquid liquid mixer 013 (volume 200mL), the transparent coil reactor 11 of FEP material is accessed after air and liquid mixer 013 out
(as shown in Figure 1) receives illumination reaction, and the bore of transparent coil reactor 11 is 4mm, length of straigh line 30cm, curved section
For arc, radius 5, the total length of transparent coil reactor is 16m, and wherein inner light source 13 is three circles equidistantly arranged
Cylindricality UVLED, power are adjusted between 100~500W, outer light source 14 be two flat UVLED, respective area with it is transparent
The planar side area equation of coil reactor, power are adjusted between 100~500W, control material in transparent coil reactor 11
Temperature is at 30~60 DEG C, and outlet sampling is analyzed using IPC-GC, product purity 97%, and the system of outflow is de- in reduced under vacuum
Except solvent obtains product yield 90%.
Comparative example 1
Difference from Example 1 is that the shape of transparent coil reactor is round screw thread, and the radius of coil pipe is 6cm,
The total length of transparent coil reactor is 16m and is fixed on cylindrical inner light source that inner light source is cylinder UVLED, power
It is adjusted between 100~500W, is not provided with outer light source, outlet sampling is analyzed using IPC-GC, product purity 95%, outflow
System obtains product yield 82% in reduced under vacuum removing solvent.
Comparative example 2
Difference from Example 1 is that the shape of transparent coil reactor is round screw thread, and the radius of coil pipe is 6cm,
The total length of transparent coil reactor is 16m, and is fixed on cylindrical inner light source, and inner light source is the cylinder of cold-trap package
UVLED, power are adjusted between 100~500W, are not provided with outer light source, and outlet sampling is analyzed using IPC-GC, and product purity is
91%, the system of outflow obtains product yield 79% in reduced under vacuum removing solvent.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
The reactor of the continuous photochemical reaction unit of the application is transparent coil reactor, therefore its internal diameter is relative to biography
The tank reactor of system greatly reduces, therefore can obtain sufficient illumination in reactant wherein, and the utilization rate of light source is higher,
And then photochemical reaction efficiency can be improved, shorten the photochemical reaction time；In addition, due to the gas for participating in reaction in the unit time
The amount of state material greatly reduces, and security risk is greatly reduced；And reaction scale can not be limited by reactor size, than
Such as multiple continuous photochemical reaction units are carried out in parallel while reacted, and then is easily achieved amplification production.Simultaneously as
Transparent coil reactor is individually supported using transparent rack, therefore is conducive to transparent coil reactor, inner light source and outer
The flexible setting of quantity and position between light source, and when transparent coil reactor amplifies design, not will receive inner light source
Limitation, therefore can satisfy the needs of more kinds of continuous photochemical reaction units.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of continuous photochemical reaction unit, which is characterized in that including reaction member, the reaction member includes:
Transparent coil reactor (11)；
Transparent rack (12), the transparent coil reactor (11) are spirally coiled on the transparent rack (12)；
Inner light source (13), the inner light source (13) extends along the coiling extending direction of the transparent coil reactor (11), described
Transparent coil reactor (11) is arranged around the inner light source (13)；
Outer light source (14), the outer light source (14) are area source and are arranged in the outside of the transparent coil reactor (11).
2. continuous photochemical reaction unit according to claim 1, which is characterized in that the transparent coil reactor (11)
It is projected as ring structure in the plane vertical with the extending direction of the inner light source (13), the ring structure includes two
Opposite and parallel straightway and two curved sections, the curved section replace connection with the straightway, the ring structure
Corresponding transparent coil reactor (11) side of each straightway is planar side.
3. continuous photochemical reaction unit according to claim 2, which is characterized in that the outer light source (14) includes two
Planar light source, each planar side is provided with the planar light source, and the planar light source is parallel with the planar side
Setting, the area of the preferably described planar light source are equal with the area of plane of the planar side.
4. continuous photochemical reaction unit according to claim 2, which is characterized in that the transparent rack (12) has more
A, the transparent rack (12) spaced set of the planar side, the preferably described transparent rack (12) is hollow stent, into one
The preferably hollow stent is walked to be connected to cold source.
5. continuous photochemical reaction unit according to claim 1, which is characterized in that the transparent coil reactor (11)
For FEP tubular reactor or quartz tube reactor.
6. continuous photochemical reaction unit according to claim 1, which is characterized in that the inner light source (13) and described outer
Light source (14) is UVLED light source.
7. continuous photochemical reaction unit according to claim 1, which is characterized in that the continuous photochemical reaction unit
It further include temperature regulating device, the reaction member is arranged in the temperature regulating device, and the preferably described temperature regulating device is air cooling device.
8. a kind of continuous photochemical reaction system characterized by comprising
Feeding device (01)；
Continuous photochemical reaction unit (02) described in one or more any one of claims 1 to 7 in parallel；
Product reception device (03), the feeding device (01), the transparent coil pipe of the continuous photochemical reaction unit (02) are anti-
Device (11) is answered to be sequentially communicated with the product reception device (03).
9. continuous photochemical reaction system according to claim 8, which is characterized in that the feeding device (01) includes:
Gas raw material power supply unit (011)；
Liquid charging stock power supply unit (012)；
Air and liquid mixer (013) is connected to the gas raw material power supply unit (011) and the liquid charging stock power supply unit (012), and
The outlet of the air and liquid mixer (013) is connected to the transparent coil reactor (11).
10. continuous photochemical reaction system according to claim 9, which is characterized in that the gas raw material power supply unit
(011) gas flow controller (014), the liquid charging stock are provided on the pipeline between the air and liquid mixer (013)
Liquid pump (015), the continuous photochemical are provided on pipeline between power supply unit (012) and the air and liquid mixer (013)
Reaction system further includes PLC control device (04), the PLC control device (04) and the gas flow controller (014), institute
The inner light source (13) for stating liquid pump (015) and the continuous photochemical reaction unit (02) is electrically connected with outer light source (14).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910195168.5A CN109806823A (en) | 2019-03-14 | 2019-03-14 | Continuous photochemical reaction unit and system |
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| CN111138651A (en) * | 2019-12-31 | 2020-05-12 | 浙江巨化技术中心有限公司 | Synthetic method of perfluoropolyether peroxide |
| CN112191203A (en) * | 2020-03-13 | 2021-01-08 | 上海合全药业股份有限公司 | LED light source photocatalysis tubular reactor and application thereof |
| CN113398858A (en) * | 2020-09-10 | 2021-09-17 | 宁波诺丁汉大学 | Photochemical reactor |
| CN114797714A (en) * | 2022-05-27 | 2022-07-29 | 凯莱英医药集团（天津）股份有限公司 | Continuous photochemical reaction unit and system |
| EP4077210A4 (en) * | 2019-12-16 | 2024-01-17 | Quantum Elements Development Inc. | Quantum printing nanostructures within carbon nanopores |
| CN117732396A (en) * | 2024-02-21 | 2024-03-22 | 天津凯莱英医药科技发展有限公司 | Continuous photocatalytic reaction device and system |
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| EP4077210A4 (en) * | 2019-12-16 | 2024-01-17 | Quantum Elements Development Inc. | Quantum printing nanostructures within carbon nanopores |
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