CN114618394B - Hexamethylenediamine synthesis system - Google Patents

Hexamethylenediamine synthesis system Download PDF

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Publication number
CN114618394B
CN114618394B CN202210263438.3A CN202210263438A CN114618394B CN 114618394 B CN114618394 B CN 114618394B CN 202210263438 A CN202210263438 A CN 202210263438A CN 114618394 B CN114618394 B CN 114618394B
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pipeline
slurry
reactor
flushing
hexamethylenediamine
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CN114618394A (en
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耿海涛
应国海
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Beijing Daosike Mining Equipment Technology Co ltd
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Beijing Daosike Mining Equipment Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/082Controlling processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/085Feeding reactive fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087Heating or cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/02Cleaning pipes or tubes or systems of pipes or tubes
    • B08B9/027Cleaning the internal surfaces; Removal of blockages
    • B08B9/032Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08Cleaning containers, e.g. tanks
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/44Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers
    • C07C209/48Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of nitriles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00115Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/00132Tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00539Pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00893Feeding means for the reactants
    • B01J2208/00902Nozzle-type feeding elements

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides a hexamethylenediamine synthesis system, which comprises a reactor, a slurry separator and a gas cooling assembly, wherein the reactor is used for generating hexamethylenediamine by material reaction and comprises a mixing feeder, a hydrogen gas inlet pipeline is arranged on the mixing feeder, and a slurry outlet is arranged on the reactor; the slurry separator is used for slurry degassing and solid-liquid separation, and is communicated with a slurry outlet of the reactor through a first pipeline, and is communicated with the mixing feeder through a second pipeline; the gas cooling component is used for cooling the gas exhausted by the reactor and the slurry separator, is respectively communicated with the tops of the reactor and the slurry separator through a gas recovery pipeline, and is communicated with the first pipeline through a flushing pipeline. The synthesis system provided by the invention can ensure stable and smooth synthesis reaction, reduce production cost and improve production efficiency of hexamethylenediamine.

Description

Hexamethylenediamine synthesis system
Technical Field
The invention relates to the technical field of chemical industry, in particular to a hexamethylenediamine synthesis system.
Background
Hexamethylenediamine is an important chemical raw material, is colorless and transparent crystals at normal temperature and normal state, is mainly used for producing nylon 66, and is prepared into various nylon resins, nylon fibers and the like, thus being a very important synthetic intermediate.
The method is characterized in that hexamethylenediamine is produced by hydrogenation of adiponitrile, and the production method is divided into a high-pressure method and a low-pressure method according to the difference of the pressure required by the reaction, wherein the high-pressure method is generally used for synthesizing hexamethylenediamine by adiponitrile and hydrogen under the catalysis of an iron-based or cobalt-copper catalyst at a high pressure of 30-60 MPa; the low-pressure method is generally used for synthesizing hexamethylenediamine by adiponitrile and hydrogen under the catalysis of Raney nickel catalyst under the pressure of 2-5MPa, and the high-pressure method has the advantages of relatively low reaction temperature and reaction pressure and relatively safe operation due to the harsh reaction conditions and high operation requirements of the high-pressure method. However, in actual production, since the materials involved in the reaction include solid-liquid-gas three phases, solid catalysts are easily deposited, and a blocking phenomenon occurs, hydrogen cannot be fully contacted with the materials or the flow rate is unstable, so that the reaction materials are unevenly mixed, the contact cannot be fully performed, the reaction is incomplete, and the stability and smoothness of the whole reaction are affected.
Disclosure of Invention
The invention aims to provide a synthesis system of hexamethylenediamine, which ensures stable and smooth synthesis reaction and improves production efficiency of hexamethylenediamine.
