CN207493676U - Continuous photochemical reaction unit and system - Google Patents
Continuous photochemical reaction unit and system Download PDFInfo
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- CN207493676U CN207493676U CN201720973262.5U CN201720973262U CN207493676U CN 207493676 U CN207493676 U CN 207493676U CN 201720973262 U CN201720973262 U CN 201720973262U CN 207493676 U CN207493676 U CN 207493676U
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Abstract
The utility model provides a kind of continuous photochemical reaction unit and system.The continuous photochemical reaction unit includes：Flow reactor；For providing illumination to flow reactor to carry out the radiation source and temperature regulating device of continuous photochemical reaction, temperature regulating device flow reactor and radiation source are located in temperature regulating device.By setting flow reactor, photochemical reaction is recurred, reaction raw materials continuously enter reactor, reaction product continuously discharges reactor, this reaction continuously flowed can be effectively improved the transmission efficiency of light radiation in the reactive mixture, so as to shorten the reaction time, reaction efficiency is improved, reduces side reaction.Not only compared with batch stable reaction, and temperature control simple operations are convenient, and factory-level, enlarge-effect smaller are amplified to from laboratory scale conducive to photochemical reaction is made.
Description
Technical field
The utility model is related to photochemical reaction fields, in particular to a kind of continuous photochemical reaction unit and are
System.
Background technology
Material molecule chemically reacts referred to as photochemical reaction caused by absorbing light quantum.Photochemical reaction have with
Lower advantage：A kind of just clean energy resource；General reactions mild condition；It carries out photochemical reaction and does not need to radical protection；In routine
In synthesis, synthetic route can be greatly shortened by being inserted into general photochemical reaction.
In the prior art, using batch photochemical reaction.It has the shortcomings that following apparent：1) batch photo chemistry technology,
The characteristics of light is propagated in reactant is the increase with reactor, and the transmission efficiency of light radiation in the reactive mixture drops rapidly
It is low, the reaction time is caused to lengthen, side reaction increases.2) batch photochemical reaction, since its reactor is to the particular/special requirement of material,
Its amplification from laboratory scale to factory-level is made to be difficult to carry out, and enlarge-effect is apparent.3) batch reactor belongs to complete mixed
Flow reactor, the product of generation cannot export in time, and the selectivity for leading to main reaction is deteriorated by this in Chemical Kinetics,
Yield declines, and the repeatability for making reaction is deteriorated.4) existing batch photochemical reaction technology, as reactor gradually increases
Greatly, the reason of concentration gradient of reaction mixture will also increase in system, this is also that reaction selectivity is caused to be deteriorated, and yield is low.
5) existing batch photo chemistry technology, heat exchange is more difficult, the probability increase that side reaction is caused to occur.Reaction time is long, by-product
Object is more, and yield is low, and temperature control is difficult.
Therefore, it is necessary to be improved to existing batch photochemical reaction, to improve reaction efficiency, reduce side reaction.
Utility model content
The main purpose of the utility model is that a kind of continuous photochemical reaction unit and system are provided, to solve existing skill
The problem of reaction efficiency is low in photochemical reaction in art.
To achieve these goals, one side according to the present utility model provides a kind of continuous photochemical reaction dress
It puts, which includes：Flow reactor；For carrying out continuous photochemical to flow reactor offer illumination
The radiation source and temperature regulating device of reaction are learned, temperature regulating device flow reactor and radiation source are located in temperature regulating device.
Further, radiation source is internal irradiation light source, and flow reactor is set around interior radiating light source.
Further, radiation source is mercury lamp or LED light.
Further, flow reactor is successive reaction coil pipe.
Further, successive reaction coil pipe coiling radiation source setting.
Further, radiation source includes center divergent light source and light source cold-trap, and light source cold-trap is around center diverging light
Source is set；Wherein, flow reactor is around the setting of light source cold-trap.
Further, light source cold-trap includes cold-trap medium inlet and cold-trap media outlet, and cold-trap medium inlet and cold-trap are situated between
Matter outlet is located around in the same level of center divergent light source and is oppositely arranged.
Further, temperature regulating device is reaction chuck, and flow reactor and radiation source are located in reaction chuck.
Further, reaction chuck includes chuck medium inlet and chuck media outlet.
