CN116393046A - Reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation and synthesis method - Google Patents

Reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation and synthesis method Download PDF

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Publication number
CN116393046A
CN116393046A CN202310345980.8A CN202310345980A CN116393046A CN 116393046 A CN116393046 A CN 116393046A CN 202310345980 A CN202310345980 A CN 202310345980A CN 116393046 A CN116393046 A CN 116393046A
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reactor
vaporizer
inlet
ethylcyclohexane
outlet
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刘勇武
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Hubei Jubang Petrochemical Co ltd
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Hubei Jubang Petrochemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • C07C5/02Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
    • C07C5/10Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of aromatic six-membered rings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/06Flash distillation
    • 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
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/04Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00Systems containing only non-condensed rings
    • C07C2601/12Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/14The ring being saturated

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The embodiment of the application provides a reaction device and a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation. The reaction device comprises a vaporizer, a reactor, a steam-water separator and a cooler: the inlet of the vaporizer is connected with a benzene feeding pipe and a hydrogen feeding pipe; the inlet of the reactor is connected with the outlet of the vaporizer; the inlet of the steam-water separator is connected with the reactor, and the outlet of the steam-water separator is connected with the inlet of the vaporizer; the inlet of the cooler is connected with the reactor, and the outlet is connected with the discharging pipe. According to the embodiment of the application, the reactor and the vaporizer are connected through the steam-water separator, a large amount of heat is carried by byproduct steam, and the heat is fully introduced into the vaporizer to heat raw material benzene without external heat supply, so that the reaction temperature can be timely reduced, reaction impurities generated by the change of the reaction temperature are reduced, and the heat utilization rate is improved; meanwhile, by arranging the steam-water separator, the liquid-phase product and the gas-phase product are filtered, separated and purified, so that the production continuity is ensured, and the production cost is reduced.

Description

Reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation and synthesis method
Technical Field
The application relates to the technical field of chemical synthesis, in particular to a reaction device and a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation.
Background
Cyclohexane is an important organic chemical, which is a main raw material for producing nylon products, and is an excellent solvent for cellulose ether, resin, wax, asphalt and rubber, so that the production of cyclohexane is becoming important.
The technological process of producing cyclohexane by benzene hydrogenation in the prior art is that liquid benzene is heated and gasified in a vaporizer and mixed with hydrogen, the mixture enters a hydrogenation reactor tube side, the reaction is carried out under the action of a catalyst, reaction heat is carried into a boiler by hot water gasification of shell side circulation to be converted into low-pressure steam, and a tube side reaction product is subjected to gas-liquid separation by a cooling and absorbing device, so that liquid-phase product cyclohexane is obtained, and noncondensable gas is discharged. The main reaction system is a hydrogenation unit. The benzene as reaction material is preheated to 120-150 deg.c, vaporized and mixed with hydrogen in hydrogenation reactor to produce addition reaction with hydrogen to produce cyclohexane and release great amount of heat. The temperature of the gas generated by the reaction under the action of the reaction heat is higher, and more heat is carried. Since benzene hydrogenation is a strongly exothermic reversible reaction, at higher reaction temperatures the equilibrium conversion of the reaction will be relatively low, while side reactions tend to occur, such as internal isomerization of cyclohexane to methylcyclopentane, and ring opening reactions at high temperatures to C5 or lower byproducts. At present, an external circulation heat exchange method is generally adopted in industry to remove reaction heat, but the effect is not ideal, secondary heat exchange equipment is also needed to be added, the process flow is long, the investment cost is high, the reaction heat utilization rate is low, and more industrial three wastes can be generated.
In summary, the reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation in the prior art has the technical problems of overhigh reaction temperature, low heat exchange efficiency, long process flow, high investment cost, low reaction heat utilization rate and more industrial three wastes.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a reaction device and a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation, which are used for solving the technical problems of overhigh reaction temperature, low heat exchange efficiency, long process flow, high investment cost, low reaction heat utilization rate and more industrial three wastes in the reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation in the prior art.