In order to achieve the above purpose, the invention provides a hexamethylenediamine synthesis system, which comprises a reactor, a slurry separator and a gas cooling component, wherein the reactor is used for reacting materials to generate hexamethylenediamine, the reactor comprises a mixing feeder, a hydrogen gas inlet pipeline is arranged on the mixing feeder, and a slurry outlet is arranged on the reactor; the slurry separator is used for slurry degassing and solid-liquid separation, and is communicated with a slurry outlet of the reactor through a first pipeline, and is communicated with the mixing feeder through a second pipeline; the gas cooling component is used for cooling the gas exhausted by the reactor and the slurry separator, is communicated with the tops of the reactor and the slurry separator through a gas recovery pipeline, and is communicated with the first pipeline through a flushing pipeline. The gaseous substances discharged from the reactor and the slurry reactor are sent to the gas cooling assembly through the gas recovery pipeline to form flushing fluid, so that the flow of the flushing fluid brings away the settled and attached solid components of the slurry in the slurry separator, the first pipeline and the second pipeline, the slurry is promoted to flow in the slurry separator, the first pipeline and the second pipeline, the whole synthesis reaction system is promoted to be smoothly carried out, and the efficiency of producing hexamethylenediamine is improved.
Further, the gas cooling assembly comprises a cooler, a cooling object separating tank and an ethanol storage tank, wherein a gas recovery pipeline is connected with an inlet of the cooler, an outlet of the cooler is connected with the cooling object separating tank, the cooling object separating tank is connected with the ethanol storage tank through an ethanol conveying pipeline, a flushing pipeline is connected with the ethanol storage tank, the gas cooling assembly can convert gaseous substances into flushing fluid, the flushing fluid is sent to the slurry separator, the first pipeline and the second pipeline through the flushing pipeline, the external circulation flow of a reaction system is guaranteed, and the reaction system is kept smooth.
Further, a heating coil is arranged in the ethanol storage tank, a liquid outlet and a vaporization outlet are arranged on the ethanol storage tank, the flushing pipeline comprises a first flushing pipeline, a second flushing pipeline and a third flushing pipeline, the first flushing pipeline is communicated with the liquid outlet of the ethanol storage tank and the first pipeline, the second flushing pipeline is communicated with the liquid outlet of the ethanol storage tank and the first pipeline, the third flushing pipeline is communicated with the vaporization outlet of the ethanol storage tank and the first flushing pipeline, the ethanol storage tank converts the recovered liquid into steam and washing liquid, the dredging and cleaning of the first pipeline, the slurry separator and the second pipeline are realized, and even if the reaction is stopped, the external circulation flow of a reaction system is also ensured, and the smooth operation of the whole reaction system is ensured; the liquid recovered is sent back to the reaction system again, so that the concentration of the whole reaction system can be kept in a moderate range.
Further, be equipped with first flushing control valve on the first flushing pipeline, be equipped with the second flushing control valve on the second flushing pipeline, be equipped with the third flushing control valve on the third flushing pipeline for control flushing fluid's on the flushing pipeline running state, guarantee that reaction system goes on smoothly, improved the efficiency of production.
Further, the first pipeline is provided with a slurry discharging regulating valve, the second pipeline is provided with a slurry feeding regulating valve, and flushing fluid is supplied through the slurry discharging regulating valve and the slurry feeding regulating valve when the synthesis reaction system is started or stopped, so that the time from stopping to running of the reaction system can be shortened, and the efficiency of producing hexamethylenediamine is improved.
Further, the connection point of the first flushing pipeline and the first pipeline is a first connection point, the connection point of the second flushing pipeline and the first pipeline is a second connection point, the slurry discharging adjusting valve is positioned between the first connection point and the second connection point, and the path of the washing liquid is timely adjusted and controlled through automatic adjustment of the slurry discharging adjusting valve, so that the whole synthesis system is kept to be smooth.
Further, the reactor also comprises a gaseous chamber, the gas recovery pipeline is communicated with the gaseous chamber, the gaseous chamber is used for gathering gaseous matters continuously separated from the slurry and can smoothly discharge the gaseous matters out of the reactor through the gas recovery pipeline so as to provide external circulation flushing fluid,
further, a nozzle is arranged on the feed inlet of the mixing feeder, the material is sprayed into the reactor through the nozzle, the slurry circulation flow in the reactor is actuated through the nozzle, so that the reactor can quickly obtain a stable circulation flow, and even if the reaction is stopped, the nozzle supplies fluid into the reactor, thereby ensuring the operation of internal and external circulation.