To achieve these goals, one side according to the present utility model provides a kind of continuous photochemical reaction system
System, continuous photochemical reaction system include raw material device, continuous photochemical reaction unit and light source controller, continuous photochemical
Reaction unit is any of the above-described kind of continuous photochemical reaction unit, and continuous photochemical reaction unit passes through raw material power conveying device
It is connected with raw material device, light source controller is connected with the radiation source of continuous photochemical reaction unit and controls radiation source
Light intensity.
Using the technical solution of the utility model, by setting flow reactor so that photochemical reaction can continuously be sent out
Raw, reaction raw materials continuously enter reactor, and reaction product continuously discharges reactor, and this reaction continuously flowed can effectively change
The transmission efficiency of kind light radiation in the reactive mixture so as to shorten the reaction time, improves reaction efficiency, reduces side reaction.No
Only compared with batch stable reaction, and temperature control simple operations are convenient, and factory level is amplified to from laboratory scale conducive to photochemical reaction is made
Not, enlarge-effect smaller.
Description of the drawings
The accompanying drawings which form a part of this application are used to provide a further understanding of the present invention, this practicality
Novel illustrative embodiments and their description do not form the improper restriction to the utility model for explaining the utility model.
In the accompanying drawings：
Fig. 1 shows the structural representation of the continuous photochemical reaction unit in a kind of preferred embodiment according to the present invention
Figure；
Fig. 2 shows the process structures of the continuous photochemical reaction system in a kind of preferred embodiment according to the present invention
Schematic diagram；
Fig. 3 shows that the structure of the continuous photochemical reaction unit in another preferred embodiment according to the present invention is shown
It is intended to；And
Fig. 4 shows that the structure of the continuous photochemical reaction unit in another preferred embodiment according to the present invention is shown
It is intended to.
Wherein, above-mentioned attached drawing is marked including the following drawings：
10th, flow reactor；20th, radiation source；30th, temperature regulating device；
21st, center divergent light source；22nd, light source cold-trap；101st, reacting material inlet；102nd, reacting material outlet；
221st, cold-trap medium inlet；222nd, cold-trap media outlet；
301st, chuck medium inlet；302nd, chuck media outlet；
01st, raw material device；02nd, raw material power conveying device；03rd, continuous photochemical reaction unit；04th, light source controller.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the application can phase
Mutually combination.The utility model will be described in detail below with reference to the accompanying drawings and embodiments.
As background technology is previously mentioned, existing photochemical reaction is batch reaction, and reaction efficiency is low, expanding production holds
It is easier that by-product is more, in order to improve this situation of the prior art, in a kind of typical embodiment of the application, provide
A kind of continuous photochemical reaction unit, shown as shown in Figure 1, Figure 3 and Figure 4, which includes：Flow reactor
10；For carrying out the radiation source 20 of continuous photochemical reaction to the offer illumination of flow reactor 10；And temperature regulating device 30,
Flow reactor 10 and radiation source 20 are located in temperature regulating device 30.
Continuous photochemical reaction unit provided herein, by setting flow reactor 10 so that photochemical reaction
It can recur, reaction raw materials continuously enter reactor, and reaction product continuously discharges reactor, this reaction continuously flowed
The transmission efficiency of light radiation in the reactive mixture can be effectively improved, so as to shorten the reaction time, reaction efficiency is improved, reduces
Side reaction.Not only compared with batch stable reaction, and temperature control simple operations are convenient, amplify conducive to photochemical reaction is made from laboratory scale
To factory-level, enlarge-effect smaller.
In above-mentioned continuous photochemical reaction unit, radiation source 20 is using existing photochemically reactive radiation source 20
Can, as long as enabling to provide light radiation to the material in flow reactor 10.I.e. radiation source 20 can be interior spoke
Irradiation source, light source are located inside flow reactor 10.Can also be external irradiation light source, light source is located at outside flow reactor 10.
In a kind of preferred embodiment of the application, radiation source 20 is internal irradiation light source, and flow reactor 10 is around interior radiating light source
Setting.
Since the illumination that in photochemical reaction, radiation source 20 is provided needs to participate in continuously instead through flow reactor 10
The chemical reaction of material in device 10 is answered, thus, the material of flow reactor 10 should be light-transmitting materials, for example be glass or stone
English.Preferably quartzy, the translucency of quartz material is good, additionally it is possible to through ultraviolet light.In actual production, radiation source 20 can be with
For mercury lamp or LED light.
