CN220496337U - Photooxidation reaction and fractionation device - Google Patents
Photooxidation reaction and fractionation device Download PDFInfo
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- CN220496337U CN220496337U CN202321777748.3U CN202321777748U CN220496337U CN 220496337 U CN220496337 U CN 220496337U CN 202321777748 U CN202321777748 U CN 202321777748U CN 220496337 U CN220496337 U CN 220496337U
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- 238000007539 photo-oxidation reaction Methods 0.000 title claims abstract description 103
- 238000005194 fractionation Methods 0.000 title claims abstract description 38
- 239000012190 activator Substances 0.000 claims abstract description 41
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000460 chlorine Substances 0.000 claims abstract description 40
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 39
- 239000001301 oxygen Substances 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000003780 insertion Methods 0.000 claims abstract description 20
- 230000037431 insertion Effects 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 230000005587 bubbling Effects 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 27
- 239000006227 byproduct Substances 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000012071 phase Substances 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 6
- PNQBEPDZQUOCNY-UHFFFAOYSA-N trifluoroacetyl chloride Chemical compound FC(F)(F)C(Cl)=O PNQBEPDZQUOCNY-UHFFFAOYSA-N 0.000 description 6
- AZPWOLJQERBBBM-UHFFFAOYSA-N 2-chloro-2,2-difluoroacetyl chloride Chemical compound FC(F)(Cl)C(Cl)=O AZPWOLJQERBBBM-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000003213 activating effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000002186 photoactivation Effects 0.000 description 3
- OHMHBGPWCHTMQE-UHFFFAOYSA-N 2,2-dichloro-1,1,1-trifluoroethane Chemical compound FC(F)(F)C(Cl)Cl OHMHBGPWCHTMQE-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000003504 photosensitizing agent Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- QAEDZJGFFMLHHQ-UHFFFAOYSA-N trifluoroacetic anhydride Chemical compound FC(F)(F)C(=O)OC(=O)C(F)(F)F QAEDZJGFFMLHHQ-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The utility model discloses a photooxidation reaction and fractionation device, which comprises a photooxidation reaction component and a fractionation component which are connected through pipelines, wherein the photooxidation reaction component comprises a photooxidation reactor, a chlorine activator and an oxygen activator which are connected through pipelines in sequence, the oxygen activator is connected with the bottom end of the photooxidation reactor through an oxygen insertion type bubbling pipe, the side part of the photooxidation reactor is connected with a chlorine insertion pipe, the chlorine insertion pipe is connected with the chlorine activator, the top of the photooxidation reactor is provided with a reactor outlet, and the reactor outlet is connected with the fractionation component; the chlorine activator and the oxygen activator are externally connected with a wavelength-adjustable light source; the fractionating assembly comprises a condenser, a fractionating tower assembly with a condenser and a tower kettle, a liquid sealing device and a recycling tower assembly with the condenser and a reboiler, which are sequentially connected through pipelines, and the condenser is connected with an outlet of the reactor. The device avoids a great amount of byproducts generated by single light source adopted in the mixed feeding of the traditional photooxidation reactor, directly improves the conversion rate, and further improves the production efficiency.
Description
Technical Field
The utility model relates to the technical field of photooxidation reaction, in particular to a photooxidation reaction and fractionation device.
Background
The photooxidation reactor is widely applied in chemical production, and trifluoroacetyl chloride and chlorodifluoroacetyl chloride are important raw materials of fluorine-containing medicines, pesticides and lithium battery additives, so that the market is paying more attention to, and the traditional production process is to obtain trifluoroacetyl chloride and chlorodifluoroacetyl chloride by oxidizing R113a and R112a respectively with sulfur trioxide in a mercury catalyst and the like, and simultaneously generate a large amount of intractable sulfuryl chloride waste, so that the clean production process for producing trifluoroacetyl chloride and chlorodifluoroacetyl chloride by photooxidation with R123 and R122 is expected by the market.