Further, a guide cylinder is arranged in the reactor to promote the up-and-down circulation flow of materials in the reactor.
Further, the hexamethylenediamine synthesis system further comprises a medium heat exchanger, a heat exchange tube is arranged in the reactor, a medium outlet of the heat exchange tube is communicated with a medium inlet of the medium heat exchanger, a medium inlet of the heat exchange tube is communicated with a medium outlet of the medium heat exchanger, heat generated by the reaction system is removed through liquid flowing in the heat exchange tube, the removed reaction heat enters the medium heat exchanger, the heat is taken away by circulating flowing liquid supplied from the outside, and when the production is continuously carried out, the reaction generated heat can be continuously removed, the stability of the reaction temperature is ensured, and the purpose of stable production is achieved.
Drawings
FIG. 1 is a flow chart of a hexamethylenediamine synthesis system according to a preferred embodiment of the present invention.
Reference numerals illustrate:
10. a reactor; 11. a gaseous chamber; 12. a reaction chamber; 13. a first pipeline; 14. a slurry outlet; 15. a slurry discharging regulating valve; 20. a mixing feeder; 21. a nozzle; 22. a slurry feed regulating valve; 23. a second pipeline; 30. a slurry separator; 40. a coarse material receiving unit; 50. a cooler; 60. a cooling object separating tank; 70. an ethanol storage tank; 71. a heating coil; 72. a vaporization outlet; 73. a liquid outlet; 81. a third flush regulating valve; 82. a third flush line; 83. a first flush regulating valve; 84. a first flush line; 85. a second flush regulating valve; 86. a second flush line; 91. a heat exchange tube; 92. a medium heat exchanger; 100. a raw material unit.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like numerals and letters indicate like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "upper", "lower", "left", "right", "inner", "outer", "front", "rear", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific direction, be configured and operated in a specific direction, and thus should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "configured," "connected," and the like are to be construed broadly and include, for example, "connected," either permanently connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The following description of the preferred embodiments is provided in accordance with the present invention, and it is to be understood that the preferred embodiments described herein are merely illustrative and explanatory of the invention, and are not restrictive of the invention.
As shown in connection with fig. 1, the hexamethylenediamine synthesizing apparatus according to the present embodiment comprises a reactor 10, a slurry separator 30 and a gas cooling unit.
Wherein, the reactor 10 is used for containing reaction slurry to generate hexamethylenediamine, the mixing feeder 20 is provided with a hydrogen gas inlet pipe, the reactor 10 is provided with a slurry outlet 14, the mixing feeder 20 is arranged at the bottom of the reactor 10, and can spray materials into the reactor 10 so as to form an up-down circulating flow (shown by arrow direction in the figure) in the reactor 10, thereby promoting the reaction materials to be fully mixed and preventing the solid catalyst from depositing at the bottom of the reactor 10.
Further, the slurry separator 30 is used for slurry degassing and solid-liquid separation, the slurry separator 30 is communicated with the slurry outlet 14 of the reactor 10 through the first pipeline 13, the slurry separator 30 is communicated with the mixing feeder 20 through the second pipeline 23, the slurry separator 30 can separate gas, products and recovered materials in reaction slurry, and the recovered materials are sent into the reactor 10 again through the second pipeline 23 to continue to participate in the reaction, so that the circulation flow of the whole reaction system is promoted, and the reaction is accelerated.
Meanwhile, gaseous substances discharged from the tops of the reactor 10 and the slurry separator 30 flow to the gas cooling assembly through the gas recovery pipeline, the gas cooling assembly can cool and separate the gaseous substances into hydrogen and liquid, the liquid can be used as washing liquid to wash the first pipeline 13, the slurry separator 30 and the second pipeline 23, the pipeline is prevented from being blocked, the slurry flow is promoted, the smooth and full progress of the whole reaction system is well ensured, and the efficiency of producing hexamethylenediamine is improved.
