CN220835474U - Two-stage oximation device - Google Patents
Two-stage oximation device Download PDFInfo
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- CN220835474U CN220835474U CN202322472602.4U CN202322472602U CN220835474U CN 220835474 U CN220835474 U CN 220835474U CN 202322472602 U CN202322472602 U CN 202322472602U CN 220835474 U CN220835474 U CN 220835474U
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- reaction kettle
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- oximation
- stage
- kettle
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- 238000006146 oximation reaction Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 130
- 238000003756 stirring Methods 0.000 claims abstract description 39
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 19
- 238000011010 flushing procedure Methods 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 12
- 238000007086 side reaction Methods 0.000 abstract description 6
- 230000036632 reaction speed Effects 0.000 abstract description 4
- 238000005192 partition Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 13
- 239000003054 catalyst Substances 0.000 description 11
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 8
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 230000004907 flux Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a two-stage oximation device which comprises a first reaction kettle and a second reaction kettle, wherein the first reaction kettle is provided with a first stirring device, the bottom of the first reaction kettle is provided with a raw material inlet, the top of the first reaction kettle is provided with a hydrogen peroxide adding port, the bottom of the first reaction kettle is connected with a mixer through a pipeline, the mixer is provided with an ammonia inlet, the mixer is connected with a heat exchanger through a pipeline, and the second reaction kettle is provided with a second stirring device. According to the two-stage oximation device, the temperature is controlled in a partition mode through the oximation reaction, so that the main reaction can be enabled to have a faster reaction speed at a higher temperature, most of the main reaction enters a low-temperature area after being completed, and the main reaction can be continued and can be effectively inhibited from generating side reactions.
Description
Technical Field
The utility model relates to the technical field of oximation devices, in particular to a two-stage oximation device.
Background
The ammoximation process adopts titanium-silicon molecular sieve as catalyst, cyclohexanone, ammonia and hydrogen peroxide as raw materials to react and generate cyclohexanone oxime, and tertiary butanol is adopted as solvent to ensure that the reaction is carried out in homogeneous phase. The cyclohexanone ammoximation reaction is a strongly exothermic reaction. In order to ensure that the reaction is carried out under the constant temperature condition, the reaction heat is removed in time in the process. The main influencing factors influencing the main and side reactions include catalyst performance, reaction temperature, reaction pressure, reaction material ratio, reaction time, catalyst concentration and the like.
In the prior art, the single kettle oximation is most commonly used, all reactants are added into the same kettle, and meanwhile, a filter element is arranged in the kettle, so that the reaction and the separation are carried out at the same time. Although the oximation reaction speed is high, a part of raw materials which are not reacted inevitably flows out of the kettle along with the filtered clear liquid. Because the effluent clear liquid does not contain catalyst, partial raw materials which do not complete the reaction do not react any more, thus reducing the reaction yield, reducing the product purity and increasing the separation cost.
Disclosure of utility model
The utility model aims to provide a two-stage oximation device, which realizes the zonal temperature control of oximation reaction, ensures that the main reaction can have a faster reaction speed at a higher temperature, and enters a low-temperature zone after the main reaction is mostly finished, so that the main reaction can be continuously carried out, the occurrence of side reactions can be effectively inhibited, the purity of products is improved, and the separation cost is reduced.
Embodiments of the present utility model are implemented as follows:
The embodiment of the utility model provides a two-stage oximation device which comprises a first reaction kettle and a second reaction kettle, wherein the first reaction kettle is provided with a first stirring device, the bottom of the first reaction kettle is provided with a raw material inlet, the top of the first reaction kettle is provided with a hydrogen peroxide adding port, the bottom of the first reaction kettle is connected with a mixer through a pipeline, the mixer is provided with an ammonia inlet, the mixer is connected with a heat exchanger through a pipeline, the second reaction kettle is provided with a second stirring device, the inlet of the second reaction kettle is connected with the overflow port of the first reaction kettle through a pipeline, the second reaction kettle is internally provided with a metal film pipe, the second reaction kettle is provided with a clear liquid discharge pipe, and the clear liquid discharge pipe is communicated with the metal film pipe.