The embodiment of the application provides a reaction device and a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation, and specifically:
in a first aspect, embodiments of the present application provide a reaction apparatus for preparing ethylcyclohexane by hydrogenating ethylbenzene, including:
the inlet of the vaporizer is connected with the benzene feeding pipe and the hydrogen feeding pipe;
the inlet of the reactor is connected with the outlet of the vaporizer;
a vapor-water separator having an inlet connected to the reactor and an outlet connected to the inlet of the vaporizer to receive and filter the vapor-phase product from the reactor and to deliver the vapor-phase product to the vaporizer;
and the inlet of the cooler is connected with the reactor, and the outlet of the cooler is connected with the discharge pipe.
In some embodiments of the present application, the reactor comprises a first reactor and a second reactor connected in series with each other, an inlet of the first reactor is connected with the vaporizer, an outlet is connected with the steam-water separator and the second reactor, an inlet of the second reactor is connected with the first reactor, and an outlet is connected with the steam-water separator and the cooler.
In some embodiments of the present application, the reactor further comprises a third reactor connected in series with the first reactor and the second reactor, an inlet of the third reactor is connected with the second reactor, and an outlet is connected with the vaporizer and the cooler.
In some embodiments of the present application, any of the first reactor, the second reactor, and the third reactor is connected in series with at least one shut-off valve and connected in parallel with one shut-off valve.
In some embodiments of the present application, the vaporizer is further connected to the inlet of the second reactor through the stop valve, the outlet of the second reactor is connected to the inlet of the first reactor through the stop valve, and the outlet of the first reactor is connected to the inlet of the third reactor through the stop valve.
In some embodiments of the present application, the first reactor and the second reactor are both tubular reactors, and a catalyst and a diluent are disposed in the first reactor and the second reactor;
the third reactor is a tank reactor, and a catalyst is arranged in the third reactor.
In some embodiments of the present application, the catalyst comprises nickel, and the catalyst is in the form of solid particles.
In some embodiments of the present application, the reaction device further comprises a recovery tube and a compressor, wherein two ends of the recovery tube are respectively connected with the discharge tube and the hydrogen feed tube, and the compressor is disposed on the recovery tube.
In some embodiments of the present application, the reaction apparatus further comprises a hydrogen buffer tank, an inlet of the hydrogen buffer tank is connected with the hydrogen feed pipe, and an outlet of the hydrogen buffer tank is connected with the vaporizer.
In a second aspect, an embodiment of the present application provides a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation, which is synthesized by using the reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation according to any embodiment of the first aspect, and includes the following steps:
introducing benzene into a vaporizer through a benzene feed line;
introducing hydrogen into the vaporizer through a hydrogen feed line;
the vaporized mixture of benzene and hydrogen generates liquid-phase products and gas-phase products in a reactor;
discharging the liquid phase product from the discharge pipe after passing through the cooler;
and filtering the gas phase product through a steam-water separator and then introducing the gas phase product into the vaporizer.
The beneficial technical effects that technical scheme that this application embodiment provided brought include: the steam-water separator is connected with the reactor and the vaporizer, by-product steam generated by the reaction in the reactor carries a large amount of heat, and the steam is totally led into the vaporizer to heat raw material benzene, so that external heat supply is not needed, the reaction temperature in the reactor can be timely reduced, the reaction temperature is kept in an ideal range, reaction impurities generated by the change of the reaction temperature are reduced, devices such as the reactor are effectively protected, the heat utilization rate in a reaction system is improved, and the energy loss caused by continuous heating of the vaporizer is reduced; meanwhile, by arranging the steam-water separator, the liquid-phase product and the gas-phase product are filtered, separated and purified, so that the production continuity is ensured, and the production cost is reduced.
Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application.
Drawings
The foregoing and/or additional aspects and advantages of the present application will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic structural diagram of a reaction apparatus for preparing ethylcyclohexane by hydrogenating ethylbenzene provided in the embodiment of the present application;
fig. 2 is a schematic flow chart of a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation according to an embodiment of the present application.
