CN219849518U - Reaction device for Beckmann rearrangement - Google Patents
Reaction device for Beckmann rearrangement Download PDFInfo
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- CN219849518U CN219849518U CN202321328223.1U CN202321328223U CN219849518U CN 219849518 U CN219849518 U CN 219849518U CN 202321328223 U CN202321328223 U CN 202321328223U CN 219849518 U CN219849518 U CN 219849518U
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 69
- 238000006237 Beckmann rearrangement reaction Methods 0.000 title claims abstract description 21
- 238000003860 storage Methods 0.000 claims abstract description 72
- 230000003197 catalytic effect Effects 0.000 claims abstract description 66
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000005070 sampling Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 4
- 239000010963 304 stainless steel Substances 0.000 claims description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910000856 hastalloy Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 15
- 238000007599 discharging Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- SCRFXJBEIINMIC-UHFFFAOYSA-N n-cyclododecylidenehydroxylamine Chemical compound ON=C1CCCCCCCCCCC1 SCRFXJBEIINMIC-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006462 rearrangement reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The embodiment of the utility model provides a reaction device for Beckmann rearrangement, which comprises: a catalytic reactor in which a catalyst is disposed; the storage tank is used for storing materials and is connected with the catalytic reactor so that the materials in the storage tank are conveyed into the catalytic reactor for reaction and then returned to the storage tank; the product tank is connected with the storage tank, so that after the reaction is finished, the product in the storage tank is sent into the product tank; and the raw material tank is connected with the storage tank and is used for feeding new raw materials into the storage tank. The reaction device can continuously and stably run for a long time, and the working efficiency is improved. The catalyst can be regenerated in situ and recycled, filtering and recycling are not needed, and the cost is saved.
Description
Technical Field
The utility model relates to the field of catalytic reaction equipment, in particular to a continuous reaction device for solid-liquid reaction, which is particularly suitable for Beckmann rearrangement type reaction devices for preparing amide and the like from ketoxime.
Background
Batch operation is a common operation means in the organic chemistry industry, has the advantages of simple equipment requirement and flexible production organization, but has a plurality of defects compared with continuous production, such as: 1. the batch stability is poor, the conversion rate and the selectivity between different batches have large fluctuation, or the operation time is not constant; 2. the working efficiency is low, and after each batch of reaction is finished, repeated operations such as kettle cleaning, drying, feeding and the like are needed, so that the production efficiency is affected; 3. the amplification effect is obvious, and under the same operation condition, the difference between the results obtained by the small-sized reaction kettle and the large-sized production device is often larger.
At present, the material monomer laurolactam is mainly prepared by adopting cyclic ketoxime liquid-phase Beckmann rearrangement, generally adopting batch operation, using mineral acid such as fuming sulfuric acid/concentrated sulfuric acid as a catalyst, or using heterogeneous catalysts such as resin, molecular sieve and the like. The process has obvious disadvantages, for example, the viscosity of the system is obviously increased by the catalyst such as sulfuric acid, the reaction is uneven, and the resin and molecular sieve catalysts need to be filtered, centrifuged and the like to realize solid-liquid separation after the reaction is completed. The catalyst is easy to break and pulverize, so that a discharge hole and a pipeline of the reaction kettle are blocked, and the subsequent operation and the production progress are affected; in addition, intermittent operation presents safety hazards and potential health concerns for operators due to the presence of large amounts of organic solvents.
Disclosure of Invention
In view of the foregoing problems of the prior art, an object of an embodiment of the present utility model is to provide a reaction apparatus suitable for continuous production of amide by liquid-phase beckmann rearrangement of ketoxime.
The technical scheme adopted by the embodiment of the utility model is that the reaction device for Beckmann rearrangement comprises:
a catalytic reactor in which a catalyst is disposed;
the storage tank is used for storing materials and is connected with the catalytic reactor so that the materials in the storage tank are conveyed into the catalytic reactor for reaction and then returned to the storage tank;
the product tank is connected with the storage tank, so that after the reaction is finished, the product in the storage tank is sent into the product tank;
and the raw material tank is connected with the storage tank and is used for feeding new raw materials into the storage tank.
In an alternative embodiment, the catalytic reactor comprises a reactor main body, a distributor arranged in the reactor main body, and a separation net, wherein an inlet and an outlet are arranged on the reactor main body, the separation net divides the reactor main body into a feeding region communicated with the inlet, a discharging region communicated with the outlet, and a reaction region arranged between the feeding region and the discharging region, the distributor is respectively arranged in the feeding region and the discharging region, and is respectively close to the separation net, and the catalyst is arranged in the reaction region.