Optionally, an ammonia gas inlet is arranged on the mixer. The ammonia concentration of the reaction liquid in the reaction kettle I can be improved by adding ammonia in advance, which is beneficial to the occurrence of main reaction.
Optionally, a back flushing pipe is arranged on the clear liquid discharge pipe, and the back flushing pipe is externally connected with a high-pressure back flushing liquid. The flux of the metal film tube can be recovered through the arrangement of the back flushing tube.
Optionally, an annular feeding distribution pipe is arranged at the bottom of the first reaction kettle, a plurality of small holes which are uniformly distributed are formed in the annular feeding distribution pipe, and the annular feeding distribution pipe is communicated with the raw material inlet. Through the arrangement of the annular feeding distribution pipes, the feeding can be ensured to be mixed with the materials in the kettle uniformly.
Optionally, the height of the overflow port of the first reaction kettle is higher than the feed port of the second reaction kettle, and the volume of the first reaction kettle is smaller than that of the second reaction kettle. Thus, the reaction liquid in the first reaction kettle can be ensured to naturally overflow into the second reaction kettle.
Optionally, the first stirring device has a power greater than that of the second stirring device, and the stirring modes of the first stirring device and the second stirring device are different. The stirring intensity of the stirring device I is higher, so that the mixing of reaction materials is facilitated, the stirring intensity of the stirring device II is properly reduced, and the protection of a powerful catalyst is realized.
Optionally, the heat exchanger is connected with a circulating pump through a pipeline, and the circulating pump is communicated with the second reaction kettle through a pipeline. The material liquid in the reaction kettle II can be circulated back into the reaction kettle I through the circulating pump.
The beneficial effects of the embodiment of the utility model include: the embodiment of the utility model provides a two-stage oximation device, which ensures that a main reaction can have a faster reaction speed at a higher temperature by realizing the partition temperature control of oximation reaction, and enters a low-temperature area after the main reaction is mostly finished, so that the main reaction can be continuously carried out and the occurrence of side reactions can be effectively inhibited;
Meanwhile, the first reaction kettle and the second reaction kettle respectively adopt different stirring types and stirring powers, so that the first reaction kettle is more rapid and uniform in stirring and mixing, the temperature gradient is smaller, and the reaction process is more favorably controlled; the second stirring of the reaction kettle is relatively mild, so that the damage to catalyst particles can be reduced, the main reaction can be enhanced, the side reaction can be inhibited, the reaction yield is higher, the impurities in the product are fewer, the product quality is better, and the cost of subsequent separation treatment is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present utility model and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram showing the overall structure of a two-stage oximation apparatus according to the present utility model.
Icon: 1. a first reaction kettle; 2. a first stirring device; 3. a raw material inlet; 4. a hydrogen peroxide adding port; 5. a mixer; 6. an ammonia gas inlet; 7. a heat exchanger; 8. a circulation pump; 9. a reaction kettle II; 10. a second stirring device; 11. a metal film tube; 12. a clear liquid discharge pipe; 13. and (5) back flushing the pipe.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present utility model more clear, the technical solutions of the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model. Thus, the following detailed description of the embodiments of the utility model, as presented in the figures, is not intended to limit the scope of the utility model, as claimed, but is merely representative of selected embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
In the description of the present utility model, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "vertical", "horizontal", "inner", "outer", etc., are directions or positional relationships based on those shown in the drawings, or those that are conventionally put in use of the inventive product, are merely for convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model. Furthermore, the terms "first," "second," "third," and the like are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal," "vertical," and the like do not denote a requirement that the component be absolutely horizontal or overhang, but rather may be slightly inclined. As "horizontal" merely means that its direction is more horizontal than "vertical", and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present utility model, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
As shown in fig. 1, the embodiment of the utility model provides a two-stage oximation device, which comprises a first reaction kettle 1 and a second reaction kettle 9, wherein a first stirring device 2 is arranged on the first reaction kettle 1, a raw material inlet 3 is arranged at the bottom of the first reaction kettle 1, a hydrogen peroxide adding port 4 is arranged at the top of the first reaction kettle 1, a mixer 5 is connected to the bottom of the first reaction kettle 1 through a pipeline, an ammonia inlet 6 is arranged on the mixer 5, a heat exchanger 7 is connected to the mixer 5 through a pipeline, a second stirring device 10 is arranged on the second reaction kettle 9, a feeding port of the second reaction kettle 9 is connected with an overflow port of the first reaction kettle 1 through a pipeline, a metal film pipe 11 is arranged in the second reaction kettle 9, a clear liquid discharge pipe 12 is arranged on the second reaction kettle 9, and the clear liquid discharge pipe 12 is communicated with the metal film pipe 11.
