CN111450779A - Reaction device and process for preparing ethylene by oxidative coupling of methane - Google Patents

Reaction device and process for preparing ethylene by oxidative coupling of methane Download PDF

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CN111450779A
CN111450779A CN202010304816.9A CN202010304816A CN111450779A CN 111450779 A CN111450779 A CN 111450779A CN 202010304816 A CN202010304816 A CN 202010304816A CN 111450779 A CN111450779 A CN 111450779A
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reaction
fixedly connected
layer
pipe
catalyst
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CN111450779B (en
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王鹏
余泽军
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Hubei Holy Spirit Technology Co ltd
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Anqing Zeyuan Chemical 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
    • B01J8/0015Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • 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
    • 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
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • 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
    • B01J8/16Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with particles being subjected to vibrations or pulsations
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2/00Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
    • C07C2/76Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation of hydrocarbons with partial elimination of hydrogen
    • C07C2/82Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation of hydrocarbons with partial elimination of hydrogen oxidative coupling
    • C07C2/84Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation of hydrocarbons with partial elimination of hydrogen oxidative coupling catalytic

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

Abstract

The invention belongs to the technical field of reaction for preparing ethylene by oxidative coupling of methane, and particularly relates to a reaction device and a process for preparing ethylene by oxidative coupling of methane; comprises a reaction barrel; a barrel cover is rotatably connected above the reaction barrel; a feed pipe is fixedly connected with the position of the center line of the barrel cover in the inner wall of the barrel cover, and the feed pipe is in a conical design; a feeding cover is sleeved above the feeding pipe; the inner wall of the feeding pipe is fixedly connected with uniformly arranged inclined plates which are arranged in a staggered manner; a reaction layer is fixedly connected in the inner wall of the reaction barrel below the feeding pipe; the invention mainly solves the problems that the existing reaction device for preparing ethylene by methane oxidative coupling has obvious hot spots in the process of preparing ethylene, when the filling amount of the catalyst is increased, the catalyst layer becomes thick, so a large amount of reaction heat is generated, and the reaction speed of the catalyst is accelerated to release more heat because the generated reaction heat can not be removed in time, so that the catalyst is sintered, and the reaction device is damaged.

