CN115591480A - Radial moving bed reactor and process for producing caprolactam - Google Patents

Radial moving bed reactor and process for producing caprolactam Download PDF

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Publication number
CN115591480A
CN115591480A CN202210805082.1A CN202210805082A CN115591480A CN 115591480 A CN115591480 A CN 115591480A CN 202210805082 A CN202210805082 A CN 202210805082A CN 115591480 A CN115591480 A CN 115591480A
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China
Prior art keywords
catalyst
reactor
heat
reaction zone
moving bed
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Chinese (zh)
Inventor
王皓
范瑛琦
罗一斌
谢丽
张晓昕
丁晖殿
李强
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Publication of CN115591480A publication Critical patent/CN115591480A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/082—Controlling processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087—Heating or cooling the reactor
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
    • C07D201/02—Preparation of lactams
    • C07D201/04—Preparation of lactams from or via oximes by Beckmann rearrangement

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention relates to a moving bed reactor, in particular to a radial moving bed reactor and a preparation method of caprolactam. The reactor comprises: the reactor comprises a reactor shell, a central pipe with a through hole, a catalyst bed layer and a material distributor, wherein the central pipe, the catalyst bed layer and the material distributor are arranged in the reactor shell from inside to outside; the heat collecting and separating device comprises a central pipe, a heat collecting and separating device and a heat collecting and separating device, wherein a plurality of heat collecting and separating devices which are vertically connected with the pipe wall of the central pipe are arranged at intervals along the circumferential direction of the central pipe; an upper ineffective reaction zone, an effective reaction zone and a lower ineffective reaction zone are arranged in the catalyst bed layer from top to bottom; wherein, the central tube is in the upper invalid reaction zone and the part of invalid reaction zone down does not have the through-hole, gets the upper portion of hot separator and sets up as the invalid portion that is in upper invalid reaction zone. The moving bed reactor disclosed by the invention has the advantages that the space utilization rate is improved, the problem of nonuniform axial distribution of airflow is effectively avoided, the reaction temperature is controlled, the moving bed reactor is used for a process for producing caprolactam by cyclohexanone oxime gas phase Beckmann rearrangement, the using amount of carrier gas can be reduced, and the reaction efficiency, the conversion rate and the selectivity are improved.

Description

Radial moving bed reactor and process for producing caprolactam
Technical Field
The invention relates to the technical field of radial moving bed reactors, in particular to a radial moving bed reactor and a preparation method of caprolactam.
Background
The moving bed reactor is a reactor for realizing fluid-solid phase contact, solid materials gradually move downwards in the reactor to the bottom by the action of gravity and are discharged, and fluid and solid materials are contacted and react. The moving bed reactor has the characteristics of both a fixed bed reactor and a fluidized bed reactor, and is particularly suitable for the reaction with moderate catalyst deactivation speed but still needing cyclic regeneration. The operating performance of the moving bed reactor and the requirements on the catalyst are between those of the fixed bed and the fluidized bed, and compared with the fixed bed, the moving bed reactor has the characteristics of small pressure drop and low investment; compared with a fluidized bed, the moving bed reactor has the advantages of small back mixing proportion, low pulverization degree of the catalyst, uniform distribution of reaction products, capability of changing the retention time of solids within a larger range, better flexibility and the like. Therefore, the moving bed reactor is widely applied to the fields of chemical processes such as catalytic reforming, gasoline desulfurization, heavy oil lightening and methanol conversion, treatment and recovery of wastes and the like.
The existing moving bed reactor can be divided into a downstream moving bed, a counter-current moving bed and a cross-flow moving bed according to the relative flow mode of solid materials and gas-phase materials, and researches show that the cross-flow moving bed can obtain a larger ventilation section, and meanwhile, channels of two phases can be separated, so that the moving bed reactor is more widely applied to industrial practice. In the gas-solid cross flow moving bed, a large flow rate is usually used to uniformly distribute the gas phase of the raw material in the catalyst bed layer, however, the large flow rate may cause the gas flow to be unevenly distributed in the axial direction of the reactor, and even cause short circuit.
In addition, the shortage of limited heat extraction in the cross-flow moving bed is always suffered from the problem, in order to solve the problem, most moving bed reactors adopt a multi-stage series and interstage heat exchange method (such as CN 102875469A) or a reactor external heat exchange method (such as CN 105218304A) for heat extraction, but the two methods can cause the space utilization rate of the reactor to be low, the equipment investment to be large and the operation to be complex.
In addition, in the moving bed reactor, because the deactivation time of different catalysts is different, the service life of the catalyst is as long as tens of hundreds of hours, and the service life of the catalyst is as short as several hours, so that the replacement frequency of the catalyst is greatly different; the former may be a batch type moving bed reactor, and the latter may be a continuous type moving bed reactor.
Disclosure of Invention
The invention aims to overcome the defects that the reaction effect is influenced by the uneven distribution of a catalyst along the axial direction of an air flow in a moving bed reactor in the prior art, and the reaction effect is influenced by the severe temperature rise caused by a large amount of exothermic heat in the reaction process, and provides a radial moving bed reactor and a preparation method of caprolactam.
In order to achieve the above object, a first aspect of the present invention provides a radial moving bed reactor, wherein the reactor comprises: the reactor comprises a reactor shell, and a central pipe, a catalyst bed layer and a material distributor which are arranged in the reactor shell from inside to outside and provided with through holes; the heat collecting and separating device comprises a central pipe, a heat collecting and separating device and a heat collecting and separating device, wherein a plurality of heat collecting and separating devices which are vertically connected with the pipe wall of the central pipe are arranged at intervals along the circumferential direction of the central pipe; an upper ineffective reaction zone, an effective reaction zone and a lower ineffective reaction zone are arranged in the catalyst bed layer from top to bottom; wherein the central pipe is provided with no through hole at the parts of the upper ineffective reaction area and the lower ineffective reaction area, and the upper part of the heat taking separator is arranged as an ineffective part in the upper ineffective reaction area.