Specifically, the reactor 10 is a cylindrical metal container, and includes a gas chamber 11 and a reaction chamber 12, generally, adiponitrile and hydrogen are used as raw materials, raney nickel is used as a catalyst, a reaction system for synthesizing hexamethylenediamine by adopting a low pressure method includes gas-liquid-solid three-phase materials, the gas chamber 11 is located at the upper part of the reaction chamber 12 and is used for gathering gaseous substances formed in the reaction process, the gaseous substances include hydrogen and gaseous liquid, and the gas chamber 11 is communicated with the cooler 50 through a gas recovery pipeline so that the gaseous substances are sent out of the gas chamber 11; the reaction chamber 12 is used for containing gas-liquid-solid three-phase materials, and the upper side wall of the reaction chamber is provided with a slurry outlet 14, and the slurry in the reaction chamber 12 is transferred to a slurry separator 30 through the slurry outlet 14. It should be noted that, in the present embodiment, the gaseous chamber 11 and the reaction chamber 12 may be integrally formed chambers or may be separate two independent chambers, which is not limited in the present embodiment.
Further, in this embodiment, in order to promote the generation of a stable internal circulation flow in the reactor 10, a guide cylinder (not shown) is provided in the reactor 10.
Further, in the present embodiment, the diameter of the cylindrical reactor 10 is 1 to 20m and the height is 5 to 50m. More preferably, the cylindrical reactor 10 has a diameter of 2 to 10m and a height of 10 to 35m.
Further, the mixing feeder 20 includes a nozzle 21, the nozzle 21 is disposed in a chamber at the bottom of the reaction chamber 12, a hydrogen gas inlet pipe is disposed at the bottom of the nozzle 21, and the material conveyed by the second pipeline 23 can be sprayed into the reaction chamber 12 through the nozzle 21, so as to generate an up-down circulation flow in the reaction chamber 12, thereby promoting sufficient mixing of the material and improving production efficiency. Meanwhile, the upper and lower circulating flows can drive the solid catalyst to move up and down, so that the solid catalyst is prevented from being deposited and hardened at the bottom of the reaction chamber 12 to influence the production efficiency. It is worth integrating that the direction of the injection of the material into the reaction chamber 12 by the nozzle 21 may be either upward or downward, and is not limited in this embodiment.
It is worth mentioning that after the materials conveyed by the hydrogen gas inlet pipeline and the second pipeline 23 are mixed by the mixing feeder 20, hydrogen is wrapped in the slurry, so that the density of the slurry is reduced, upward movement of the slurry is facilitated, internal circulation of the slurry is promoted, meanwhile, hydrogen solution is dissolved in the slurry, and hydrogen and adiponitrile fully undergo addition reaction under the catalysis of a catalyst, so that the reaction is accelerated.
It is worth integrating that, in the present embodiment, the mixture feeder 20 is used for conveying H 2 In turn, for transporting the slurry separated by the slurry separator 30, and for transporting the flushing fluid, and for transporting the mixed liquor of the raw material unit 100.
As shown in connection with fig. 1, a slurry separator 30 is provided for receiving and separating the slurry flowing into the reactor 10 and delivering the separated materials to designated locations, respectively. Specifically, a rotation unit is disposed in the slurry separator 30, the slurry separator 30 is connected to the slurry outlet 14 of the reactor 10 through the first pipeline 13, a slurry discharging adjusting valve 15 for adjusting the flow rate of the slurry is disposed on the first pipeline 13, the slurry flowing into the slurry separator 30 from the reactor 10 includes three phases of gas, liquid and solid, and the rotation unit facilitates the separation of the three phases of gas, solid and liquid during the rotation process.
Specifically, lighter vapors accumulate in the upper portion of the slurry separator 30 and a gas recovery line, which communicates with the top of the slurry separator 30, is sent out of the slurry separator 30. It is worth mentioning that the liquid phase separated by the slurry separator 30 does not substantially contain hydrogen gas.