Flow reactor 10 in above-mentioned continuous photochemical reaction unit can realize continuous reaction using existing
Reactor can also be improved on the basis of existing batch reactor to realize continuous reaction, for example, using
The reactor of common batch photochemical reaction device carries out continuous feeding to material inlet, and from material outlet continuous discharge,
So as to fulfill serialization photochemical reaction.In a kind of preferred embodiment of the application, flow reactor 10 is successive reaction disk
Pipe.The volume of reactor can be adjusted flexibly by the height of coiled coil for successive reaction coil pipe, in the situation for improving treating capacity
Under need not extend reaction time or enhancing intensity of illumination, thus not only reaction efficiency effectively improves, but also reduces secondary anti-
The generation and the generation of by-product answered.
Correspondingly, above-mentioned flow reactor 10 further includes reacting material inlet 101 and reacting material outlet 102, so as to
Raw material device 01 is connected with collection of products device, so as to fulfill the continuous discharge reaction for continuously entering reactor and product of raw material
Device.
In above-mentioned preferred embodiment, when flow reactor 10 is successive reaction coil pipe, radiation source 20 equally may be used
To be arranged on the center of inside of successive reaction coil pipe, the periphery of successive reaction coil pipe can also be arranged on.From simple in structure and light
Source utilization ratio angle considers, in a kind of preferred embodiment of the application, successive reaction coil pipe coiling radiation source 20 is set.
03 more compact structure of continuous photochemical reaction unit set in this way, light utilization ratio higher.
Radiation source 20 in above-mentioned continuous photochemical reaction unit also slightly has not according to its specific kind of different structure
Together.In a kind of preferred embodiment of the application, internal irradiation light source includes：Center divergent light source 21 and light source cold-trap 22, light
Source cold-trap 22 is set around center divergent light source 21, and flow reactor 10 is set around light source cold-trap 22.Lead in light source cold-trap 22
It crosses and is passed through cooling medium, center divergent light source 21 can be avoided to generate heat the adverse effect to reaction.Certainly, when radiation source 20 is
During LED light, 22 structure of light source cold-trap can be saved, flow reactor 10 is directly surrounded and is arranged on outside LED light.
When selected radiation source need set light source cold-trap 22 when, due to light source cold-trap 22 effect when reduce center
Divergent light source 21 generates heat to photochemically reactive harmful effect, thus needs to be passed through cooling medium in light source cold-trap 22.In this Shen
Please be in a kind of preferred embodiment, light source cold-trap 22 includes cold-trap medium inlet 221 and cold-trap media outlet 222, cold-trap medium
Entrance 221 and cold-trap media outlet 222 are located around in the same level of center divergent light source 21 and are oppositely arranged, and set in this way
It is equipped with that the light source of different location is made to generate heat and can relatively evenly be cooled down, so that the different positions of flow reactor 10
The reaction condition put keeps relatively uniform stabilization, and so as to which reaction product is single, side reaction is few.
In above-mentioned continuous photochemical reaction unit, the structure and form of temperature regulating device 30 not particular determination, as long as can
Suitable reaction temperature condition is provided for continuous reaction device, suitable for the application.In a kind of preferred embodiment of the application
In, above-mentioned temperature regulating device 30 is reaction chuck, and flow reactor 10 and radiation source 20 are located in reaction chuck.By continuous
Reaction chuck outside reactor 10 is set, can be more convenient directly to regulate and control the temperature condition of continuous reaction device.
In above preferred embodiment, reacting needs to be passed through chuck medium in chuck to regulate and control the temperature of chuck, and then regulate and control
The temperature of continuous reaction device.In a kind of preferred embodiment of the application, reaction chuck includes chuck medium inlet 301 and folder
Cover media outlet 302.Specific chuck medium inlet 301 and the installation position of chuck media outlet 302 are unlimited, as long as can have
Effect carries out temperature control using medium in chuck.In this application, preferred jacket medium entrance is arranged on the lower part of chuck, chuck
Media outlet 302 is arranged on the top of chuck, can fully be changed with the material in flow reactor 10 by bottom in and top out
Heat, temperature control are efficient.