In a second aspect, the present invention provides a process for producing caprolactam, the process comprising: introducing raw materials and a catalyst into a reactor respectively for reaction; the raw materials comprise cyclohexanone oxime, carrier gas and solvent; wherein the reactor is the moving bed reactor of the first aspect.
According to the technical scheme, on one hand, the radial moving bed reactor provided by the invention is provided with the plurality of heat-taking separators, so that a larger ventilation section can be obtained when a cross flow form is adopted, and the catalyst can be conveniently and fully contacted with reaction raw materials; and the reactor can be operated in a mode of lower pressure drop by adopting a cross flow mode; meanwhile, the service life cycle of the catalyst is matched in a moving mode, so that the long-period operation of a reaction system can be ensured; on the other hand, the heat-taking partition can also complete the heat exchange process in the reaction process, realize the stable temperature gradient in the bed layer, realize the heat exchange in the reactor, effectively stabilize the reaction temperature, solve the heat transfer problem commonly existing in the moving bed reactor and improve the reaction effect; in the third aspect, the catalyst discharge port comprises an inner ring group and an outer ring group, and the limited relationship can improve the flowing effect of the catalyst in the catalyst bed layer; the arrangement of the ineffective reaction zone ensures that the influence of the bed moving process on the reaction process is small.
Moreover, the space utilization rate of the whole reactor is improved, the problem of uneven axial distribution of airflow is effectively avoided, and the requirement of production load can be met; is particularly suitable for the process for producing caprolactam by the gas phase Beckmann rearrangement of cyclohexanone oxime.
The preparation method of caprolactam provided by the invention can reduce the using amount of carrier gas, improve the reaction efficiency and simultaneously improve the reaction conversion rate and the reaction selectivity.
Other advantages of the present invention will be described in detail in the following detailed description.
Drawings
FIG. 1 is a schematic structural view of one embodiment of a radial moving bed reactor of the present invention;
FIG. 2 is a schematic view of the structure of a central tube and heat-extracting partitions in a radial moving-bed reactor according to the present invention;
FIG. 3 shows the axial length h of the central tube in the radial moving bed reactor according to the invention 1 The total length H and the height H of the ineffective part of the heat-taking separating part 2 A graph relating to the total height L;
FIG. 4 is a sectional top view of the arrangement of the inner and outer ring sets of catalyst discharge ports in a radial moving bed reactor of the present invention.
Description of the reference numerals
1-reactor shell 2-catalyst bed 3-first material inlet and outlet
4-inlet and outlet of second material 5-central tube 6-heat-taking separator
7-catalyst conveying pipe 8-material distributor 9-through hole
101-catalyst inlet 102-catalyst outlet
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, in the case where no reverse explanation is made, the radial moving bed reactor is vertically arranged perpendicular to the horizontal plane, and the use of the directional words such as "upper, lower", "upper end, lower end", "top, bottom" generally means upper or lower based on the respective parts shown in the drawings, and also corresponds to upper or lower of the natural space; "inner and outer" refer to the inner and outer contours of the corresponding component (e.g., the inner and outer of the reactor shell or the inner and outer of the catalyst bed), and "from inner to outer" refers to the direction of extension from the center tube toward the reactor shell, merely for convenience and simplicity of description, and does not indicate or imply that the device or component being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the invention.
As mentioned above, the first aspect of the present invention provides a radial moving bed reactor, a preferred embodiment of which is shown in fig. 1 and 3, wherein the reactor comprises: the device comprises a reactor shell 1, and a central pipe 5, a catalyst bed layer 2 and a material distributor 8 which are arranged in the reactor shell 1 from inside to outside and provided with through holes 9; wherein, a plurality of heat-taking separators 6 vertically connected with the pipe wall of the central pipe 5 are arranged at intervals along the circumferential direction of the central pipe 5; an upper ineffective reaction zone, an effective reaction zone and a lower ineffective reaction zone are arranged in the catalyst bed layer 2 from top to bottom; wherein the central tube 5 has no through hole in the upper and lower ineffective reaction zones, and the upper part of the heat-taking partition 6 is provided as an ineffective part in the upper ineffective reaction zone.
The inventor researches and discovers that the moving bed reactor is compact in space and is not easy to add new parts, so that the temperature rise is difficult to effectively control in a mode of arranging a heat-taking or heat-absorbing inner component in the reactor for the reaction with strong heat release or strong heat absorption. In addition, the conventional radial reactor needs to accurately control the heat extraction process, fully considers the heat transfer properties built in the heat transfer, and influences of reaction kinetics on the heat transfer process, which increases the design difficulty. In addition, for a radial moving bed, uniform distribution of the fluid in the bed is an important concern in reactor design, and uniformity of the reactor bed is one of the design difficulties. According to the invention, through the arrangement of the heat-taking partition 6 in the upper ineffective reaction zone and the effective reaction zone of the catalyst bed layer 2 and the combination of the size limitation and the mutual relation of the central pipe 5 and the heat-taking partition 6 in the upper ineffective reaction zone, the flow and the uniform distribution of fluid can be facilitated, meanwhile, the heat exchange can be effectively carried out, the reaction temperature can be controlled, and the reaction effect can be improved.
In the present invention, the upper ineffective reaction zone and the lower ineffective reaction zone refer to the zones in the catalyst bed 2 where no reaction is performed. The upper ineffective reaction zone enables the catalyst entering from the top of the reactor shell 1 to be remixed and distributed through the zone and then enter the effective reaction zone of the catalyst bed layer 2 to contact with the catalyst for reaction; the lower inefficient reaction zone is used to buffer the deactivated catalyst and is discharged quantitatively.