In an alternative embodiment, the reaction device comprises a plurality of catalytic reactors connected in series in sequence, wherein in two adjacent catalytic reactors, an outlet of the catalytic reactor positioned at the upstream is connected with an inlet of the catalytic reactor positioned at the downstream through a connecting pipeline, a material return pipeline is arranged on the connecting pipeline, and the material return pipeline is connected to a material inlet of the storage tank.
In an alternative embodiment, the catalytic reactor and the storage tank are respectively connected with a heat conduction oil furnace, and the heat conduction oil furnace respectively provides heating oil for the catalytic reactor and the storage tank so as to provide heat required by the reaction.
In an alternative embodiment, jackets are respectively arranged outside the catalytic reactor and the storage tank, an oil supply pipeline is arranged between an inlet and an outlet of the jackets, the heat conduction oil furnace is arranged on the oil supply pipeline, and a first pump for providing power for heat conduction oil flow is further arranged on the oil supply pipeline.
In an alternative embodiment, the storage tank comprises a storage tank main body, a feed inlet, a discharge outlet and a sampling port which are arranged on the storage tank main body, wherein the feed inlet of the storage tank is connected with the outlet of the catalytic reactor through a first pipeline, the feed inlet of the storage tank is also connected with the outlet of the raw material tank through a second pipeline, and the discharge outlet of the storage tank is connected with the inlet of the catalytic reactor through a third pipeline; the first pipeline is provided with a first valve, the second pipeline is provided with a second valve, and the third pipeline is provided with a third valve.
In an alternative embodiment, the third pipeline is provided with a second pump, the third pipeline is connected with a discharging pipeline, the connection part of the discharging pipeline and the third pipeline is positioned at the downstream of the second pump, and the discharging pipeline is connected to the product tank.
In an alternative embodiment, the connecting pipeline and the return pipeline are respectively provided with an insulating layer.
In an alternative embodiment, the materials of the catalytic reactor and the storage tank are any one of 304 stainless steel, 316L stainless steel, hastelloy, titanium material and glass lining respectively.
The catalyst for the Beckmann rearrangement reaction device provided by the embodiment of the utility model can be regenerated in situ and recycled, filtering and recycling are not needed, the cost is saved, the continuous and stable operation of the reaction device for a long time is ensured, and the working efficiency is improved.
The miniaturization of the reaction device is also suitable for evaluating the solid Beckmann rearrangement catalyst.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the utility model, as claimed.
An overview of various implementations or examples of the technology described in this disclosure is not a comprehensive disclosure of the full scope or all of the features of the technology disclosed.
Drawings
In the drawings, which are not necessarily drawn to scale, like numerals may describe similar components in different views. The accompanying drawings illustrate various embodiments by way of example in general and not by way of limitation, and together with the description and claims serve to explain the inventive embodiments. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts.
Fig. 1 is a schematic structural diagram of a reaction apparatus for beckmann rearrangement according to an embodiment of the present utility model.
Fig. 2 is a schematic structural view of a catalytic reactor according to an embodiment of the present utility model.
FIG. 3 is a schematic diagram of a series connection of catalytic reactors according to an embodiment of the present utility model.
Fig. 4 is a schematic structural view of a tank according to an embodiment of the present utility model.
Reference numerals:
1-a catalytic reactor; 11-a reactor body; 12-a distributor; 13-a screen; 14-inlet; 15-outlet; 16-a feed zone; 17-a discharge area; 18-reaction zone; 2-a storage tank; 21-a tank body; 22-a feed inlet; 23-a discharge hole; 24-sampling port; 25-level gauge; 26-thermometer; 27-jacket; 28-a first conduit; 29-a third conduit; 291-second pump; 3-a product tank; 31-a discharge pipeline; 4-a raw material tank; 41-a second conduit; 5-connecting pipelines; 51-a three-way valve; 6-a return pipeline; 7-a heat conduction oil furnace; 8-an oil supply pipeline; 81-first pump.
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 of the embodiments of the present utility model. It will be apparent that the described embodiments are some, but not all, embodiments of the utility model. All other embodiments, which can be made by a person skilled in the art without creative efforts, based on the described embodiments of the present utility model fall within the protection scope of the present utility model.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this utility model belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
In order to keep the following description of the embodiments of the present utility model clear and concise, the detailed description of known functions and known components thereof have been omitted.