The publication US5259938A discloses the preparation of TFAC by liquid phase oxidation of HCFC-123, which improves the selectivity of the reaction by filtering out the part of the light source having a wavelength less than 280nm, while avoiding the corrosion problem of the glass reactor, requiring liquid phase material to fill the whole reactor, without buffering the gas phase space in the reactor, which is unsafe in industrial production.
The publication No. US5296640 discloses that TFAC is prepared by oxidizing HCFC-123 in a supercritical state, hydrofluoric acid and TFAA are produced as byproducts in the reaction, and the high temperature and high pressure in the supercritical state are harsh to the reactor, so that the preparation is difficult to realize industrially.
In view of the prior art, the production device disclosed by the utility model is safe and reliable, utilizes different chemical bond energy conditions to select different light sources to activate free radicals to participate in the reaction, can reduce the intervention of photosensitizer chlorine to reduce byproducts, not only plays the role of cleaning photooxidation reaction, but also avoids generating a large amount of byproducts, and has great significance.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the utility model provides a photooxidation reaction and fractionation device and a process to solve the technical problems.
Technical proposal
In order to solve the technical problems, the utility model adopts the following specific technical scheme: the photooxidation reaction and fractionation device comprises a photooxidation reaction component and a fractionation component which are connected through pipelines, wherein the photooxidation reaction component comprises a photooxidation reactor, a chlorine activator and an oxygen activator which are sequentially connected through pipelines, the oxygen activator is connected with the bottom end of the photooxidation reactor through an oxygen insertion bubbling pipe, the side part of the photooxidation reactor is connected with a chlorine insertion pipe, the chlorine insertion pipe is connected with the chlorine activator, the top of the photooxidation reactor is provided with a reactor outlet, and the reactor outlet is connected with the fractionation component; the chlorine activator and the oxygen activator are externally connected with a wavelength-adjustable light source; the fractionating assembly comprises a condenser, a fractionating tower assembly with a condenser and a tower kettle, a liquid sealing device and a recycling tower assembly with a condenser and a reboiler, which are sequentially connected through pipelines, and the condenser is connected with an outlet of the reactor.
The device can be used as a reaction and fractionation device for synthesizing trifluoroacetyl chloride and chlorodifluoroacetyl chloride by photooxidation, can realize photooxidation reaction and fractionation, and simultaneously, the chlorine activator and the oxygen activator can regulate proper wavelength through the wavelength-adjustable light source to perform the photoactivation of chlorine and oxygen, so as to realize the factor of activating free radicals according to different substances, activate different reactants by adopting different wavelength light rays to generate the free radicals to enter a reactor for reaction, avoid the generation of a large number of byproducts caused by single light source in the mixed feeding of the traditional photooxidation reactor, directly improve the conversion rate and further improve the production efficiency.
Preferably, the light sources are necessary conditions for photooxidation reaction, the wavelength, the number and the arrangement mode of the light sources have great influence on the reaction, and a plurality of light sources are uniformly distributed at intervals in the photooxidation reactor, the light sources are uniformly distributed in a crossed manner, and the wavelength of the light sources is 330-360nm, so that the photooxidation reaction is most suitable.
Preferably, the uniform mixing of materials plays a vital role in improving the reaction efficiency and the completeness, and because the top end inside the photooxidation reactor is connected with a liquid distributor, the top end inside the photooxidation reactor is connected with a gas distributor, and because liquid and gas interfaces exist inside the photooxidation reactor during the reaction, the bottom of the photooxidation reactor is in a liquid phase, and the top is in a gas phase, the liquid distributor is arranged at the bottom end inside the photooxidation reactor, and the gas distributor is arranged at the top end inside the photooxidation reactor.
Preferably, the fractionating tower component with the condenser and the tower kettle comprises a fractionating tower condenser and a tower kettle fractionating tower, wherein the condenser is connected to the middle lower part of the tower kettle fractionating tower, and the fractionating tower condenser is positioned at the middle upper part of the tower body of the tower kettle fractionating tower.