The marks in the figure:
a 1-benzene feed tube; 2-hydrogen feed pipe; 3-vaporizer; 4-a reactor;
41-a first reactor; 42-a second reactor; 43-third reactor;
5-a steam-water separator; a 6-cooler; 7-a discharge pipe; 8-a compressor;
9-a hydrogen buffer tank; 10-a preheater; 11-a hydrogen heat exchanger;
12-a reaction product separation tank; 13-a recycle hydrogen condenser;
14-circulating hydrogen knockout; 15-a reaction product flash tank;
16-flash gas condenser; 17-reaction product was pumped out.
Detailed Description
Embodiments of the present application are described below with reference to the drawings in the present application. It should be understood that the embodiments described below with reference to the drawings are exemplary descriptions for explaining the technical solutions of the embodiments of the present application, and the technical solutions of the embodiments of the present application are not limited.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless expressly stated otherwise, as understood by those skilled in the art. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of other features, information, data, steps, operations, elements, components, and/or groups thereof, etc. that may be implemented as desired in the art. It will be understood that when an element is referred to as being "connected" or "coupled" to another element, it can be directly connected or coupled to the other element or intervening elements may be present. Further, "connected" or "coupled" as used herein may include wirelessly connected or wirelessly coupled.
For the purpose of making the objects, technical solutions and advantages of the present application more apparent, the embodiments of the present application will be described in further detail below with reference to the accompanying drawings. It should be noted that the following embodiments may be referred to, or combined with each other, and the description will not be repeated for the same terms, similar features, similar implementation steps, and the like in different embodiments.
The embodiment of the application provides a reaction device and a synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation, and specifically:
in a first aspect, an embodiment of the present application provides a reaction apparatus for preparing ethylcyclohexane by ethylbenzene hydrogenation, as shown in fig. 1, fig. 1 is a schematic structural diagram of the reaction apparatus for preparing ethylcyclohexane by ethylbenzene hydrogenation provided in the embodiment of the present application. A reaction device comprising a vaporizer 3, a reactor 4, a steam-water separator 5 and a cooler 6:
the inlet of the vaporizer 3 is connected with the benzene feed pipe 1 and the hydrogen feed pipe 2;
a reactor 4, the inlet of which is connected with the outlet of the vaporizer 3;
a steam-water separator 5, the inlet of which is connected to the reactor 4, and the outlet of which is connected to the inlet of the vaporizer 3, to receive and filter the gas-phase product from the reactor 4, and to transfer the gas-phase product into the vaporizer 3;
and the cooler 6 is connected with the reactor 4 at the inlet and connected with the discharging pipe 7 at the outlet.
The reactor 4 and the vaporizer 3 are connected through the steam-water separator 5, the byproduct steam generated by the reaction in the reactor 4 carries a large amount of heat, and the heat generated by introducing the steam into the vaporizer 3 heats raw material benzene, so that the reaction temperature in the reactor 4 can be timely reduced, the reaction temperature is kept in an ideal range, reaction impurities generated by the change of the reaction temperature are reduced, the devices such as the reactor 4 are effectively protected, and on the other hand, the heat utilization rate in a reaction system is improved, and the energy loss caused by continuous heating of the vaporizer 3 is reduced; meanwhile, the vapor-water separator 5 is arranged to filter, separate and purify the liquid-phase product and the vapor-phase product, thereby ensuring the continuity of production and reducing the production cost.
In some embodiments of the present application, the reactor 4 includes a first reactor 41 and a second reactor 42 connected in series with each other, an inlet of the first reactor 41 is connected to the vaporizer 3, an outlet is connected to the steam-water separator 5 and the second reactor 42, an inlet of the second reactor 42 is connected to the first reactor 41, and an outlet is connected to the steam-water separator 5 and the cooler 6.
In this embodiment, the benzene feed pipe 1, the hydrogen feed pipe 2 are connected to the vaporizer 3, and the vaporizer 3, the reactor 4, and the cooler 6 are sequentially connected in series, specifically, the vaporizer 3, the first reactor 41, the second reactor 42, and the cooler 6 are sequentially connected in series.
When the gas phase raw materials are connected in series, the gas phase raw materials need to pass through the first reactor 41 and the second reactor 42, a plurality of layers of catalysts are arranged in the first reactor 41 and the second reactor 42, and as the reaction is exothermic, the reaction zone in each reactor 4 is elongated, the reaction is sufficient, only the catalyst at the lowest layer is a pure catalyst, and the rest layers are all added with diluents.