It is to be understood that the catalyst bed 2 is arranged in a sandwich between the central tube 5 and the material distributor 8; the central tube 5 passes through the upper, active and lower inactive reaction zones of the catalyst bed 2. The through hole on the central tube 5 is used for materials to pass through, and the part with the through hole is positioned in the effective reaction area, so that the materials can circulate between the central tube 5 and the catalyst bed layer 2; the material distributor 8 is used for dispersing gas (carrying reaction raw materials) feeding, uniformly distributing the gas to the catalyst bed layer 2 along the radial direction, and the reacted gas passes through the catalyst bed layer 2, is collected to the central pipe 5 again and is sent out of the moving bed reactor through the outlet 4; or the material is fed through the central pipe 5, the gas is uniformly distributed to the catalyst bed layer 2 under the action of the material distributor 8, and the material passing through the material distributor 8 is sent out of the moving bed reactor through the outlet 3; the catalyst in the catalyst bed layer 2 moves from top to bottom by the action of gravity.
According to a preferred embodiment of the present invention, as shown in fig. 2, the heat extraction separator 6 is provided on the outer peripheral surface of the center pipe 5 and is formed in a plate shape extending in the axial direction of the center pipe 5.
According to the present invention, preferably, as shown in fig. 2, the heat-taking partition 6 is located within the catalyst bed 2; in the direction perpendicular to the axial direction of the central tube 5, the distance between two adjacent heat taking separators 6 is gradually increased from inside to outside; that is, a plurality of the heat separators 6 are radially distributed around the outer periphery of the center pipe 5. Therefore, the catalyst bed layer 2 can be distributed more uniformly, the space utilization rate of the reactor is improved, and meanwhile, effective heat exchange in the moving bed reactor is further facilitated, so that the reaction temperature can be controlled accurately.
In a preferred embodiment, the shortest distance between two adjacent heat-extraction partitions 6 is 6 times or more, more preferably 10 times or more, the average particle diameter of the catalyst particles packed in the catalyst bed 2. Under the preferred scheme, the heat extraction is more facilitated, and the catalyst flow is more facilitated.
In the present invention, there is no limitation on the catalyst particle size, and any conventional catalyst in the art may be used in the present invention, and for example, the particle size of the catalyst particles may be preferably 0.5mm or more, and more preferably 0.8 to 5mm.
In the present invention, it is preferable that a plurality of the heat extraction partitions 6 are provided in the direction extending along the diameter of the center pipe 5, and in this case, the cross section formed by adjacent two heat extraction partitions 6 is a sector. Further preferably, the plurality of heat-extracting partitions 6 are evenly spaced around the circumference of the central tube 5.
In the present invention, the heat extraction separator 6 achieves the heat extraction by heat exchange for controlling the temperature during the catalytic reaction, which can be achieved by any existing means; preferably, a channel for circulating a heat exchange medium is arranged in the heat taking partition 6. By adopting the preferred scheme of the invention, the reaction temperature can be more favorably and effectively controlled, and the heat transfer problem can be solved, so that the reaction in the catalyst bed layer 2 can be more stably and uniformly carried out. It is understood that the channels may be sealed, with a heat exchange medium previously disposed therein; the heat exchanger can also be an unsealed channel, and in this case, a person skilled in the art can also set a heat exchange medium inlet and a heat exchange medium outlet on the heat extraction separator 6 according to actual needs, and the heat exchange medium inlet and the heat exchange medium outlet are communicated with the channel.
Preferably, the heat extraction separator 6 is provided with a heat exchange medium inlet (not shown in the figure) and a heat exchange medium outlet (not shown in the figure), and the heat exchange medium inlet and the heat exchange medium outlet are respectively communicated with the channel for the circulation of the heat exchange medium.
More preferably, the heat exchange medium inlet and the heat exchange medium outlet are located at the top and bottom of the heat extraction partition 6, respectively. It should be understood that the heat medium may be taken up and out in this embodiment, or in a form of going up and out.
Preferably, the reactor further comprises a heat exchange line connected to the heat extraction partition 6, said heat exchange line being disposed above (preferably directly above) the heat extraction partition 6 and within the upper inactive reaction zone. In this preferred embodiment, the heat exchange lines do not affect the fluid flow within the catalyst bed 2.
It should be understood that the heat exchange pipeline can realize the heat exchange function of the heat extraction partition 6, and may specifically use any existing device and its matching pipeline, which is not limited by the present invention.
The heat exchange medium is not limited at all, and preferably, the heat exchange medium is molten salt, heat transfer oil or water. The molten salt is a heat-conducting molten salt, and may be at least one of melts of halides, nitrates and sulfates of alkali metals and alkaline earth metals, for example, a melt of sodium nitrate and/or potassium nitrate.
In one embodiment, the heat extraction separator 6 is a pair of plates. The pair of plates are a pair of plates in which heat exchange media can flow, and the plates are preferably pillow type heat exchange plates or plate type heat exchange plates.
In the invention, the fixing mode of the heat extraction separator 6 is not limited as long as the fluid in the catalyst bed layer 2 is favorably flowed and uniformly distributed; for example, the heat removal partition 6 is suspended within the catalyst bed 2 by the top. It is understood that a gap can be left between the heat extraction separator 6 and the catalyst bed 2 and the central pipe 5, and the skilled person can select the gap according to actual needs; for example, the gap is smaller than the particle size of the catalyst so that the catalyst does not get stuck in the gap and does not pass through the gap.
In a specific embodiment of the present invention, the arrangement of the central tube 5 and the heat extraction separator 6 in the upper ineffective reaction zone can be beneficial to improving the stability of the reaction system and exerting the technical effect of the catalyst. Preferably, as shown in fig. 3, the axial length h of the portion of the central tube 5 in the upper dead zone 1 And the total length H of the central tube 5 satisfies: h is 1 H.ltoreq.0.4, preferably H 1 The ratio of the/H to the total weight is less than or equal to 0.3. In the present invention, h 1 And H are both referred to in the vertical direction.
In one embodiment of the invention, the height h of the inactive portion of the heat extraction partition 6 is preferably perpendicular to the vertical direction 2 And the total height L of the heat-taking partition 6 satisfies the following conditions: h is 2 L.ltoreq.0.2, preferably h 2 L is less than or equal to 0.1. Wherein h is 2 And L are both referred to in the vertical direction.