As shown in figure 1, the tertiary butanol solution of the cyclohexanone serving as a reaction raw material enters from a raw material inlet 3 at the bottom of a reaction kettle I1, is uniformly discharged through small holes provided with an annular feeding distribution pipe at the bottom of the reaction kettle I1, so that the feeding is ensured to be mixed with the materials in the reaction kettle I1 uniformly, hydrogen peroxide is added into the reaction kettle I1 from a hydrogen peroxide adding port 4 at the upper part of the reaction kettle I1 and mixed with the reaction raw material under the stirring of a stirring device I2, ammonia gas is fully mixed with the circulating materials carrying the catalyst and coming out of a reaction kettle II 9 in a mixer 5 through an ammonia gas inlet 6, enters from the bottom of the reaction kettle I1, and then each material is fully mixed and contacted under the stirring effect, so that the reaction can be rapidly carried out.
In this embodiment, as shown in fig. 1, an ammonia gas inlet 6 is provided in the mixer 5.
As shown in FIG. 1, the pre-addition of ammonia gas can increase the ammonia concentration of the reaction solution in the first reaction kettle 1, thereby being beneficial to the occurrence of main reaction.
In this embodiment, a back flushing pipe 13 is disposed on the clear liquid discharge pipe 12, and the back flushing pipe 13 is externally connected with a high-pressure back flushing liquid.
As shown in fig. 1, the flux of the metal film tube 11 can be recovered by the arrangement of the backwash tube 13.
In this embodiment, the bottom of the first reactor 1 is provided with an annular feeding distribution pipe, and a plurality of uniformly distributed small holes are formed in the annular feeding distribution pipe, and the annular feeding distribution pipe is communicated with the raw material inlet 3.
As shown in fig. 1, by arranging the annular feeding distribution pipe, the feeding can be ensured to be mixed with the materials in the kettle uniformly.
In this embodiment, as shown in fig. 1, the height of the overflow port of the first reaction kettle 1 is higher than the feed port of the second reaction kettle 9, and the volume of the first reaction kettle 1 is smaller than the second reaction kettle 9.
As shown in fig. 1, the reaction liquid in the first reaction kettle 1 can naturally overflow into the second reaction kettle 9.
In this embodiment, as shown in fig. 1, the first stirring device 2 has a higher power than the second stirring device 10, and the stirring modes are different.
As shown in fig. 1, the stirring intensity of the stirring device one 2 is higher, which is favorable for mixing reaction materials, and the stirring intensity of the stirring device two 10 is properly reduced, so that the protection of the catalyst is enhanced.
In this embodiment, as shown in fig. 1, the heat exchanger 7 is connected with a circulation pump 8 through a pipeline, and the circulation pump 8 is communicated with a second reaction kettle 9 through a pipeline.
As shown in fig. 1, the feed liquid in the second reaction vessel 9 can be circulated back to the first reaction vessel 1 by the circulation pump 8.