In some embodiments of the present application, the reactor 4 further comprises a third reactor 43 connected in series with the first reactor 41 and the second reactor 42, wherein an inlet of the third reactor 43 is connected with the second reactor 42, and an outlet is connected with the vaporizer 3 and the cooler 6.
On the basis of the above embodiment, the vaporizer 3, the first reactor 41, the second reactor 42, and the third reactor 43 are sequentially connected in series. The first reactor 41 and the second reactor 42 are used as the main reactor 4, the reaction is stable, the service life is long, the replacement times of the catalyst can be reduced, the third reactor 43 is used as the supplementary reaction, the reaction quantity is small, but the reaction temperature is not higher, and the consumption is less.
In some embodiments of the present application, any of the first reactor 41, the second reactor 42, and the third reactor 43 is connected in series with at least one shut-off valve and connected in parallel with one shut-off valve.
In this embodiment, the inlet and outlet of each reactor 4 are each connected in series with a shut-off valve, while each reactor 4 is connected in parallel with a shut-off valve. When two corresponding series cut-off valves of the reactor 4 are disconnected, corresponding parallel cut-off valves are conducted, the main pipeline is conducted, meanwhile, no production raw material enters the reactor 4, so that when the catalyst in the first reactor 41 or the second reactor 42 needs to be replaced, the first reactor 41 or the second reactor 42 can be disconnected from the reaction pipeline by controlling the cut-off valves, the replacement catalyst is removed and reflected, no furnace shutdown is needed, and the production continuity can be ensured.
When the catalyst in the first reactor 41 needs to be replaced, the stop valve is controlled to ensure that the first reactor 41 breaks a main passage, the second reactor 42 and the third reactor 43 are in series connection for operation, the first reactor 41 is taken down for replacing the catalyst, no furnace shutdown is needed, and the production continuity can be ensured; similarly, by operating each shut-off valve, the first reactor 41 and the third reactor 43 can be operated in series, and the second reactor 42 can be removed to replace the catalyst.
Similarly, by controlling the on/off of the different shut-off valves, any one or both of the first reactor 41, the second reactor 42, and the third reactor 43 may be connected to the passage, and maintenance may be performed on the disconnected reactor.
In some embodiments of the present application, the vaporizer 3 is further connected to the inlet of the second reactor 42 through the stop valve, the outlet of the second reactor 42 is connected to the inlet of the first reactor 41 through the stop valve, and the outlet of the first reactor 41 is connected to the inlet of the third reactor 43 through the stop valve.
On the basis of the above-described embodiment, the piping connected in the following order is disconnected by controlling the shut-off valve: vaporizer 3, first reactor 41, second reactor 42, and third reactor 43. At the same time, the pipes connected in this order are turned on, and the vaporizer 3, the second reactor 42, the first reactor 41, and the third reactor 43 are connected. I.e. the order in which the first reactor 41 and the second reactor 42 are connected into the reaction line may be interchanged.
In some embodiments of the present application, a catalyst and a diluent are disposed in the first reactor 41 and the second reactor 42, and a catalyst is disposed in the third reactor 43.
The first reactor 41 and the second reactor 42 are used as the main reactor 4, the catalyst in the main reactor is added with a diluent, the reaction is stable, the service life is longer, the replacement times of the catalyst can be reduced, the third reactor 43 is used as the supplementary reaction, the reaction quantity is small, and the consumption is small due to the pure catalyst.
The first reactor 41 can complete about 75% of the reaction, the second reactor 42 can complete about 23% of the reaction, the catalyst in the two reactors 4 is added with a diluent, the reaction is stable, the service life is longer, the replacement times of the catalyst can be reduced, the third reactor 43 is used as a supplementary reaction, only about 2% of the reaction is completed, the consumption of the pure catalyst in the reaction is less, and the conversion rate of benzene is improved to more than 99.9%.
In some embodiments of the present application, the first reactor 41 and the second reactor 42 are both tubular reactors 4, and the third reactor 43 is a tank reactor 4.