In one embodiment of the present invention, preferably, the upper edge of the heat-removing partition 6 is higher than the lower edge of the part of the central tube 5 in the upper ineffective reaction zone in the vertical direction (as shown by the dotted line in fig. 3).
In one embodiment of the present invention, preferably, as shown in fig. 3, the through holes 9 are provided on the pipe wall of the central pipe 5 between two adjacent heat-extracting partitions 6. Preferably, the portion of the central tube 5 within the active reaction zone (as shown in the lower portion of the dashed line in fig. 3) has a varying porosity in the area responsible for the distribution of the flow. For example, the porosity decreases from top to bottom. Preferably, the open porosity varies from 1% to 15% from top to bottom along the central tube 5.
In one embodiment of the present invention, it is preferable that the ratio of the pore diameter of the through-holes to the diameter of the catalyst particles is not more than 1, and preferably not more than 0.8. I.e. the pore size of the through-holes is smaller than the catalyst particle diameter.
In a specific preferred embodiment, the radial moving bed reactor further comprises a plurality of catalyst discharge pipes 7 arranged in the reactor shell 1, wherein the plurality of catalyst discharge pipes 7 are positioned above the catalyst bed layer 2 and are distributed at intervals along the circumferential direction of the central pipe 5; for flowing catalyst into the catalyst bed 2. The number of catalyst offtake 7 can be freely chosen by the person skilled in the art according to the actual requirements.
The present invention limits the position of the material inlet and outlet (materials such as raw materials) of the radial moving bed reactor, so that the raw materials and the catalyst can contact and react in the catalyst bed layer 2. Preferably, as shown in fig. 1, the moving bed reactor further comprises: a catalyst inlet 101, a catalyst outlet 102, a first material inlet and outlet 3 and a second material inlet and outlet 4; the catalyst feeding hole 101 and the catalyst discharging hole 102 are communicated with the catalyst bed layer 2; the catalyst feeding hole 101 and the catalyst discharging hole 102 are respectively arranged at the upper end and the lower end of the reactor shell 1 and are used for introducing a catalyst into the catalyst bed layer 2 to react with a raw material and then leading out an inactivated catalyst after reaction; the second material inlet and outlet 4 is communicated with the central pipe 5, and the first material inlet and outlet 3 is communicated with the catalyst bed layer 2. The first material inlet and outlet 3 and the second material inlet and outlet 4 are preferably arranged on opposite sides of the reactor housing 1, respectively.
In the present invention, the first material inlet/outlet 3 and the second material inlet/outlet 4 refer to that each port can be used as an inlet or an outlet, for example, in one mode, the first material inlet/outlet 3 is an outlet, the second material inlet/outlet 4 is an inlet, and in another mode, the first material inlet/outlet 3 is an inlet, and the second material inlet/outlet 4 is an outlet.
In the present invention, the catalyst freely falls from the catalyst bed layer to the catalyst outlet 102 for discharging by its own weight, and those skilled in the art can further add a collector to facilitate better discharging, and the collector can adopt any existing device for collecting materials, and the present invention has no limitation to this. The catalyst outlet 102 is provided with a valve for continuous or intermittent discharge. Generally, in view of catalyst deactivation, the skilled person usually uses a continuous discharge to discharge the deactivated catalyst, and the discharge amount can be selected by the skilled person according to actual requirements.
In one embodiment of the present invention, as shown in fig. 4, preferably, the catalyst outlet 102 includes: a plurality of openings arranged annularly along the circumferential direction of the reactor shell 1. I.e. the openings are arranged around the central axis of the reactor shell 1 and distributed to form a circular ring.
In one embodiment of the present invention, the plurality of openings are preferably divided into an inner ring group and an outer ring group, wherein the inner ring group is disposed below the central tube 5, and the outer ring group is disposed below the material distributor 8.
In the present invention, the plurality of openings included in the inner ring group and the outer ring group may be annularly disposed at equal intervals along the circumferential direction of the reactor shell 1. The diameter of the plurality of openings may be the same, and the diameter of the openings may be set to be 15 to 50 times the diameter of the catalyst particles. The number of openings comprised by each of the inner and outer ring sets can be adapted to the diameter of the reactor shell 1, ensuring that the catalyst removal according to the invention is fulfilled, as shown for example in fig. 4.
In one embodiment of the present invention, as shown in FIG. 4, (a) shows the case of the inner ring set and the center tube, and (b) shows the case of the outer ring set and the reactor shell. Preferably, the diameter d of a circle formed by the centers of the openings surrounded by the inner ring set 1 The diameter d of a circle formed by the centers of the openings surrounded by the outer ring group 2 Diameter D of the central tube 5 1 And the diameter D of the reactor shell 1 2 Satisfies the following conditions: d 1 -d 1 ≤0.3D 2 ，D 2 -d 2 ≤0.3D 2 (ii) a Preferably, D 1 -d 1 ≤0.15D 2 ，D 2 -d 2 ≤0.15D 2 。
In the radial moving bed reactor of the present invention, the feedstock may pass through the catalyst bed layer 2 in a centrifugal or centripetal manner. The centrifugal type is that raw materials enter the central tube 5, the catalyst bed layer 2 and the material distributor 8 in sequence by taking a second material inlet and outlet 4 as a feeding hole, and are moved out from a first material inlet and outlet 3; the centripetal type means that raw materials enter a material distributor 8, a catalyst bed layer 2 and a central pipe 5 in sequence by taking a first material inlet and outlet 3 as a feeding hole, and are moved out of the reactor from a second material inlet and outlet 4.
In one embodiment of the present invention, preferably, when the first material inlet/outlet 3 is filled with reaction raw materials and the second material inlet/outlet 4 is used for discharging products, each opening included in the inner ring group is closed, and each opening included in the outer ring group is open, so as to discharge the catalyst that is deactivated first outside the catalyst bed layer 2; or
When the second material inlet and outlet 4 is filled with reaction raw materials and the first material inlet and outlet 3 discharges products, the openings of the outer ring group are closed, and the openings of the inner ring group are open, so that the deactivated catalyst inside the catalyst bed layer 2 is discharged.