Description

Reaction device and process for preparing ethylene by oxidative coupling of methane
Technical Field
The invention belongs to the technical field of reaction for preparing ethylene by oxidative coupling of methane, and particularly relates to a reaction device and a process for preparing ethylene by oxidative coupling of methane.
Background
Ethylene is an important product of petrochemical and organic chemical industries, and with the development of the world economy, the demand of ethylene increases year by year. In the future, the world ethylene production capacity will continue to increase faster, and the raw materials are lighter and more diversified. The natural gas resource is not only rich in source, but also clean and environment-friendly. Methane is the main component of natural gas, shale gas, coal bed gas and combustible ice. In the long run, the technology for preparing ethylene from methane has better development prospect. Compared with an indirect conversion method of natural gas, the method for preparing ethylene by Oxidative Coupling of Methane (OCM) can convert methane into ethylene by only one-step reaction, has the advantages of short flow and good economy, and the application of the OCM technology is a revolution in the development process of the traditional ethylene production process and is generally regarded by all countries in the world. At present, the high yield of ethylene is realized by improving the performance of the catalyst and optimizing the structure of the reactor by research and development units at home and abroad. The foreign OCM technology (US2017/0107162A1) was developed most typically by Siluria, and is currently under pilot development. The national institute of Chinese academy of sciences Lanzhou chemical and physical research (CN 1187118C, CN102093157A) develops a Na2WO3-Mn/SiO2 catalyst aiming at the OCM process, and has good application prospect. It is worth noting that the technology for preparing ethylene by anaerobic catalytic conversion developed by the institute of chemical and physical sciences of the Chinese academy of sciences has gained wide attention at home and abroad, and the introduction of preparing ethylene by oxidative coupling of methane can be referred to the journal: the technical progress of ethylene preparation by methane oxidative coupling of pani, Shanxi chemical industry, 2018 and 02, however, certain problems still exist in the current process of ethylene preparation by methane oxidative coupling, and the method specifically comprises the following aspects:
the reaction device for preparing ethylene by oxidative coupling of methane in the prior art has obvious hot spots in the process of preparing ethylene, and a catalyst layer can be thickened when the filling amount of the catalyst is increased, so that a large amount of reaction heat is generated, and the reaction speed of the catalyst is accelerated to emit more heat because the generated reaction heat cannot be removed in time, so that the catalyst generates a sintering phenomenon, and meanwhile, the reaction device can be damaged.
There are also some proposals for producing ethylene by oxidative coupling of methane, such as patent No. 201810430243.7, entitled a reaction apparatus and method for producing ethylene by oxidative coupling of methane, which uses a fluidized bed reactor to make catalyst particles move violently under the action of an ascending gas flow, but the catalyst does not completely react with methane during the reaction process, thereby resulting in the problem that the produced ethylene is not pure.
In view of the above, in order to overcome the above technical problems, the present invention designs and develops a reaction apparatus for preparing ethylene by oxidative coupling of methane and a process thereof, and a special reaction apparatus is manufactured, so as to solve the above technical problems.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a novel active light-emitting design method for a light source panel for traffic signs, which mainly solves the problems that the existing reaction device for preparing ethylene by methane oxidative coupling has obvious hot spots in the process of preparing ethylene, when the filling amount of a catalyst is increased, a catalyst layer becomes thick, so a large amount of reaction heat is generated, and the generated reaction heat cannot be removed in time, so that the reaction speed of the catalyst is accelerated to release more heat, so that the catalyst is sintered, and the reaction device is damaged.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a reaction device for preparing ethylene by oxidative coupling of methane, which is characterized in that: comprises a reaction barrel; a barrel cover is rotatably connected above the reaction barrel; a feed pipe is fixedly connected with the position of the center line of the barrel cover in the inner wall of the barrel cover, and the feed pipe is in a conical design; a feeding cover is sleeved above the feeding pipe; the inner wall of the feeding pipe is fixedly connected with uniformly arranged inclined plates which are arranged in a staggered manner; a reaction layer is fixedly connected in the inner wall of the reaction barrel below the feeding pipe; a sliding layer is rotatably connected above the reaction layer through a support rod, and the sliding layer is designed in an arc shape; the sliding layer is designed to be smooth and is not attached to the reaction layer; arc-shaped grooves which are uniformly distributed are formed in the inner wall of the sliding layer; the upper surface of the sliding layer is fixedly connected with an electric telescopic rod at the central line position of the sliding layer, and the