As shown in fig. 1, an embodiment of the present utility model provides a reaction apparatus for beckmann rearrangement, which mainly includes a catalytic reactor 1, a storage tank 2, a product tank 3, and a raw material tank 4. The catalytic reactor 1 is internally provided with a catalyst. The storage tank 2 is used for storing materials, the storage tank 2 is connected with the catalytic reactor 1, so that the materials in the storage tank 2 are conveyed into the catalytic reactor 1 for reaction, and the materials are returned to the storage tank 2 after the reaction. The product tank 3 is connected with the storage tank 2, and after the reaction reaches the end point, the product in the storage tank 2 is sent into the product tank 3 by monitoring the composition change of the material in the storage tank 2. The raw material tank 4 is connected with the storage tank 2 for feeding new raw material into the storage tank 2.
In the reaction device of the embodiment of the utility model, firstly, the reaction materials in the storage tank 2 are conveyed into the catalytic reactor 1 filled with the catalyst for rearrangement reaction, and then returned into the storage tank 2; by monitoring the composition change of the materials in the storage tank 2 at fixed time, when the reaction reaches the end point, the product in the storage tank 2 is discharged to the product tank 3 to enter the subsequent refining working section, then the new materials in the raw material tank 4 are added into the storage tank 2, and the new materials added into the storage tank 2 start a new round of reaction, thereby realizing the continuous reaction process.
It will be appreciated that when the reaction reaches the end, only a portion of the product in the tank 2 may be discharged and fresh material may be added to the tank 2.
In an alternative embodiment, as shown in fig. 2, the catalytic reactor 1 comprises a reactor body 11, a distributor 12 provided within the reactor body 11, and a screen 13. The reactor body 11 is provided with an inlet 14 and an outlet 15. The partition net 13 divides the interior of the reactor body 11 into a feed region 16 communicated with the inlet 14, a discharge region 17 communicated with the outlet 15, and a reaction region 18 located between the feed region 16 and the discharge region 17, the distributors 12 are respectively located in the feed region 16 and the discharge region 17 and are respectively located close to the partition net 13, and the catalyst is disposed in the reaction region 18. The screen 13 can prevent catalyst leakage. The screen 13 may be a metal screen 13 and may be simultaneously matched with ceramic balls to prevent catalyst leakage.
The catalytic reactor 1 of this embodiment is rational in infrastructure, and the catalyst in the catalytic reactor 1 can reuse, need not to filter the recovery, saves cost, improves work efficiency, and the catalyst changes simply, does not have the problem of jam. Compared with the novel reactors such as a tubular reactor, a micro-channel reactor and the like, the reactor has the advantages of small pressure drop and large treatment capacity; compared with the traditional radial flow fixed bed reactor, the assembly is simpler and the combination is more flexible.
Further, as shown in fig. 3, the reaction apparatus includes a plurality of catalytic reactors 1 connected in series in turn, wherein, in two adjacent catalytic reactors 1, an outlet 15 of the catalytic reactor 1 located upstream is connected to an inlet 14 of the catalytic reactor 1 located downstream through a connecting pipe 5, a feed back pipe 6 is provided on the connecting pipe 5, and the feed back pipe 6 is connected to a feed inlet 22 of the storage tank 2 (it is understood that the feed back pipe 6 corresponds to the first pipe 28, or the feed back pipe 6 is connected to the first pipe 28). The reaction device can regulate the number, the size and the combination mode of the catalytic reactors 1 according to the production scale, namely, each catalytic reactor 1 can be singly used or combined in a series connection mode so as to achieve different purposes of increasing single treatment capacity, reducing cycle reaction time and the like, and has no amplification effect. The catalyst can be regenerated in situ, and the long-time stable operation of the reaction device is ensured; in practical applications, if a redundancy is designed, replacement of the catalyst without stopping can be achieved.
With continued reference to fig. 2, the reactor body 11 of each catalytic reactor 1 includes a body portion and top and bottom covers detachably mounted at both ends of the body portion. The main body part can be of a structure with square cross sections and two open ends, wherein the cross sections of the four sides are equal in side length, and the top cover and the bottom cover can be connected with the two ends of the main body part through bayonets respectively. Gasket rings are additionally arranged between the top cover and the main body part as well as between the bottom cover and the main body part to prevent leakage. The top cover is provided with an inlet 14, and the bottom cover is provided with an outlet 15.
In some embodiments, catalytic reactor 1 and storage tank 2 are each connected to a heat transfer oil furnace 7, and heat transfer oil furnace 7 provides heating oil to catalytic reactor 1 and storage tank 2, respectively, to provide the heat required for the reaction.