In another typical embodiment of the application, a kind of continuous photochemical reaction system is provided, such as Fig. 2 institutes
Show, which includes：Raw material device 01, continuous photochemical reaction unit 03 and light source controller 04,
Continuous photochemical reaction unit 03 is any of the above-described kind of continuous photochemical reaction unit 03, and continuous photochemical reaction unit 03 passes through
Raw material power conveying device 02 is connected with raw material device；The exposure light of light source controller 04 and continuous photochemical reaction unit 03
Source is connected and controls the light intensity of radiation source.The continuous photochemical reaction system, continuous high-efficient, compared with batch interval photochemical reaction
Stablize, side reaction is few, and the reaction time shortens, and temperature control is simple, easy to operate.It can connect and be operated in parallel.
Further illustrate the advantageous effect of the application below in conjunction with specific embodiments.
The reaction unit reacted using attached continuous photochemical reaction unit shown in FIG. 1 and existing batch is respectively under
Row spiral alkane carries out carbonylation, and specific reaction process is shown below, and the comparison result of two kinds of reactions is shown in Table 1.
Table 1：
As can be seen from Table 1, in terms of the reaction time, the light application time of batch reaction is not fixed, according to reactor
Depending on size, General reactions device is bigger, and the propagation of light in the reactor is more difficult, since the reaction time of batch reaction is to pass through
Light source irradiation time controls, thus luminous energy is weaker, causes the reaction time also longer.In upper table, 10g grades of batch reaction response
Time is 2~3h, and when the reaction for being amplified to 20L (1Kg) grade, reaction just needs could complete within 2~3 days.This is batch reaction
Enlarge-effect in terms of the reaction time.And continuous reaction technique：Since the illumination that all sites receive in reactor is equal
Uniformity.Even if reaction scale to be thus amplified to 1Kg grades from 10g grades, since the pipe diameter of reactor does not change, because
And enlarge-effect can almost be ignored.The reaction time of successive reaction is to control (pipeline by material flow and pipeline length
Volume is equal in the case that material flow is multiplied by residence time/reaction time of the material in pipeline so equipment determines, pipeline
Volume is certain, and the reaction time is inversely proportional with material flow, and flow velocity is fast, and the reaction time is short, otherwise flow velocity is slow, the reaction time
It is long), it after reaction scale expands, only need to extend duct length, accordingly accelerate the flow velocity of logistics, reaction time variation is little.
The data from upper table are it can also be seen that 10g grades of successive reactions, it is only necessary to and 5~10min can be completed, after being put into 20L, reaction
Time is still 5~10min, and there is no enlarge-effects.
In terms of reaction temperature, since batch reaction typical time is very long, side reaction can increase, it is therefore desirable to pass through control
Controlling reaction temperature side reaction quantity and rate processed.It is shown in upper table, the reaction temperature of batch reaction is -30~-20 DEG C.It puts
Greatly to after 20L, reaction temperature needs are further decreased to -40~-30 DEG C.And the reaction time of successive reaction is very short, it is anti-
Answer temperature that can carry out at room temperature.And without enlarge-effect.It is shown in upper table, the reaction of 10g and the reaction of 20L, reaction temperature
Degree is room temperature (20~30 DEG C).
It can be seen that continuous photochemical reaction unit provided herein, by setting flow reactor so that photochemical
Learning reaction can recur, and reaction raw materials continuously enter reactor, and reaction product continuously discharges reactor, this continuous flowing
Reaction can be effectively improved the transmission efficiency of light radiation in the reactive mixture, so as to shorten the reaction time, improve reaction effect
Rate reduces side reaction.Not only compared with batch stable reaction, and temperature control simple operations are convenient, conducive to photochemical reaction is made from laboratory
Scale is amplified to factory-level, enlarge-effect smaller.Thus propellane carbonylation, and energy are realized using continuous photochemical
It is enough suitably to carry out industrialization amplification.
In addition, continuous flowing reactive can effectively improve the transmission efficiency of light radiation in the reactive mixture, so as to contract
Short reaction time reduces side reaction.The dynamics of reaction can also be changed, so as to change the selectivity of reaction, and make reaction
Repeatability it is more preferable.Traditional batch reaction is substituted with continuous flowing reactive and carries out photochemical reaction, can mix reactant
It is more rapid, so as to reduce concentration gradient.Traditional batch reaction is substituted with continuous flowing reactive and carries out photochemical reaction, may be used also
So that heat exchange is more efficient, so as to reduce the probability of side reaction generation.