electric telescopic rods are electrically connected with a controller through leads; the end surface of the top of the electric telescopic rod is rotatably connected with a port plug, and the port plug corresponds to the pipe orifice of the feeding pipe; a liquid storage tank is fixedly connected below the reaction layer, and cooling liquid is contained in the liquid storage tank; a temperature sensor is fixedly connected in the inner wall of the reaction barrel at the left side of the feeding pipe and is electrically connected with a controller through a lead; a first air pump is fixedly connected in the inner wall of the reaction barrel below the temperature sensor; the left side of the first air pump is fixedly connected with a first guide pipe, and the other end of the first guide pipe extends into the liquid storage tank; a first spiral pipe is fixedly connected in the liquid storage tank and is communicated with a first guide pipe; the first spiral pipe is made of copper-aluminum alloy; the other end of the first spiral pipe extends out of the liquid storage tank and extends to the upper part of the reaction layer;
when the reactor is used, firstly methane gas is introduced into the reaction barrel, the catalyst is injected into the feed pipe, the feed cover is closed, and the feed pipe is designed in a conical shape, and the inclined plates which are uniformly arranged are fixedly connected in the feed pipe, so that the falling speed of the catalyst can be reduced, make the catalyst roll slowly in the inlet tube, when the catalyst rolls to the sliding layer on, because the arc wall of evenly arranging has been seted up in the sliding layer inner wall, and smooth design, the catalyst can be through the even arc wall that evenly arranges drop to the reaction layer upper surface, can prevent at this in-process that the catalyst from piling up and producing the thick layer, thereby improve the reaction heat of catalyst, when the temperature in the reaction barrel is sensed to temperature-sensing ware, controller control electric telescopic handle stretches this moment, stop stretching when the mouth stopper contacts with the mouth of pipe of inlet pipe, can prevent that the content of catalyst from increasing once more in this in-process, thereby accelerate reaction rate, produce a large amount of reaction heat, make the catalyst appear sintering phenomenon, can also prevent simultaneously that the reaction heat temperature that the reaction produced is too high can cause the damage to the reaction barrel, the work of first air pump of controller control simultaneously, can store up the gaseous suction through first pipe in the in a large amount of reaction heat in the in-process of first air pump work In the first spiral pipe of liquid incasement, because the splendid attire has the coolant liquid in the liquid reserve tank, thereby can reduce the gaseous temperature in the first spiral pipe, because first spiral pipe is made for copper aluminium alloy, thereby can improve the absorptive capacity of first spiral pipe, at the cooling of cooperation coolant liquid to first spiral pipe, can further reduce gaseous temperature, thereby prevent gaseous high temperature, accelerate the reaction rate of methane and catalyst, cause the influence to reaction barrel and catalyst, can get into the reaction layer top through first spiral pipe after gaseous process liquid reserve tank, with this circulation.
Preferably, the arc-shaped grooves uniformly arranged in the inner wall of the sliding layer are all arranged in a staggered manner; during operation, because the arc-shaped grooves which are uniformly arranged and are arranged in the inner wall of the sliding layer are arranged in a staggered manner, the catalyst can be uniformly arranged on the surface of the reaction layer in the process of rolling off the catalyst, so that the catalyst can be prevented from being unevenly distributed in the process, the reaction speed of the catalyst is different, and the phenomenon of hot spots appears on the reaction layer.
Preferably, an air groove is formed in the inner wall of the reaction layer; the first spiral pipe extends into the air tank; uniformly distributed air holes are formed in the inner wall of the air groove and are communicated with the cavity above the reaction layer; a support rod fixedly connected with the bottom of the sliding layer extends into the air groove; the outer surface of one side of the support rod extending into the air groove is fixedly connected with a rotating wheel; the lower surface of the sliding layer is fixedly connected with stirring rods which are uniformly arranged; when the catalyst sintering device works, the first spiral pipe extends into the gas tank, after gas in the first spiral pipe enters the gas tank, the gas in the gas tank can be sprayed to the reaction layer through the uniformly arranged gas holes, the catalyst above the reaction layer can be blown away in the process, so that the catalyst is prevented from being accumulated, the reaction speed of the catalyst reaction is synchronous, and the catalyst sintering phenomenon is caused, because the rotating wheel is fixedly connected to the outer surface of one side of the support rod extending into the gas tank, the rotating wheel can be impacted in the process of rotating the gas in the gas tank, the sliding layer can be driven to rotate after the rotating wheel is impacted, the catalyst falling from the feeding pipe can be blown away in the rotating process of the sliding layer, so that the catalyst is prevented from being accumulated into blocks to influence the reaction effect, because the lower surface of the sliding layer is fixedly connected with uniformly arranged stirring rods, the uniformly arranged stirring rods can be driven to rotate in the rotating process of the sliding layer, the catalyst on the reaction layer can be stirred at the pivoted in-process of stirring rod, can flatten the catalyst to even thickness at this in-process to guarantee the reaction rate of catalyst, can also overturn the catalyst simultaneously, can prevent that the catalyst from keeping a state always at this in-process, produced reaction heat can cause the damage to the reaction layer.