Because the specific gravity of the solid catalyst in the slurry is greater than that of the liquid, the solid catalyst can be firstly settled at the bottom of the slurry separator 30, the slurry separator 30 is communicated with the mixing feeder 20 through the second pipeline 23, the solid-liquid slurry at the bottom of the slurry separator 30 flows to the mixing feeder 20 through the second pipeline 23 and is sent into the reactor 10 again to continue to participate in the reaction, the recycling of the solid catalyst is realized, the production cost is reduced, and meanwhile, the slurry separator 30 realizes the circulating flow of the slurry in the reactor 10, which is beneficial to the full mixing of the slurry, promotes the rapid reaction, and can also avoid the deposition of the solid catalyst in the reaction system or the blockage of a pipeline. Meanwhile, a slurry feeding regulating valve 22 for regulating and controlling the flow rate of the materials is arranged on the second pipeline 23.
Preferably, in the present embodiment, the slurry separator 30 is provided at the upper end of the mixing feeder 20 so that the recovered material flows toward the mixing feeder 20 by gravity, reducing power consumption.
Further, the hexamethylenediamine synthesizing system further comprises a coarse material receiving unit 40, and a discharge port is provided at a sidewall of the slurry separator 30, and when the reaction system is detected to be completed, the coarse hexamethylenediamine liquid separated by the slurry separator 30 flows out through the discharge port and is received at the coarse material receiving unit 40.
Referring to fig. 1, the cooler 50 is used for receiving the gaseous materials flowing out of the reactor 10 and the slurry separator 30, the gaseous materials are separated into hydrogen and liquid after passing through the cooler 50, the liquid is mainly a mixed liquid of water and ethanol, the hydrogen and the liquid are all collected at the position of the cooler separating tank 60, wherein the hydrogen is gathered at the upper part of the cooler separating tank 60, the liquid is gathered at the bottom of the cooler separating tank 60, a hydrogen outlet is arranged at the top of the cooler separating tank 60, the hydrogen flows out through the hydrogen outlet and is finally conveyed to the mixing feeder 20 (not shown in the figure), and the mixture feeder 20 is re-conveyed into the reactor 10 to participate in the reaction, so that the loss of the hydrogen is avoided, and the production cost is saved.
It should be noted that the cooler 50 may be disposed inside the coolant separation tank 60 or may be disposed outside the coolant separation tank 60, and is not limited in this embodiment.
Further, the ethanol storage tank 70 is connected to the condensate separation tank 60 through an ethanol transfer line 74, and the liquid accumulated at the bottom of the condensate separation tank 60 is transferred into the ethanol storage tank 70 through the ethanol transfer line 74. Preferably, a circulation pump for delivering liquid is provided on the communicating ethanol delivery line 74.