In the present invention, before the catalyst is discharged from the moving bed reactor, it is generally necessary to purge the catalyst, and an inert gas is preferably used as a purge medium.
In the present invention, preferably, the reactor housing 1 is not limited at all, and preferably, the reactor housing 1 has a cylindrical shape. In the present invention, the radial moving bed reactor is usually further provided with a temperature control component for controlling the reaction temperature of the reaction in the catalyst bed 2, a pressure regulating component for controlling the reaction pressure, and the like, which are not described herein again.
The invention has no limitation on the application object of the radial moving bed reactor, can be applied to any reaction process with strong heat absorption or strong heat release, and has small change to the reaction temperature gradient in the reaction process. In addition, the moving bed reactor of the present invention can be used for reactions requiring continuous catalyst withdrawal due to the limited catalyst single pass life. The moving bed reactor is particularly suitable for a process for producing caprolactam by gas-phase Beckmann rearrangement of cyclohexanone oxime, and reaction raw materials (comprising a mixture of cyclohexanone oxime, a carrier gas and a solvent) of the process enter the moving bed reactor in a gas phase. When in application, a plurality of moving bed reactors can be connected in parallel or in series by a person skilled in the art according to actual requirements, so that a plurality of catalyst bed layers can work together, and the treatment capacity is improved; preferably, the total number of moving bed reactors in parallel or in series is no more than 4.
When the radial moving bed reactor of the present invention is used, in a specific embodiment, as shown in fig. 1, raw materials enter from the first material inlet/outlet 3, pass through the material distributor 8, and then enter the catalyst bed layer 2; meanwhile, the catalyst is sent to an upper ineffective area of the catalyst bed layer 2 from the catalyst feed port 101 through a catalyst discharge pipe 7, and the heat-exchanged catalyst enters an effective reaction area of the catalyst bed layer 2 and flows from top to bottom by the self-gravity; meanwhile, a heat exchange medium flows through the heat extraction separator 6. The raw materials and the catalyst are catalytically reacted in an effective reaction zone of the catalyst bed layer 2. In the reaction process, the temperature of the reaction is controlled by controlling the heat exchange medium of the heat taking separator 6, so that the temperature gradient in the bed is stable. After the reaction is finished, the reactant is led out from the second material inlet and outlet 4 through the central pipe 5, and the deactivated catalyst is discharged from the catalyst discharge port 102 continuously or intermittently.
In the present invention, if the activity of the catalyst cannot meet the reaction requirement, the regenerated or fresh catalyst can be optionally introduced from the catalyst inlet 101, and the catalyst is removed from the catalyst outlet 102, and further removed from the openings of the inner ring group or the openings of the outer ring group corresponding to the above-mentioned different operations. When the moving bed reactor is used for preparing caprolactam, the activity life time of the rearrangement reaction catalyst is longer, and intermittent loading and unloading can be adopted.
In the invention, the heat exchange medium and the catalyst can form cross-flow mixing by controlling the flow direction of the heat exchange medium, and the heat exchange in the moving bed reactor can be realized in a cross-flow state.
The invention provides the radial moving bed reactor, the structural characteristics are cooperated to solve the problems that the catalyst in the moving bed reactor is not uniformly distributed along the axial direction of the airflow, and the temperature rise caused by a large amount of reaction heat release in the reaction process is severe, so that the reaction efficiency in the reactor can be effectively improved.
In a second aspect, the present invention provides a process for producing caprolactam, the process comprising: introducing raw materials and a catalyst into a reactor respectively for reaction; the raw materials comprise cyclohexanone oxime, carrier gas and solvent; wherein the reactor is the moving bed reactor of the first aspect.
In the present invention, preferably, a heat exchange medium is circulated in the heat extraction partition 6 in the moving bed reactor. The optional range of the heat exchange medium is the same as that of the heat exchange medium in the first aspect, and details are not repeated here.
Preferably, the vaporization rate of the heat exchange medium is not more than 30%. Under the preferred scheme, the bed temperature of the catalyst bed layer 2 is more uniform.
Preferably, the raw material passes through the catalyst bed layer 2 of the moving bed reactor in a centrifugal or centripetal manner. The eccentric or centripetal manner is as described above.
According to the present invention, preferably, the molar ratio of the carrier gas to the cyclohexanone oxime is 5-100:1, more preferably 5 to 50:1. the method of the invention can reduce the dosage of the carrier gas.
Preferably, the weight ratio of the solvent to the cyclohexanone oxime is 1-100:1, more preferably 1 to 20:1.
the carrier gas is not limited in the present invention, and preferably, the carrier gas is a protective gas, more preferably at least one of nitrogen, argon, a saturated hydrocarbon having a boiling point of not more than 180 ℃, and a halogenated hydrocarbon having a boiling point of not more than 180 ℃. The saturated hydrocarbon having a boiling point of not more than 180 ℃ may be, for example, at least one of methanol, ethanol, and propanol, and the halogenated hydrocarbon having a boiling point of not more than 180 ℃ may be, for example, at least one of 1-chloroethane, 1-chloropropane, and 1-chlorobutane.
The solvent is not limited in the present invention, and preferably, the solvent is an organic solvent, more preferably an aliphatic alcohol having 1 to 6 carbon atoms, and further preferably at least one of methanol, ethanol, and propanol.
According to the present invention, preferably, the reaction conditions include: the reaction temperature is 200-500 ℃, the reaction pressure is 0.1-1MPa, and the weight hourly space velocity of the cyclohexanone-oxime is 0.3-20h -1 More preferably 0.3 to 5 hours -1 。
According to a preferred embodiment of the invention, the method further comprises: the temperature rise of the reaction is controlled by the heat removal partition 6 to be not higher than 100 c, preferably not higher than 80 c, more preferably not higher than 60 c. More preferably, the reaction temperature is above 300 ℃. Specifically, the temperature rise of the reaction can be controlled by controlling the inlet temperature and the outlet temperature of the reaction raw materials of the reactor so that the reaction temperature is within the above range.