It should be noted that, when the two-stage oximation device is used, the tert-butyl alcohol solution of the reaction raw material cyclohexanone enters from the raw material inlet 3 at the bottom of the reaction kettle I1, and then is uniformly discharged through the small holes of the annular feeding distribution pipe arranged at the bottom of the reaction kettle I1, so that the feeding is ensured to be mixed uniformly with the amount of the materials in the reaction kettle I1, then hydrogen peroxide is added into the reaction kettle I1 from the hydrogen peroxide adding port 4 at the upper part of the reaction kettle I1, is mixed with the reaction raw material under the stirring of the stirring device I2, then ammonia gas is fully mixed with the circulating materials carrying the catalyst and coming out of the reaction kettle II 9 in the mixer 5 through the ammonia gas inlet 6, then the materials are fully mixed and contacted under the stirring action, the reaction is rapidly carried out, and most of the reaction is completed in the reaction kettle I1, and the reaction of the reaction kettle I1 is ensured to be higher than the feeding port of the reaction kettle II 9 due to the fact that the volume of the reaction kettle I1 is smaller than the reaction kettle II, and the arrangement position of the overflow port of the reaction kettle I is ensured, so that the reaction raw material naturally overflows into the reaction kettle II 9. The reaction kettle I controls the reaction temperature to be 90-120 ℃ and the reaction pressure to be 0.2-0.4 MPaG to ensure the reaction progress;
The oximation reaction is mostly completed in the first reaction kettle 1, and a small amount of unreacted residual raw materials in the second reaction kettle 9 continue to react, so that the temperature of the second reaction kettle 9 is controlled to be 70-100 ℃ lower than that of the first reaction kettle 1 in production, the occurrence of side reaction can be effectively inhibited while the completion of main reaction is ensured, the second reaction kettle 9 is more in charge of the task of separating feed liquid from catalyst, one or more layers of metal film pipes 11 are arranged in the second reaction kettle 9, the separation of the reacted materials from the oximation catalyst is completed through the built-in metal film pipes 11, the produced clear liquid is extracted and enters the subsequent process, and when the film flux is insufficient, the film flux can be recovered by back flushing the metal film pipes 11 through back flushing pipes 13.
The above is only a preferred embodiment of the present utility model, and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.
Claims (7)
1. The utility model provides a two-stage oximation device, includes reation kettle one (1) and reation kettle two (9), its characterized in that: be provided with agitating unit one (2) on reation kettle one (1), the bottom of reation kettle one (1) is provided with raw materials pan feeding mouth (3), the top of reation kettle one (1) is provided with hydrogen peroxide solution and adds mouth (4), there is blender (5) the bottom of reation kettle one (1) through the pipe connection, be provided with ammonia entry (6) on blender (5), there is heat exchanger (7) on blender (5) through the pipe connection, be provided with agitating unit two (10) on reation kettle two (9), pass through the pipe connection between the overflow mouth of feed inlet and reation kettle one (1) of reation kettle two (9), be provided with metal film tube (11) in reation kettle two (9), be provided with clear liquid discharge pipe (12) on reation kettle two (9), clear liquid discharge pipe (12) and metal film tube (11) intercommunication.
2. A two-stage oximation apparatus according to claim 1, wherein: an ammonia gas inlet (6) is arranged on the mixer (5).
3. A two-stage oximation apparatus according to claim 1, wherein: a back flushing pipe (13) is arranged on the clear liquid discharge pipe (12), and the back flushing pipe (13) is externally connected with high-pressure back flushing liquid.
4. A two-stage oximation apparatus according to claim 1, wherein: the bottom of the first reaction kettle (1) is provided with an annular feeding distribution pipe, a plurality of small holes which are uniformly distributed are formed in the annular feeding distribution pipe, and the annular feeding distribution pipe is communicated with a raw material inlet (3).
5. A two-stage oximation apparatus according to claim 1, wherein: the height of the overflow port of the first reaction kettle (1) is higher than that of the feed port of the second reaction kettle (9), and the volume of the first reaction kettle (1) is smaller than that of the second reaction kettle (9).
6. A two-stage oximation apparatus according to claim 1, wherein: the power of the stirring device I (2) is larger than that of the stirring device II (10), and the stirring modes of the stirring device I and the stirring device II are different.
7. A two-stage oximation apparatus according to claim 1, wherein: the heat exchanger (7) is connected with a circulating pump (8) through a pipeline, and the circulating pump (8) is communicated with a second reaction kettle (9) through a pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322472602.4U CN220835474U (en) | 2023-09-12 | 2023-09-12 | Two-stage oximation device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322472602.4U CN220835474U (en) | 2023-09-12 | 2023-09-12 | Two-stage oximation device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220835474U true CN220835474U (en) | 2024-04-26 |
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ID=90775358
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322472602.4U Active CN220835474U (en) | 2023-09-12 | 2023-09-12 | Two-stage oximation device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220835474U (en) |
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2023
- 2023-09-12 CN CN202322472602.4U patent/CN220835474U/en active Active
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