Further, as shown in fig. 1, a heating coil 71 is disposed in the ethanol storage tank 70, a vaporizing outlet 72 and a liquid outlet 73 are disposed at the top and bottom of the ethanol storage tank 70, the liquid outlet 73 is respectively connected to the first pipeline 13 through a first flushing pipeline 84 and a second flushing pipeline 86, the connection point between the first flushing pipeline 84 and the first pipeline 13 is a first connection point a, the connection point between the second flushing pipeline 86 and the first pipeline 13 is a second connection point B, the first connection point a and the second connection point B are respectively located at the left and right sides of the slurry discharging adjusting valve 15, the vaporizing outlet 72 is connected to the first flushing pipeline 84 through a third flushing pipeline 82, when the heating coil 71 heats the liquid in the ethanol storage tank 70, part of the liquid is vaporized, the vapor is sent out through the third flushing pipeline 82, and the unvaporized liquid is sent out through the first flushing pipeline 84 and the second flushing pipeline 86. Specifically, when the slurry discharge regulating valve 15 is closed, the first pipe 13 connecting the reactor 10 and the slurry separator 30 is blocked, wherein the washing liquid and steam fed from the first washing line 84 and the third washing line 82 flow into the reactor 10, and the washing liquid fed from the second washing line 86 flows into the slurry separator 30; when the slurry discharge regulating valve 15 is opened, steam in the third flush line 82, the first flush line 84 and the wash liquid in the second flush line 86 all flow with the slurry into the slurry separator 30. In this process, when the slurry discharging adjusting valve 15 is closed, the reactor 10 cannot convey slurry into the slurry separator 30, the slurry flow in the first pipeline 13 is stopped, the solid catalyst is deposited in the pipeline, at this time, the flowing washing liquid and steam can wash the first pipeline 13, the solid catalyst is prevented from blocking the first pipeline 13, on the other hand, the washing liquid and steam are returned to the slurry, and the change of the slurry concentration caused by the liquid loss in the reaction process can be prevented. It is worth integrating that during vaporization of the liquid, the vaporized vapor will create a pressure in the ethanol storage tank 70 that will promote vapor flow in the first, second and third flush lines 84, 86 and 82. Meanwhile, the uninterrupted flushing of the pipeline is ensured, so that even if the whole reaction system is stopped, the problem that the pipeline is blocked and cannot be restarted is avoided, and the production process is further accelerated.
Further, a first flushing regulator 83, a second flushing regulator 85 and a third flushing regulator 81 for controlling the flow rate of the washing liquid or the steam are provided on the first flushing line 84, the second flushing line 86 and the third flushing line 82, respectively.
Further, in the present embodiment, the flow rate of the liquid or vapor in the first flush line 84, the second flush line 86, and the third flush line 82 is set to 0.12 to 0.50m/s. Preferably, the flow rate of the liquid or vapor in the first, second and third flush lines 84, 86 and 82 is 0.12-0.35m/s.
Further, in the present embodiment, the flow rate of the slurry in the first pipe 13 is set to 0.001 to 0.15m/s. Preferably, the flow rate of the slurry in the first line 13 is 0.02m/s.
Further, the hexamethylenediamine synthesis system further comprises a control unit for monitoring and controlling the operation state of the synthesis device and controlling the opening and closing states of the valves.
Further, the hexamethylenediamine synthesis system further comprises a pressure detection unit, and the monitoring information is transmitted to the control unit for monitoring the pressure in the reactor 10 so as to control the pressure in the reactor 10 to be 1-5MPa. Preferably, the pressure within the reactor 10 is 2MPa.
Further, the hexamethylenediamine synthesis system further comprises a medium heat exchanger 92, the heat exchange tube 91 is arranged in the reaction chamber 12, a medium outlet of the heat exchange tube 91 is communicated with a medium inlet of the medium heat exchanger 92, a medium inlet of the heat exchange tube 91 is communicated with a medium outlet of the medium heat exchanger 92, the heat exchange tube 91 is uniformly distributed and fixed in a bottom containing cavity of the reaction chamber 12, and the side wall of the reaction chamber 12 is arranged in an upward extending manner, and heat generated in the reaction chamber 12 is brought out of the reaction chamber 12 through liquid circularly flowing between the heat exchange tube 91 and the medium heat exchanger 92, so that the temperature in the reaction chamber 12 is kept constant, and the purpose of stable production is achieved.