Preferably, the bottom end of the fractionating tower component with the condenser and the tower kettle is connected with the bottom interface of the photooxidation reactor at the bottom end of the photooxidation reactor through a circulating spray pump to form fractionating circulation, components at all positions are dynamically balanced through the fractionating circulation, and meanwhile, reaction temperature is controlled within a smaller temperature range by utilizing evaporation and circulating spraying of reaction raw materials, so that the problem that a cooling system is required to be arranged inside and outside the reactor due to too much heat release of the traditional photooxidation reactor is avoided, the production amount of byproducts due to high temperature is reduced, and efficient continuous operation is achieved.
Preferably, the recovery tower component with the condenser and the reboiler comprises a recovery tower condenser, a reboiler and a recovery tower, wherein the recovery condenser is arranged at the top of the recovery tower, the reboiler is arranged at the bottom of the recovery tower, the recovery tower is connected with the liquid seal device, and the recovery tower condenser is connected with the fractionation tower component with the condenser and the tower kettle.
Preferably, the circulating spray pump is connected with a main raw material inlet at the top of the photooxidation reactor.
Preferably, the liquid seal device and the recovery tower component with condenser and reboiler are connected through a gas phase balance pipe.
Preferably, the fractionating tower component with the condenser and the tower kettle are connected with the liquid sealing device through a gas phase balance pipe.
Advantageous effects
Compared with the prior art, the utility model has the following beneficial effects:
1. the device can realize photooxidation reaction and fractionation, and simultaneously, the chlorine activator and the oxygen activator can adjust proper wavelength through the wavelength-adjustable light source to perform the photoactivation of chlorine and oxygen, so that the element of activating free radicals according to different substances is realized, different reactants are activated by adopting different wavelength light rays to generate free radicals to enter the reactor to perform reaction, a great amount of byproducts generated by single light source in the mixed feeding of the traditional photooxidation reactor are avoided, the conversion rate is directly improved, and the production efficiency is further improved;
2. the device is provided with a plurality of light sources which are uniformly distributed at intervals in the photooxidation reactor, the light sources are uniformly distributed in a crossed manner, and the wavelength of the light sources is 330-360nm, so that the photooxidation reaction conversion rate is improved;
3. the bottom end of the fractional tower component with the condenser and the tower kettle of the device is connected with the bottom interface of the photooxidation reactor at the bottom end of the oxidation reactor through the circulating spray pump to form fractional circulation, components at all positions are dynamically balanced through fractional circulation, and meanwhile, reaction temperature is controlled within a smaller temperature range by utilizing evaporation and circulating spray of reaction raw materials, so that the condition that the traditional photooxidation reactor needs to be internally and externally provided with a cooling system due to too much heat release is avoided, the production amount of byproducts due to high temperature is reduced, and efficient continuous operation is achieved.
Drawings
FIG. 1 is a schematic illustration of the process flow of the present photooxidation and fractionation apparatus;
FIG. 2 is a cross-sectional view of a photooxidation reactor of the present photooxidation reaction and fractionation apparatus;
FIG. 3 is a horizontal cross-sectional view of the light source arrangement inside the photooxidation reactor of the present photooxidation reaction and fractionation apparatus.
In the figure:
1. a recovery tower assembly with a condenser and a reboiler; 2. a liquid sealing device; 3. a fractionating tower component with a condenser and a tower kettle; 4. a circulating spray pump; 5. a condenser; 6. a photooxidation reactor; 7 a chlorine activator; 8. an oxygen activator; 9. a main raw material inlet; 10. a light source; 11. an oxygen insertion type bubbling tube; 12. a chlorine gas insertion tube; 13. a liquid insertion tube; 14. a gas distributor; 15. a liquid distributor; 16. an outlet of the reactor; 17. and a bottom interface of the photooxidation reactor.