According to the present invention, preferably, the catalyst is a molecular sieve catalyst. The molecular sieve catalyst can be at least one of an all-silicon molecular sieve and a titanium-silicon molecular sieve. Granulating to obtain granules, and filling to form catalyst bed layer. The particle diameter of the agent particles may be preferably 0.5mm or more, and more preferably 0.8 to 5mm.
The method provided by the invention further controls the temperature condition in the moving bed reactor, and can be beneficial to effectively improving the reaction activity of the catalyst, reducing the removal amount of the catalyst and improving the reaction effect. In a preferred embodiment of the present invention, the average temperature T of the upper ineffective reaction zone in the moving bed reactor is preferably 1 (average of the maximum and minimum temperatures of the upper ineffective zone) and the minimum temperature T of the effective reaction zone min Satisfies the following conditions: t is a unit of min Satisfies the following conditions: t is min -T 1 Less than or equal to 50 ℃, preferably T min -T 1 ≤30℃。
In a preferred embodiment of the present invention, the average temperature T of the lower ineffective reaction zone in the moving bed reactor is preferably 2 (average of the highest and lowest temperatures of the lower dead zone) and T min Satisfies the following conditions: t is min -T 2 ≤80℃。
According to the caprolactam preparation method provided by the invention, the radial moving bed reactor is used and the condition characteristics are combined for limitation, so that the reduction of the carrier gas consumption can be realized synergistically, the reaction efficiency is improved, and the reaction conversion rate and the reaction selectivity are improved.
The present invention will be described in detail below by way of examples. Wherein the content of the first and second substances,
caprolactam selectivity% = caprolactam formation/amount of cyclohexanone oxime converted x 100%.
Example 1
This example illustrates a radial moving bed reactor and a process for the preparation of caprolactam in accordance with the present invention.
As shown in fig. 1 to 4, in the radial moving bed reactor, the reactor shell 1 is cylindrical, the heat taking partitions 6 are disposed in the effective reaction area in the catalyst bed layer 2, are disposed on the outer circumferential surface of the central tube 5, and are formed in a plate shape extending in the axial direction of the central tube 5, the number of the heat taking partitions 6 is 110, and are uniformly arranged in the circumferential direction of the central tube 5 and are respectively located in the diametrical extension direction of the central tube 5, and the shortest distance between two adjacent heat taking partitions 6 is 15mm.
Diameter D of the reactor shell 2 3m, diameter D of the central tube 5 1 2m, a height H of the central tube of 6m, wherein the axial length H 1 0.8m, a height L of the heat-taking spacer 6 of 4m, and a height h of an ineffective portion of the heat-taking spacer 6 2 0.4m, inner ring group diameter d 1 Distance from the center tube D 1 Is 0.4m. The inner ring group is composed of 5 openings which are arranged at equal intervals, and the diameter of each opening is 50mm. The height of the effective reaction zone of the central tube was 4m, the upper portion of the effective reaction zone had an open area of 10%, the lower portion of the effective reaction zone had an open area of 8%, and the upper and lower open areas each occupied 50% of the height of the effective reaction zone.
A mixed gas (namely a raw material) of cyclohexanone oxime, methanol and nitrogen enters a central pipe 5 from a second material inlet and outlet 4, and then the raw material in the central pipe is distributed in the catalyst bed layer 2 through the central pipe 5; wherein the inlet temperature of the raw material in the catalyst bed layer 2 is 350 ℃. Meanwhile, the all-silicon molecular sieve (specifically S-1, with an average particle size of 1.5 mm) enters the catalyst bed 2 from the catalyst feed port 101, and flows from top to bottom in the catalyst bed 2 by its own weight. The raw materials and the catalyst are contacted and reacted in an effective reaction area, reaction heat is removed through a heat taking partition 6, reactants passing through a catalyst bed layer 2 are collected by a material distributor 8 and leave the reactor through a first material inlet and outlet 3, the discharged reactants enter downstream separation and refining, and the reactants and the solvent are separated in a rectification mode to obtain a caprolactam crude product. The rearrangement catalyst has long active life, and is loaded and unloaded intermittently, and the catalyst is discharged from the inner ring group opening of the catalyst discharge port 102.
Because the reaction is exothermic, the heat in the reaction process is continuously removed through the heat taking partition 6, the temperature rise of the bed layer is stably controlled to be not more than 60 ℃, and the gasification rate of the heat exchange medium is 15%. The heat exchange medium is high-pressure (the pressure is 3.5 MPa) saturated water.
Wherein the unloading amount of the catalyst is 50kg/h, and the molar ratio of nitrogen to cyclohexanone oxime is 35:1, the mass ratio of methanol to cyclohexanone oxime is 2.0:1; the inlet temperature of a second material inlet and outlet 4 of the reactor is 340 ℃, the outlet temperature of a first material inlet and outlet 3 of the reactor is 395 ℃, the reaction pressure is 0.46MPa, and the weight hourly space velocity of the cyclohexanone-oxime is 1h -1 . At this time, the average temperature T of the upper ineffective reaction zone 1 315 ℃, the lowest temperature of the effective reaction zone is 340 ℃, and the average temperature T of the lower ineffective reaction zone 2 The temperature was 300 ℃.
After running for 1000 hours, the flow uniformity of the fluid in the bed layer is 97%, the catalyst is sampled from the catalyst outlet 102, and the carbon deposition amount of the obtained catalyst is 3.2wt% of the weight of the catalyst through thermogravimetric analysis.
The product was analyzed by gas chromatography, the conversion of cyclohexanone oxime was 99.99%, the selectivity of caprolactam was 96.5%, and the conversion of cyclohexanone oxime and the selectivity of caprolactam did not change with time.