The tubular reactor 4 has better reaction effect, can timely take away the reaction heat, but has higher cost, and the third reactor 43 is used for supplementing reaction, so that the cost of the whole equipment can be reduced.
In some embodiments of the present application, the catalyst comprises nickel, and the catalyst is in the form of solid particles.
The nickel catalyst has high hydrogenation activity, good catalytic activity, high mechanical strength, insensitivity to poison and good thermal conductivity. Is suitable for being used as a heat carrier to take away the reaction heat.
The nickel catalyst is used for gas phase hydrogenation under certain conditions to obtain high-purity ethylcyclohexane.
In some embodiments of the present application, the reaction device further comprises a recovery pipe and a compressor 8, wherein two ends of the recovery pipe are respectively connected with the discharging pipe 7 and the hydrogen feeding pipe 2, and the compressor 8 is disposed on the recovery pipe.
Residual hydrogen in the discharging pipe 7 can be reacted again through the recycling pipe and the compressor 8, so that the utilization rate of raw materials is improved, the consumption of raw materials is reduced, and the production cost is saved.
Optionally, a preheater 10 is arranged between the benzene feed pipe 1 and the steam-water reactor, the cooler 6 comprises a hydrogen heat exchanger 11, an outlet of the reactor 4 is connected with an inlet of the hydrogen heat exchanger 11, and an outlet of the hydrogen heat exchanger 11 is respectively connected with an inlet of the preheater 10 and an inlet of the vaporizer 3. The preheater 10 can preheat the raw material benzene from the benzene feed pipe 1, the outlet of the preheater 10 is connected with the vaporizer 3, and preheated benzene is vaporized in the vaporizer 3 to form gas-phase benzene. The hydrogen flowing through the hydrogen heat exchanger 11 exchanges heat with the recycle gas.
Optionally, the outlet of the preheater 10 is sequentially connected with a reaction product cooler 6, a reaction product separation tank 12, a recycle hydrogen condenser 13, a recycle hydrogen knockout 14 and a compressor 8, and the other end of the compressor 8 is connected with the outlet of the hydrogen feed pipe 2; the other branch of the reaction product separating tank 12 is connected with a reaction product flash tank 15, a reaction product delivery pump 17 and a discharge pipe 7 in sequence, and the other branch of the reaction product flash tank 15 is connected with a flash condenser 16.
In some embodiments of the present application, the reaction device further comprises a hydrogen buffer tank 9, wherein an inlet of the hydrogen buffer tank 9 is connected with the hydrogen feeding pipe 2, and an outlet of the hydrogen buffer tank is connected with the vaporizer 3.
In some embodiments, the reaction apparatus further comprises a hydrogen buffer tank 9, an outlet of the hydrogen buffer tank 9 being connected to an inlet of a hydrogen heat exchanger 11, an outlet of the hydrogen heat exchanger 11 being connected to an inlet of the vaporizer 3.
The hydrogen buffer tank 9 is used for temporarily storing hydrogen, the hydrogen in the hydrogen buffer tank 9 firstly enters the hydrogen heat exchanger 11 to exchange heat with circulating gas, so that the temperature of the hydrogen is increased, the hydrogen with the increased temperature enters the vaporizer 3 to be mixed with vaporized benzene, and then enters the reactor 4 through a mixed gas outlet of the vaporizer 3 to react. The heat of the circulating gas is utilized to reduce the energy consumption of hydrogen preheating.
In some embodiments of the present application, ethylbenzene is introduced into the benzene feed pipe 1, and the reaction product is ethylcyclohexane.
The reactants are cooled in a cooler 6 to obtain liquid cyclohexane, and the complete reaction of benzene can be ensured by adjusting the proportion of hydrogen and benzene, so that the influence on the subsequent process is avoided.
Optionally, a benzene feed pipe 1 and a hydrogen feed pipe 2 in the reaction device are connected with two sets of evaporators 3, a reactor 4, a steam-water separator 5, a cooler 6 and a discharge pipe 7. One set of the two sets of systems can be independently started or both sets of systems can be started at the same time according to actual production requirements.
The reaction product flash tank 15 operates at as low a pressure as possible to flash as much dissolved hydrogen as possible from the product, reducing the load on the tank farm for oil and gas recovery, so the product needs to be pumped up to the tank farm.