Specifically, the catalytic reactor 1 and the storage tank 2 are respectively provided with a jacket 27, and the medium in the jacket 27 is heat conduction oil. An oil supply pipeline 8 is arranged between the inlet 14 and the outlet 15 of the jacket 27, the heat conduction oil furnace 7 is arranged on the oil supply pipeline 8, and a first pump 81 for providing power for the heat conduction oil to flow is also arranged on the oil supply pipeline 8. In this way, each catalytic reactor 1 can be immersed in the heat transfer oil, ensuring the temperature required for the reaction. The storage tank 2 can keep the temperature of the materials by arranging the jacket 27.
The inlet 14 and the outlet 15 of the jacket 27 are provided with temperature monitoring points and sensors, respectively, inside the heat conducting oil tank for providing heat conducting oil to the heat conducting oil furnace 7, for controlling the temperature of the storage tank 2 and the catalytic reactor 1.
As shown in fig. 4, the storage tank 2 comprises a storage tank main body 21, a feed inlet 22, a discharge outlet 23 and a sampling port 24 which are arranged on the storage tank main body 21, wherein the feed inlet 22 of the storage tank 2 is connected with the outlet 15 of the catalytic reactor 1 through a first pipeline 28, the feed inlet 22 of the storage tank 2 is also connected with the outlet of the raw material tank 4 through a second pipeline 41, and the discharge outlet 23 of the storage tank 2 is connected with the inlet of the catalytic reactor 1 through a third pipeline 29; the first pipe 28 is provided with a first valve, the second pipe 41 is provided with a second valve, and the third pipe 29 is provided with a third valve. The structural design is reasonable, and the continuous stable operation of the reaction device is facilitated.
By designing the sampling port 24 on the tank 2, the change of the material in the tank 2 can be monitored at the sampling timing to determine whether the reaction reaches the end point. The liquid level meter 25 and the thermometer 26 are arranged on the storage tank 2 at the same time, so that the liquid level and the temperature in the storage tank 2 can be controlled, and the continuous and stable operation of the reaction is ensured.
As shown in fig. 1, a second pump 291 is provided on the third pipe 29, a discharge pipe 31 is connected to the third pipe 29, a junction of the discharge pipe 31 and the third pipe 29 is located downstream of the second pump 291, and the discharge pipe 31 is connected to the product tank 3. The flow of the material is thus powered so that the material in the tank 2 can enter the catalytic reactor 1 and also after the reaction has reached the end point, into the product tank 3.
The heat preservation layers are arranged on the pipelines of the reaction device to prevent materials from being cooled in the conveying process. Each pipe comprises a first pipe 28, a second pipe 41, a third pipe 29, a connecting pipe 5, a return pipe 6 and a discharge pipe 31.
The materials of the catalytic reactor 1 and the storage tank 2 are any one of 304 stainless steel, 316L stainless steel, hastelloy, titanium material and glass lining respectively. Glass lining is preferred.
The following will describe the application of the reaction apparatus of the present utility model to the preparation of laurolactam by Beckmann rearrangement of cyclododecanone oxime
In the first step, 50kg of catalyst was contained in each of the catalytic reactors 1, and a total of 200kg of catalyst was used in a manner that four catalytic reactors 1 (2+2) were connected in series. Before each reaction, 400kg of an acetonitrile solution of cyclododecanone oxime was added to the tank 2 via the feed tank 4, wherein 100kg of cyclododecanone oxime was contained and 300kg of acetonitrile was contained. The conduction oil furnace 7 is opened, the first pump 81 is started, the temperature in the storage tank 2 is set to be 70 ℃, the internal temperature of the catalytic reactors 1 is set to be 85-90 ℃, after the preset temperature is reached, the second pump 291 is started, the flow rate of the second pump 291 is set to be 200L/h, and the reaction is carried out only through the first two catalytic reactors 1 and the second two catalytic reactors 1 as a redundant design by regulating and controlling the three-way valve 51 on the connecting pipeline 5. After two hours of circulation, the reaction end point is reached through sampling analysis, a valve on a discharge pipeline 31 is opened, the product in the storage tank 2 is placed in a product tank 3, 400kg of material is added into the storage tank 2 again, and the next batch of circulation catalytic reaction is carried out. Typically, the catalyst life of the two catalytic reactors 1 is 8-10 cycles, and when a decrease in catalytic efficiency of the catalyst is detected, the materials are switched to the latter two catalytic reactors 1 to continue the reaction.