Comparative example 1
The process of example 1 was followed except that no heat removal separator was provided and the amount of recycle gas was increased by 30% in order to maintain the process parameters required for the same process parameters.
In this comparative example, the temperature rise of the catalyst bed was around 100 ℃. The detection proves that the conversion rate of the cyclohexanone-oxime is 99.99 percent, the selectivity of the caprolactam is 94 percent, and the conversion rate of the cyclohexanone-oxime and the selectivity of the caprolactam are not changed along with the change of time.
Example 2
The process of example 1 is followed except that the molar ratio of nitrogen to cyclohexanone oxime is 20:1, the mass ratio of methanol to cyclohexanone oxime is 5:1; the outlet temperature of the first material inlet and outlet 3 is 390 ℃, the reaction pressure is 0.46MPa, and the weight hourly space velocity of the cyclohexanone-oxime is 1h -1 。
The product was analyzed by gas chromatography, the conversion of cyclohexanone oxime was 99.99%, the selectivity of caprolactam was 96.5%, and the conversion of cyclohexanone oxime and the selectivity of caprolactam did not change with time.
Example 3
The process of example 1 was followed except that the number of the heat-extracting spacers 6 was 80, the shortest distance between two adjacent heat-extracting spacers 6 was 22mm, and the cyclohexanone oxime conversion and caprolactam selectivity were not changed with time.
In this example, the reaction temperature rise was stabilized within 80 ℃, the cyclohexanone oxime conversion was 99.99%, and the caprolactam selectivity was 95%.
Example 4
The method of example 1 was followed except that the height h of the ineffective portion of the heat-extracting separator 6 2 Is 0m; average temperature T of upper ineffective reaction zone 1 Is 280 ℃; and the cyclohexanone oxime conversion rate and caprolactam selectivity do not change along with the change of time.
In this example, the catalyst removal rate was increased to 60kg/h, and the same effect as in example 1 was maintained.
Example 5
The procedure of example 1 was followed, except that,
axial length h of the central tube 1 0.4m, height h of the ineffective part of the heat-taking separator 6 2 Is 0m;
average temperature T of upper ineffective reaction zone 1 The temperature was 240 ℃. And the conversion rate of cyclohexanone-oxime and the selectivity of caprolactam are not dependentThe time varies.
In this example, the catalyst removal rate was increased to 70kg/h, the cyclohexanone oxime conversion was 99.9% and the caprolactam selectivity was 94%.
Example 6
The procedure of example 1 was followed, except that,
diameter d of inner ring set 1 With a central tube D 1 The distance between them is 0.8m.
In this example, the effect was different from that of example 1 in that the catalyst outlet 102 was sampled with a catalyst, and the amount of carbon deposition in the catalyst obtained by thermogravimetric analysis was 2.5wt% based on the weight of the catalyst.
Example 7
The process of example 1 was followed except that the center tube was uniformly perforated in the axial direction and had an opening ratio of 10%.
In this example, after the reaction was carried out for 1000 hours, the flow uniformity of the fluid in the bed was 95%, the conversion of cyclohexanone oxime was 99.95%, and the selectivity of caprolactam was 96%.
From the above results, it can be seen that the example using the radial moving bed reactor provided by the present invention has better cyclohexanone oxime conversion rate and caprolactam selectivity when used for the preparation of caprolactam, compared to comparative example 1. Among these, it can be seen from comparing example 1 with examples 2 and 3 that the solution using the preferably provided heat extraction separator of the present invention shows higher caprolactam selectivity while having high conversion.
By comparing example 1 with examples 4 and 5, it can be seen that the axial length h of the central tube is controlled 1 And the height h of the ineffective part of the heat-taking partition 6 2 Within the limited range of the invention, the catalyst reaction activity can be effectively improved, the removal amount of the catalyst is reduced, and the method is favorable for improving the reaction effect.
Compared with the embodiment 6, the embodiment 1 has the advantages that the catalyst is more reasonably discharged by adopting the method for limiting the arrangement of the catalyst outlet, and the utilization rate of the catalyst is effectively improved.
As can be seen from the comparison between example 1 and example 7, the method for opening the pore ratio provided by the invention has the advantages of more stable reaction and better overall stability of the reaction bed layer under the long-period operation condition.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (16)

1. A radial moving bed reactor, characterized in that it comprises: the device comprises a reactor shell (1), and a central pipe (5) with a through hole, a catalyst bed layer (2) and a material distributor (8) which are arranged from inside to outside in the reactor shell (1); wherein a plurality of heat-taking separators (6) vertically connected with the pipe wall of the central pipe (5) are arranged at intervals along the circumferential direction of the central pipe (5); an upper ineffective reaction zone, an effective reaction zone and a lower ineffective reaction zone are arranged in the catalyst bed layer (2) from top to bottom; wherein the central pipe (5) is provided with no through hole at the parts of the upper ineffective reaction zone and the lower ineffective reaction zone, and the upper part of the heat taking partition (6) is arranged as an ineffective part in the upper ineffective reaction zone.
2. The reactor according to claim 1, wherein the heat-extracting partition (6) is provided on the outer peripheral surface of the center pipe (5) and is formed in a plate shape extending in the axial direction of the center pipe (5).
3. Reactor according to claim 1 or 2, characterized in that a plurality of heat-removing partitions (6) are arranged in the direction of the diametrical extension of the central tube (5).
4. A reactor according to any one of claims 1-3, characterized in that the shortest distance between two adjacent heat-extraction partitions (6) is more than 6 times, more preferably more than 10 times, the average particle size of the catalyst particles packed in the catalyst bed (2).
5. A reactor according to any one of claims 1 to 4, characterized in that the heat-extraction partitions (6) are provided with channels for the circulation of a heat exchange medium;
preferably, a heat exchange medium inlet and a heat exchange medium outlet are arranged on the heat taking partition (6), and the heat exchange medium inlet and the heat exchange medium outlet are respectively communicated with the channels; more preferably, the heat exchange medium inlet and the heat exchange medium outlet are located at the top and bottom of the heat extraction partition (6), respectively;
preferably, the moving bed reactor further comprises a heat exchange line connected to the heat extraction partition (6), the heat exchange line being disposed above the heat extraction partition (6) and within the upper ineffective reaction zone.