It is to be noted that, in the present embodiment, the shape and the number of the heat exchange tubes 91 are not limited.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solution of the present invention, and not limiting thereof; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (8)

1. A hexamethylenediamine synthesis system, comprising:
the reactor (10) is used for generating hexamethylenediamine by material reaction, the reactor (10) comprises a mixing feeder (20), a hydrogen gas inlet pipeline is arranged on the mixing feeder (20), and a slurry outlet (14) is arranged on the reactor (10);
a slurry separator (30) for slurry degassing and solid-liquid separation, the slurry separator (30) being in communication with the slurry outlet (14) of the reactor (10) through a first conduit (13), the slurry separator (30) being in communication with the mixture feeder (20) through a second conduit (23);
a gas cooling assembly for cooling the gas exiting the reactor (10) and the slurry separator (30), the gas cooling assembly being in communication with the top of the reactor (10) and the slurry separator (30) through a gas recovery line, the gas cooling assembly being in communication with the first conduit (13) through a flushing line;
the gas cooling assembly includes:
-a cooler (50), the gas recovery line being in communication with an inlet of the cooler (50);
a cooling matter separating tank (60), wherein an outlet of the cooler (50) is connected with the cooling matter separating tank (60);
an ethanol storage tank (70), wherein the condensate separation tank (60) is connected with the ethanol storage tank (70) through an ethanol delivery pipeline, and the flushing pipeline is connected with the ethanol storage tank (70);
be equipped with heating coil (71) in ethanol storage tank (70), be equipped with liquid outlet (73) and vaporization export (72) on ethanol storage tank (70), the flushing pipeline includes first flushing pipeline (84), second flushing pipeline (86) and third flushing pipeline (82), first flushing pipeline (84) intercommunication liquid outlet (73) of ethanol storage tank (70) with first pipeline (13), second flushing pipeline (86) intercommunication liquid outlet (73) of ethanol storage tank (70) with first pipeline (13), third flushing pipeline (82) intercommunication gas vaporization export (72) of ethanol storage tank (70) with first flushing pipeline (84).
2. Hexamethylenediamine synthesis system according to claim 1, characterized in that the first flushing line (84) is provided with a first flushing regulating valve (83), the second flushing line (86) is provided with a second flushing regulating valve (85), and the third flushing line (82) is provided with a third flushing regulating valve (81).
3. Hexamethylenediamine synthesis system according to claim 2, characterized in that the first pipeline (13) is provided with a slurry outlet regulating valve (15) and the second pipeline (23) is provided with a slurry inlet regulating valve (22).
4. A hexamethylenediamine synthesis system according to claim 3, characterized in that the connection point of the first flushing line (84) to the first pipe (13) is a first connection point, the connection point of the second flushing line (86) to the first pipe (13) is a second connection point, the slurry take-off regulating valve (15) being located between the first connection point and the second connection point.
5. Hexamethylenediamine synthesis system according to any one of claims 1 to 4, characterized in that the reactor (10) comprises a gaseous chamber (11), the gas recovery line being in communication with the gaseous chamber (11).
6. Hexamethylenediamine synthesis system according to any one of claims 1 to 4, characterized in that the feed inlet of the mixing feeder (20) is provided with a nozzle (21).
7. Hexamethylenediamine synthesis system according to any one of claims 1 to 4, characterized in that a guide shell is provided inside the reactor (10).
8. The hexamethylenediamine synthesis system according to any one of claims 1-4, further comprising a medium heat exchanger (92), wherein a heat exchange tube (91) is arranged in the reactor (10), a medium outlet of the heat exchange tube (91) is communicated with a medium inlet of the medium heat exchanger (92), and a medium inlet of the heat exchange tube (91) is communicated with a medium outlet of the medium heat exchanger (92).
CN202210263438.3A 2022-03-17 2022-03-17 Hexamethylenediamine synthesis system Active CN114618394B (en)

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JP5409370B2 (en) * 2007-09-27 2014-02-05 新日鉄住金エンジニアリング株式会社 Synthetic reaction system
US10363535B1 (en) * 2018-04-18 2019-07-30 Shanghai Yankuang Energy R&D Co., Ltd. Gas-liquid-solid three-phase slurry bed industrial reactor capable of achieving continuous operation
CN108514854A (en) * 2018-06-07 2018-09-11 淄博恒亿化工科技有限公司 A kind of circulation flow reactor of adipic dinitrile hydrogenation production hexamethylene diamine
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CN209555114U (en) * 2018-11-13 2019-10-29 中国化学赛鼎宁波工程有限公司 A kind of production system of hexamethylene diamine
CN109438256A (en) * 2018-11-13 2019-03-08 中国化学赛鼎宁波工程有限公司 A kind of production method and production system of hexamethylene diamine
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