Detailed Description
The utility model provides a photooxidation reaction and fractionation device, as shown in figure 1, comprising a photooxidation reaction component and a fractionation component which are sequentially connected through pipelines, wherein the photooxidation reaction component comprises a photooxidation reactor 6, a chlorine activator 7 and an oxygen activator 8 which are sequentially connected through pipelines, the oxygen activator 8 is connected with the bottom end of the photooxidation reactor 6 through an oxygen insertion bubbling pipe 11, the side part of the photooxidation reactor 6 is connected with a chlorine insertion pipe 12, the chlorine insertion pipe 12 is connected with the chlorine activator 7, the top of the photooxidation reactor 6 is provided with a reactor outlet 16, and the reactor outlet 16 is connected with the fractionation component; the chlorine activator 7 and the oxygen activator 8 are externally connected with a wavelength-adjustable light source; the fractionating assembly comprises a condenser 5, a fractionating tower assembly 3 with a condenser and a tower kettle, a liquid sealing device 2 and a recycling tower assembly 1 with a condenser and a reboiler, which are sequentially connected through pipelines, wherein the condenser 5 is connected with a reactor outlet 16. The device can realize photooxidation reaction and fractionation, and meanwhile, the chlorine activator 7 and the oxygen activator 8 can adjust proper wavelength through the wavelength-adjustable light source to perform the photoactivation of chlorine and oxygen, so that the element of activating free radicals according to different substances is realized, different reactants are activated by adopting different wavelength light rays to generate free radicals to enter the reactor to perform reaction, a great amount of byproducts generated by single light source are avoided in the mixed feeding of the traditional photooxidation reactor, the conversion rate is directly improved, and the production efficiency is further improved.
The production of trifluoroacetyl chloride and the byproduct R113a by photooxidation of R123, the same photooxidation of R122 can produce chlorodifluoroacetyl chloride and by-product R112a, and the three parts of a reaction process, a reaction part and a separation part are introduced, and the production of trifluoroacetyl chloride is taken as an example.
The reaction process is as follows:
activating oxygen
Activated chlorine
Photosensitizers
Main reaction
Side reactions
The device comprises a photooxidation reaction component and a fractionation component which are sequentially connected through pipelines, wherein the photooxidation reaction component is used for realizing the reaction part, the photooxidation reaction component comprises a photooxidation reactor 6, a chlorine activator 7 and an oxygen activator 8 which are sequentially connected through pipelines, the oxygen activator 8 is connected with the bottom end of the photooxidation reactor 6 through an oxygen insertion type bubbling pipe 11, the side part of the photooxidation reactor 6 is connected with a chlorine insertion pipe 12, the chlorine insertion pipe 12 is connected with the chlorine activator 7, a plurality of light sources 10 are uniformly distributed at intervals inside the photooxidation reactor 6, the wavelength of the light sources 10 is 330-360nm, a reactor outlet 16 is arranged at the top of the photooxidation reactor 6, and the reactor outlet 16 is connected with the fractionation component; the chlorine activator 7 and the oxygen activator 8 are externally connected with a wavelength-adjustable light source; the main raw material R123 is pumped in from a main raw material inlet 9, the corresponding wavelength light source is utilized to carry out light activation on oxygen and chlorine in an oxygen activator 8 and a chlorine activator 7, the wavelength of the selective activation oxygen is less than 330nm, the wavelength of the activation chlorine is more than 360nm, oxygen and chlorine containing active free radicals are generated, respectively, oxygen is bubbled into a liquid phase of a photooxidation reactor 6 from the bottom of the reactor through an oxygen insertion bubbling pipe 11 from the outlet of the oxygen activator 8, the chlorine enters the bottom of a gas phase part above the liquid phase of the photooxidation reactor 6 from the side of the reactor through a chlorine insertion pipe 12, the bottom end inside the photooxidation reactor 6 is connected with a liquid distributor 15, the top end inside the photooxidation reactor 6 is connected with a gas distributor 14, as shown in figure 3, the reactor is provided with a multi-layer light source 10, and R123 with the wavelength of 330-360nm in the photooxidation reactor 6 reacts to generate TFAC and HCl and simultaneously emits a large amount of heat, the bottom end of the fractionating tower component 3 with the condenser and the tower kettle is connected with the bottom interface 17 of the photooxidation reactor 6 through the circulating spray pump 4, the generated heat enables R123 in the reactor to further vaporize including circulating spray liquid, the temperature in the reactor is slightly higher than the boiling point of R123 due to the vaporization refrigeration of R123, the reaction products TFAC, HCl, vaporized R123, unreacted oxygen and chlorine, and a small amount of reaction byproducts R113a leave the reactor outlet 16 along with the R123 in the entrained form of reaction airflow and mist to enter the condenser 5, and the material condensed by the condenser 5 enters the tower body of the fractionating tower component 3 with the condenser and the tower kettle to enter the separation stage.