6. Reactor according to any one of claims 1 to 5, characterized in that the axial length h of the portion of the central tube (5) which is in the upper inactive reaction zone 1 And the total length H of the central tube (5) satisfies the following conditions: h is 1 H.ltoreq.0.4, preferably H 1 /H≤0.3；
Preferably, the height h of the inactive portion of the heat-extraction partition (6) is selected in the vertical direction 2 And the total height L of the heat-taking separator (6) satisfies the following conditions: h is 2 L.ltoreq.0.2, preferably h 2 /L≤0.1；
Preferably, the upper edge of the ineffective part of the heat taking partition (6) is higher than the lower edge of the part of the central pipe (5) in the upper ineffective reaction zone in the vertical direction.
7. The moving bed reactor according to any of claims 1-6, characterized in that the through holes are provided in the wall of the central tube (5) between two adjacent heat extraction partitions (6);
preferably, the portion of the central tube (5) within the effective reaction zone has a varying porosity;
preferably, the open-cell content varies from 1% to 15% from top to bottom along the central tube (5).
8. A reactor according to any one of claims 1-7, characterized in that the moving bed reactor further comprises a plurality of catalyst offtake (7) arranged in the reactor shell (1), the plurality of catalyst offtake (7) being located above the catalyst bed (2) and being spaced apart along the circumference of the central tube (5).
9. The reactor of any one of claims 1-8, wherein the moving bed reactor further comprises; the device comprises a catalyst inlet (101), a catalyst outlet (102), a first material inlet and outlet (3) and a second material inlet and outlet (4);
the catalyst feeding hole (101) and the catalyst discharging hole (102) are communicated with the catalyst bed layer (2); the catalyst feeding hole (101) and the catalyst discharging hole (102) are respectively arranged at the upper end and the lower end of the reactor shell (1);
the second material inlet and outlet (4) is communicated with the central pipe (5), and the first material inlet and outlet (3) is communicated with the catalyst bed layer (2).
10. The reactor according to claim 9, wherein the catalyst outlet (102) comprises: a plurality of openings arranged annularly along the circumferential direction of the reactor shell (1);
preferably, the plurality of openings are divided into an inner ring group and an outer ring group, wherein the inner ring group is arranged below the central tube (5) and the outer ring group is arranged below the material distributor (8).
11. The bed reactor of claim 10, wherein the inner ring set includes a diameter d of a circle formed by the center of each opening surrounded by 1 The diameter d of a circle formed by the centers of the openings surrounded by the outer ring group 2 Diameter D of the central tube (5) 1 And the reactor shell (1) Diameter D of 2 Satisfies the following conditions: d 1 -d 1 ≤0.3D 2 ，D 2 -d 2 ≤0.3D 2 (ii) a Preferably, D 1 -d 1 ≤0.2D 2 ，D 2 -d 2 ≤0.2D 2 。
12. The bed reactor according to claim 10 or 11, characterized in that when the first material inlet/outlet (3) is filled with reaction raw material and the second material inlet/outlet (4) is used for discharging product, each opening included in the inner ring group is closed, and each opening included in the outer ring group is open, so as to discharge the catalyst which is deactivated first outside the catalyst bed layer (2); or
When reaction raw materials are introduced into the second material inlet and outlet (4) and products are discharged from the first material inlet and outlet (3), the openings of the outer ring group are closed, and the openings of the inner ring group are opened, so that the deactivated catalyst in the catalyst bed layer (2) is discharged.
13. A process for producing caprolactam, the process comprising: introducing raw materials and a catalyst into a reactor respectively for reaction; the raw materials comprise cyclohexanone oxime, carrier gas and solvent; characterized in that the reactor is a moving bed reactor according to any one of claims 1 to 12.
14. The method according to claim 13, characterized in that a heat exchange medium is circulated in the heat-withdrawing partition (6) of the moving bed reactor;
preferably, the gasification rate of the heat exchange medium is not more than 30%;
and/or the heat exchange medium is molten salt, heat conduction oil or water;
preferably, the raw material passes through the catalyst bed layer (2) of the moving bed reactor in a centrifugal mode or a centripetal mode.
15. Process according to claim 13 or 14, wherein the molar ratio of carrier gas to cyclohexanone oxime is in the range of 5 to 100:1, the weight ratio of the solvent to the cyclohexanone oxime is 1-100:1;
preferably, the carrier gas is at least one of nitrogen, argon, a saturated hydrocarbon having a boiling point of not more than 180 ℃, and a halogenated hydrocarbon having a boiling point of not more than 180 ℃; and/or
The solvent is C1-C6 fatty alcohol;
preferably, the conditions of the reaction include: the reaction temperature is 200-500 ℃, the reaction pressure is 0.1-1MPa, and the weight hourly space velocity of the cyclohexanone-oxime is 0.3-20h -1 ；
Preferably, the method further comprises: the temperature rise of the reaction is controlled by the heat removal partition (6) to be not higher than 100 ℃, preferably not higher than 80 ℃, more preferably not higher than 60 ℃.
16. The method of any one of claims 13-15, wherein the average temperature T of the upper ineffective reaction zone in the moving bed reactor 1 Minimum temperature T with effective reaction zone min Satisfies the following conditions: t is min -T 1 Less than or equal to 50 ℃, preferably T min -T 1 ≤30℃；
Preferably, the average temperature T of the lower ineffective reaction zone in the moving bed reactor 2 And T min Satisfies the following conditions: t is min -T 2 ≤80℃。
CN202210805082.1A 2021-07-09 2022-07-08 Radial moving bed reactor and process for producing caprolactam Pending CN115591480A (en)

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CN202110776920 2021-07-09

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