In this embodiment, the reaction product is still in gas phase after passing through the preheater 10 and the hydrogen heat exchanger 11, and gas-liquid separation in the heat exchanger is not required. The gas phase volume fraction of the reaction product after passing through the cooler 6 is more than 99.5%, the problem of pipeline vibration of the gas-liquid two-phase flow is basically not considered, the reaction product can directly enter the reaction product separation tank 12 for gas-liquid separation, and the gas-liquid separation effect is better than that of a heat exchanger. The gas phase volume fraction of the circulating hydrogen after being cooled by the chilled water of the circulating hydrogen condenser 13 is more than 99.9%, and the gas-liquid separation in the circulating hydrogen liquid separating tank is better as in the cooler 6. The coil pipe in the lower section of the vaporizer 3 heats the medium to be gasified completely, and then the medium is heated to the temperature required by the reaction through the upper section tube type heat exchanger. For intrinsic safety, the coil material should be stainless steel. 5. Circulating cooling water: 0.4MPaG,32-40 ℃, chilled water: 0.4MPaG,7-12 ℃.
The inlet of the preheater 11 is provided with a flow regulating valve, which is connected with a shut-off valve. The inlet of the carburetor 3 is provided with a temperature regulating valve which is connected with a stop valve and is filled with medium-pressure steam and air and discharges low-pressure steam. The inlet of the steam-water separator 5 is filled with desalted water, low-pressure steam is discharged, the inlet is provided with a liquid level regulating valve, the liquid level regulating valve is connected with a stop valve, and the outlet is provided with a pressure remote sensor. The hydrogen buffer tank 9 is connected with a pressure remote sensor, the pressure remote sensor is connected with a stop valve, one end of the stop valve discharges air, the other end of the stop valve is connected with another stop valve, the other stop valve is controlled by a flow regulating valve, the flow regulating valve is connected with a circulating hydrogen dispenser 14, the circulating hydrogen dispenser 14 is also connected with the pressure remote sensor, an online hydrogen analysis instrument and a liquid level regulating valve, and the liquid level regulating valve is connected with the stop valve. Both ends of the cooler 6 are respectively connected with a circulating cooling water feed pipe and a circulating cooling water return pipe, both ends of the circulating hydrogen condenser 13 are respectively connected with a chilled water feed pipe and a chilled water return pipe, and both ends of the flash evaporation gas condenser 16 are respectively connected with a chilled water feed pipe and a chilled water return pipe.
In a second aspect, an embodiment of the present application provides a method for preparing ethylcyclohexane by ethylbenzene hydrogenation, as shown in fig. 2, and fig. 2 is a schematic flow chart of the method for preparing ethylcyclohexane by ethylbenzene hydrogenation provided in the embodiment of the present application. The synthesis method adopts the reaction device for preparing the ethylcyclohexane by hydrogenating the ethylbenzene according to the embodiment of the first aspect for synthesis, and comprises the following steps:
s1, introducing benzene into a vaporizer 3 through a benzene feed pipe 1;
s2, introducing hydrogen into the vaporizer 3 through a hydrogen feeding pipe 2;
s3, generating a liquid-phase product and a gas-phase product in the reactor 4 from the vaporized mixture of the benzene and the hydrogen;
s4, discharging the liquid-phase product from a discharge pipe 7 after passing through a cooler 6;
s5, filtering the gas phase product through a steam-water separator 5 and then introducing the gas phase product into the vaporizer 3.
The order between steps S1 and S2 and between steps S4 and S5 may be reversed or may be performed simultaneously.
Compared with the prior art, the method and the device can realize at least the following beneficial effects: 1. prolonging the service life of the catalyst. The number of catalyst changes is reduced.
2. The cost of the whole equipment can be reduced, and the production cost is reduced.
3. Ensure the continuity of production and improve the production efficiency.
4. The conversion rate of benzene and the quality of cyclohexane are improved.
In the description of the present application, the directions or positional relationships indicated by the words "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., are based on the exemplary directions or positional relationships shown in the drawings, are for convenience of description or simplifying the description of the embodiments of the present application, and do not indicate or imply that the apparatus or components referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present application.