The fractionating assembly is used for realizing the fractionating part, and comprises a condenser 5, a fractionating tower assembly 3 with a condenser and a tower kettle, a liquid sealing device 2 and a recycling tower assembly 1 with a condenser and a reboiler, which are connected through pipelines in sequence, wherein the condenser 5 is connected with a reactor outlet 16. The fractionating tower component 3 with the condenser and the tower kettle comprises a fractionating tower condenser and a tower kettle fractionating tower, wherein the condenser 5 is connected to the middle lower part of the tower kettle fractionating tower, and the fractionating tower condenser is positioned at the middle upper part of the tower body of the tower kettle fractionating tower. The recovery tower component 1 with the condenser and the reboiler comprises a recovery tower condenser, a reboiler and a recovery tower, wherein the recovery condenser is arranged at the top of the recovery tower, the reboiler is arranged at the bottom of the recovery tower, the recovery tower is connected with the liquid seal device 2, and the recovery tower condenser is connected with the fractionation tower component 3 with the condenser and the tower kettle. The circulating spray pump 4 is connected with a main raw material inlet 9 at the top of the photooxidation reactor 6. The liquid seal device 2 and the recovery tower component 1 with the condenser and the reboiler are connected through a gas phase balance pipe. The fractionating tower component 3 with condenser and tower kettle is connected with the liquid sealing device 2 through a gas phase balance pipe.
As shown in fig. 2, the reactant product TFAC, HCl, R a and unreacted oxygen and chlorine gas including R123 flow out from the reactor outlet 16 of the photooxidation reactor 6, are cooled by the condenser 5 and then enter the middle lower part of the tower body of the combined condenser and tower kettle fractionating tower 3, and because the boiling point of TFAC, HCl, oxygen and chlorine gas is lower, the cooling of the tower top of the combined condenser and tower kettle fractionating tower 3 is not liquefied and flows out to the next process; the condensed R123-based and small amount of R113a flows into a tower kettle, the R123-based and small amount of R113a of the tower kettle is circularly acted by a liquid phase balance pipe or a circulating spray pump 4 at the bottom of the tower kettle to keep the liquid level of the photooxidation reactor 6 and the liquid level of the tower kettle on the same horizontal plane, part of materials at the tower kettle flow through a liquid seal device 2 through an overflow port to enter a tower body with a condenser and reboiler recovery tower combination 1, the reflux separation R113a is adopted from the bottom of the reboiler to enter the next procedure, and light components mainly comprising R123 and entrained in the tower top are adopted from the tower top to enter the tower body with the condenser and tower kettle fractionation tower combination 3 for re-separation.
In summary, the bottom end of the fractionating tower component 3 with the condenser and the tower kettle of the device is connected with the bottom interface 17 of the photooxidation reactor at the bottom end of the oxidation reactor 6 through the circulating spray pump 4 to form a fractionating cycle, components at all positions are dynamically balanced through the fractionating cycle, and meanwhile, the reaction temperature is controlled within a smaller temperature range by utilizing evaporation and circulating spray of reaction raw materials, so that the cooling system is not required to be arranged inside and outside the reactor due to too much heat release of the traditional photooxidation reactor, the production of byproducts due to high temperature is reduced, the efficient continuous operation is achieved, and the circulation and continuous operation can lead the components of the reactor and the tower kettle to be dynamically balanced.