The above descriptions are merely preferred embodiments of the present invention, is not intended to limit the utility model, for this
For the technical staff in field, various modifications and changes may be made to the present invention.It is all in the spirit and principles of the utility model
Within, any modification, equivalent replacement, improvement and so on should be included within the scope of protection of this utility model.
Claims (9)
1. a kind of continuous photochemical reaction unit, which is characterized in that the continuous photochemical reaction unit includes：
Flow reactor (10)；
For carrying out the radiation source (20) of continuous photochemical reaction to the flow reactor (10) offer illumination；And
Temperature regulating device (30), the flow reactor (10) and the radiation source (20) are in the temperature regulating device (30)；
The radiation source (20) includes：
Center divergent light source (21)；And
Light source cold-trap (22), the light source cold-trap (22) are set around the center divergent light source (21)；
Wherein, the flow reactor (10) is set around the light source cold-trap (22).
2. continuous photochemical reaction unit according to claim 1, which is characterized in that the radiation source (20) is interior spoke
Irradiation source, the flow reactor (10) is around the interior radiating light source setting.
3. continuous photochemical reaction unit according to claim 1, which is characterized in that the radiation source (20) is mercury lamp
Or LED light.
4. continuous photochemical reaction unit according to claim 1, which is characterized in that the flow reactor (10) is connects
Continuous reaction coil pipe.
5. continuous photochemical reaction unit according to claim 4, which is characterized in that the successive reaction coil pipe coils institute
State radiation source (20) setting.
6. continuous photochemical reaction unit according to claim 1, which is characterized in that the light source cold-trap (22) is including cold
Trap medium inlet (221) and cold-trap media outlet (222), the cold-trap medium inlet (221) and cold-trap media outlet (222) position
In around the center divergent light source (21) same level on and be oppositely arranged.
7. continuous photochemical reaction unit according to any one of claim 1 to 6, which is characterized in that the temperature control dress
(30) are put to react in chuck positioned at described for reaction chuck, the flow reactor (10) and the radiation source (20).
8. continuous photochemical reaction unit according to claim 7, which is characterized in that the reaction chuck is situated between including chuck
Matter entrance (301) and chuck media outlet (302).
9. a kind of continuous photochemical reaction system, which is characterized in that the continuous photochemical reaction system includes：
Raw material device (01)；
Continuous photochemical reaction unit (03), the continuous photochemical reaction unit (03) are any one of claim 1 to 8 institute
The continuous photochemical reaction unit stated, the continuous photochemical reaction unit (03) pass through raw material power conveying device (02) and institute
Raw material device (01) is stated to be connected,
Light source controller (04), the radiation source of the light source controller (04) and the continuous photochemical reaction unit (03)
(20) it is connected and controls the light intensity of the radiation source (20).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486115A (en) * | 2017-08-04 | 2017-12-19 | 凯莱英医药化学（阜新）技术有限公司 | The continuous preparation method of continuous photochemical reaction unit, system and propellane carbonylation |
| CN109111460A (en) * | 2018-09-18 | 2019-01-01 | 许博 | A kind of cyclobutanetetracarboxylic dianhydride preparation facilities |
| CN110354778A (en) * | 2019-08-19 | 2019-10-22 | 江苏集萃分子工程研究院有限公司 | A kind of continuous Photoreactor of novel multi-pass amount and its system |
-
2017
- 2017-08-04 CN CN201720973262.5U patent/CN207493676U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486115A (en) * | 2017-08-04 | 2017-12-19 | 凯莱英医药化学（阜新）技术有限公司 | The continuous preparation method of continuous photochemical reaction unit, system and propellane carbonylation |
| CN109111460A (en) * | 2018-09-18 | 2019-01-01 | 许博 | A kind of cyclobutanetetracarboxylic dianhydride preparation facilities |
| CN109111460B (en) * | 2018-09-18 | 2021-04-30 | 山东德晨能源科技有限公司 | Preparation device of cyclobutane tetracarboxylic dianhydride |
| CN110354778A (en) * | 2019-08-19 | 2019-10-22 | 江苏集萃分子工程研究院有限公司 | A kind of continuous Photoreactor of novel multi-pass amount and its system |
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