The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present application, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art in a specific context.
In the description of the present specification, a particular feature, structure, material, or characteristic may be combined in any suitable manner in one or more embodiments or examples.
The foregoing is only a part of the embodiments of the present application, and it should be noted that, for those skilled in the art, other similar implementation means based on the technical ideas of the present application are adopted without departing from the technical ideas of the solutions of the present application, and also belong to the protection scope of the embodiments of the present application.

Claims (10)

1. A reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation, which is characterized by comprising:
the inlet of the vaporizer is connected with the benzene feeding pipe and the hydrogen feeding pipe;
the inlet of the reactor is connected with the outlet of the vaporizer;
a vapor-water separator having an inlet connected to the reactor and an outlet connected to the inlet of the vaporizer to receive and filter the vapor-phase product from the reactor and to deliver the vapor-phase product to the vaporizer;
and the inlet of the cooler is connected with the reactor, and the outlet of the cooler is connected with the discharge pipe.
2. The reaction device for preparing ethylcyclohexane by hydrogenating ethylbenzene according to claim 1, wherein the reactor comprises a first reactor and a second reactor which are mutually connected in series, wherein an inlet of the first reactor is connected with the vaporizer, an outlet of the first reactor is connected with the vapor-water separator and the second reactor, an inlet of the second reactor is connected with the first reactor, and an outlet of the second reactor is connected with the vapor-water separator and the cooler.
3. The reaction device for preparing ethylcyclohexane by hydrogenating ethylbenzene according to claim 2, wherein the reactor further comprises a third reactor connected in series with the first reactor and the second reactor, wherein an inlet of the third reactor is connected with the second reactor, and an outlet is connected with the vaporizer and the cooler.
4. The reaction apparatus for producing ethylcyclohexane by hydrogenating ethylbenzene according to claim 3, wherein at least one stop valve is connected in series with one stop valve and one stop valve is connected in parallel with any one of the first reactor, the second reactor and the third reactor.
5. The reaction device for preparing ethylcyclohexane by hydrogenating ethylbenzene according to claim 4, wherein the vaporizer is further connected with an inlet of the second reactor through the stop valve, an outlet of the second reactor is connected with an inlet of the first reactor through the stop valve, and an outlet of the first reactor is connected with an inlet of the third reactor through the stop valve.
6. The reaction device for preparing ethylcyclohexane by hydrogenating ethylbenzene according to claim 3, wherein the first reactor and the second reactor are tubular reactors, and a catalyst and a diluent are arranged in the first reactor and the second reactor;
the third reactor is a tank reactor, and a catalyst is arranged in the third reactor.
7. The reaction device for preparing ethylcyclohexane by hydrogenating ethylbenzene according to claim 6, wherein the catalyst comprises nickel, and the catalyst is in the form of solid particles.
8. The reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation according to claim 1, further comprising a recovery pipe and a compressor, wherein both ends of the recovery pipe are respectively connected with the discharge pipe and the hydrogen feed pipe, and the compressor is arranged on the recovery pipe.
9. The reaction device for preparing ethylcyclohexane by hydrogenating ethylbenzene according to claim 1, wherein the reaction device further comprises a hydrogen buffer tank, an inlet of the hydrogen buffer tank is connected with the hydrogen feed pipe, and an outlet of the hydrogen buffer tank is connected with the vaporizer.
10. A synthesis method for preparing ethylcyclohexane by ethylbenzene hydrogenation, which is characterized by adopting the reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation according to any one of claims 1-9, and comprising the following steps:
introducing benzene into a vaporizer through a benzene feed line;
introducing hydrogen into the vaporizer through a hydrogen feed line;
the vaporized mixture of benzene and hydrogen generates liquid-phase products and gas-phase products in a reactor;
discharging the liquid phase product from the discharge pipe after passing through the cooler;
and filtering the gas phase product through a steam-water separator and then introducing the gas phase product into the vaporizer.
CN202310345980.8A 2023-03-31 2023-03-31 Reaction device for preparing ethylcyclohexane by ethylbenzene hydrogenation and synthesis method Pending CN116393046A (en)

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