It will be evident to those skilled in the art that the present utility model is not limited to the details of the foregoing illustrative embodiments, and that the present utility model may be embodied in other specific forms without departing from the spirit or scope of the utility model. Accordingly, the present embodiments are exemplary and non-limiting. The scope of the present utility model is defined by the appended claims rather than the foregoing description, and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. A photooxidation reaction and fractionation device is characterized by comprising a photooxidation reaction component and a fractionation component which are connected by a pipeline in sequence,
the photooxidation reaction assembly comprises a photooxidation reactor (6), a chlorine activator (7) and an oxygen activator (8) which are sequentially connected through pipelines, wherein the oxygen activator (8) is connected with the bottom end of the photooxidation reactor (6) through an oxygen insertion bubbling pipe (11), the side part of the photooxidation reactor (6) is connected with a chlorine insertion pipe (12), the chlorine insertion pipe (12) is connected with the chlorine activator (7), the top of the photooxidation reactor (6) is provided with a reactor outlet (16), and the reactor outlet (16) is connected with the fractionation assembly;
the chlorine activator (7) and the oxygen activator (8) are externally connected with a wavelength-adjustable light source;
the fractionating assembly comprises a condenser (5), a fractionating tower assembly (3) with a condenser and a tower kettle, a liquid sealing device (2) and a recycling tower assembly (1) with a condenser and a reboiler, which are sequentially connected through pipelines, wherein the condenser (5) is connected with a reactor outlet (16).
2. The photooxidation reaction and fractionation device according to claim 1, wherein a plurality of light sources (10) are uniformly arranged at intervals inside the photooxidation reactor (6), and the wavelength of the light sources (10) is 330-360nm.
3. The photooxidation reaction and fractionation device according to claim 1, wherein the bottom end inside the photooxidation reactor (6) is connected with a liquid distributor (15), and the top end inside the photooxidation reactor (6) is connected with a gas distributor (14).
4. The photooxidation reaction and fractionation apparatus according to claim 1, wherein the column assembly (3) with condenser and column bottom comprises a fractionating column condenser and a column bottom fractionating column, the condenser (5) is connected to a middle lower portion of the column bottom fractionating column, and the fractionating column condenser is located at a middle upper portion of a column body of the column bottom fractionating column.
5. The photooxidation reaction and fractionation device according to claim 1, wherein the bottom end of the fractionation tower assembly (3) with the condenser and the tower kettle is connected with a photooxidation reactor bottom interface (17) at the bottom end of the photooxidation reactor (6) through a circulating spray pump (4).
6. The photooxidation reaction and fractionation device according to claim 1, wherein the recovery tower assembly (1) with a condenser and a reboiler comprises a recovery tower condenser, a reboiler and a recovery tower, the recovery condenser is arranged at the top of the recovery tower, the reboiler is arranged at the bottom of the recovery tower, the recovery tower is connected with the liquid sealing device (2), and the recovery tower condenser is connected with the fractionation tower assembly (3) with the condenser and the tower kettle.
7. The photooxidation and fractionation apparatus according to claim 5, wherein the circulation shower pump (4) is connected to a main raw material inlet (9) at the top of the photooxidation reactor (6).
8. A photooxidation reaction and fractionation unit according to any one of claims 1 to 7, wherein the liquid seal unit (2) and the recovery column unit (1) with condenser and reboiler are connected by a gas phase balance pipe.
9. A photooxidation reaction and fractionation unit according to any one of claims 1 to 7, wherein the column unit (3) with condenser and column bottom and the liquid seal unit (2) are connected by a gas phase balance pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321777748.3U CN220496337U (en) | 2023-07-07 | 2023-07-07 | Photooxidation reaction and fractionation device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321777748.3U CN220496337U (en) | 2023-07-07 | 2023-07-07 | Photooxidation reaction and fractionation device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220496337U true CN220496337U (en) | 2024-02-20 |
Family
ID=89869473
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202321777748.3U Active CN220496337U (en) | 2023-07-07 | 2023-07-07 | Photooxidation reaction and fractionation device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220496337U (en) |
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2023
- 2023-07-07 CN CN202321777748.3U patent/CN220496337U/en active Active
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