For the deactivated catalyst in the first two catalytic reactors 1, the in situ regeneration is carried out by the following method: firstly, the catalyst is washed by 100% acetonitrile, the flow rate is set to be 100L/hour, washing is carried out for 1-2 hours, then the catalyst is switched to acetonitrile solution containing 0.05% cobalt naphthenate for circulation, the catalyst is activated, the flow rate is set to be 50L/hour, the catalyst is continuously circulated for 4-6 hours, then the catalyst is washed by 100% acetonitrile, the flow rate is set to be 150L/hour, and washing is carried out for 1.0 hour, thus the catalyst regeneration is completed.
If the catalyst needs to be replaced, a batch replacement method can be adopted, and only the deactivated catalyst reactor is replaced.
The above description is intended to be illustrative and not limiting, and variations, modifications, alternatives, and variations of the above embodiments may be made by those of ordinary skill in the art within the scope of the present disclosure. Also, the above examples (or one or more aspects thereof) may be used in combination with each other, and it is contemplated that the embodiments may be combined with each other in various combinations or permutations.
Claims (9)
1. A reaction apparatus for beckmann rearrangement, comprising:
a catalytic reactor in which a catalyst is disposed;
the storage tank is used for storing materials and is connected with the catalytic reactor so that the materials in the storage tank are conveyed into the catalytic reactor for reaction and then returned to the storage tank;
the product tank is connected with the storage tank, so that after the reaction is finished, the product in the storage tank is sent into the product tank;
and the raw material tank is connected with the storage tank and is used for feeding new raw materials into the storage tank.
2. The reaction device for beckmann rearrangement according to claim 1, wherein the catalytic reactor comprises a reactor body, a distributor provided in the reactor body, and a screen provided on the reactor body, the screen dividing the reactor body into a feed region communicating with the inlet, a discharge region communicating with the outlet, and a reaction region between the feed region and the discharge region, the distributor being provided in the feed region and the discharge region, respectively, and being provided adjacent to the screen, respectively, and a catalyst being provided in the reaction region.
3. The reaction device for beckmann rearrangement according to claim 2, wherein the reaction device comprises a plurality of catalytic reactors connected in series in sequence, wherein the outlet of the catalytic reactor positioned at the upstream and the inlet of the catalytic reactor positioned at the downstream are connected through a connecting pipeline, a feed back pipeline is arranged on the connecting pipeline, and the feed back pipeline is connected to the feed inlet of the storage tank.
4. The reaction apparatus for beckmann rearrangement according to claim 1, wherein the catalytic reactor and the storage tank are respectively connected to a heat conducting oil furnace which provides heating oil for the catalytic reactor and the storage tank, respectively, to provide heat required for the reaction.
5. The reaction device for Beckmann rearrangement according to claim 4, wherein jackets are respectively arranged outside the catalytic reactor and the storage tank, an oil supply pipeline is arranged between an inlet and an outlet of the jackets, the heat conduction oil furnace is arranged on the oil supply pipeline, and a first pump for providing power for heat conduction oil flow is further arranged on the oil supply pipeline.
6. The reaction device for beckmann rearrangement according to claim 1, wherein the tank comprises a tank main body, a feed port, a discharge port and a sampling port which are provided on the tank main body, the feed port of the tank is connected with the outlet of the catalytic reactor through a first pipe, the feed port of the tank is also connected with the outlet of the raw material tank through a second pipe, and the discharge port of the tank is connected with the inlet of the catalytic reactor through a third pipe; the first pipeline is provided with a first valve, the second pipeline is provided with a second valve, and the third pipeline is provided with a third valve.
7. The reaction device for beckmann rearrangement of claim 6, wherein a second pump is provided on the third pipe, a discharge pipe is connected to the third pipe, the connection of the discharge pipe and the third pipe is located downstream of the second pump, and the discharge pipe is connected to the product tank.
8. A reaction device for beckmann rearrangement according to claim 3, wherein the connecting pipe and the return pipe are respectively provided with a heat insulating layer.
9. The reaction device for beckmann rearrangement according to claim 1, wherein the materials of the catalytic reactor and the storage tank are any one of 304 stainless steel, 316L stainless steel, hastelloy, titanium material and glass lining, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321328223.1U CN219849518U (en) | 2023-05-29 | 2023-05-29 | Reaction device for Beckmann rearrangement |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321328223.1U CN219849518U (en) | 2023-05-29 | 2023-05-29 | Reaction device for Beckmann rearrangement |
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| CN219849518U true CN219849518U (en) | 2023-10-20 |
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| CN202321328223.1U Active CN219849518U (en) | 2023-05-29 | 2023-05-29 | Reaction device for Beckmann rearrangement |
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