Preferably, a spring is fixedly connected between every two air holes; a vibration layer is fixedly connected above each spring and is mutually attached to the uniformly arranged stirring rods; the stirring rod is designed to be elastic; when the device works, the vibration layer is fixedly connected above the reaction layer through the spring, when the uniformly arranged air holes jet air outwards, the vibration layer can be impacted, the vibration layer can vibrate after the vibration layer is impacted, the catalyst above the vibration layer can jump in the vibration process of the vibration layer, the damage to a reaction barrel caused by burning points formed by the accumulated catalyst can be further prevented in the process, the vibration layer can be indirectly pressed in the rotating process of the stirring rod due to the mutual attachment of the stirring rod and the vibration layer, the vibration degree of the vibration layer can be improved and limited in the process, so that the catalyst is prevented from falling down from the vibration layer due to the excessively violent vibration of the vibration layer, and the vibration layer can have certain buffering capacity in the upward vibration process of the vibration layer due to the elastic design of the stirring rod, so that the vibration layer is prevented from excessively violent, the catalyst is made to fall off from the vibration layer, and the stirring rod can apply downward pressure to the vibration layer in the downward vibration process of the vibration layer, so that the pressure required by vibration can be provided for the vibration layer, and the vibration duration of the vibration layer is prolonged.
Preferably, the inner wall of the vibration layer is fixedly connected with uniformly arranged conveying pipes, and the conveying pipes extend to the lower part of the reaction layer; a collecting box is fixedly arranged above the liquid storage box, and the conveying pipes extend into the collecting box; the inner surface of the reaction barrel is fixedly connected with a second air pump on the inner surface of the right side of the reaction barrel; a second guide pipe is fixedly connected to the right side of the second air pump and extends into the liquid storage tank; a second spiral pipe is fixedly connected in the liquid storage tank and is communicated with a second guide pipe; the other end of the second spiral pipe extends to the top of the collecting box; an air outlet pipe is fixedly connected in the inner wall of the right side of the collecting box and extends to the outer side of the reaction barrel; during operation, as the conveying pipe fixedly connected with the inner wall of the vibration layer is communicated with the collecting box, the accumulated catalyst on the surface of the vibration layer can be shaken down into the collecting box through the conveying pipe in the rotating process of the stirring rod, excessive accumulation of the catalyst and over violent reaction can be prevented in the process, so that a large amount of reaction heat and catalyst sintering phenomena are generated, after the methane in the reaction barrel is completely reacted, the controller controls the second air pump to work, the gas above the reaction layer can be pumped into the second spiral pipe in the liquid storage box in the working process of the second air pump, the temperature of the gas after reaction can be reduced in the process, so that the flowing degree of the gas is reduced, as the second spiral pipe extends into the collecting box, when the gas flows into the collecting box, as the catalyst falling from the conveying pipe is stored in the collecting box, when the gas is contacted with the catalyst, can be for the gas of incomplete reaction carry out the secondary catalysis, can improve gaseous reaction degree at this in-process, prevent that gaseous reaction from making the ethylene that makes incompletely impure, can flow into the external world through the outlet duct after gaseous reaction, it can to collect through the collecting vessel.
Preferably, the first spiral pipe passes through the collection box; the first spiral pipe penetrates through the inner wall of one side of the collecting box and is provided with uniformly distributed through holes; during operation, because the first spiral pipe passes the one side surface of collecting box and offers the through-hole of evenly arranging, the gaseous through first spiral pipe can flow into in the collecting box through the through-hole of evenly arranging, can continue the reaction when gaseous and the catalyst contact in the collecting box, can improve the preparation efficiency of ethylene at this in-process, can also prevent that the heat that the catalyst emitted from excessively forms the sintering phenomenon simultaneously.
A process for preparing ethylene by oxidative coupling of methane, which is suitable for a reaction device for preparing ethylene by oxidative coupling of methane as claimed in any one of claims 1-6, and comprises the following steps:
s1: firstly, introducing methane gas into a reaction barrel, then injecting a catalyst into a feed pipe, and starting to react to prepare ethylene when the methane gas and the catalyst are opened;
s2: when a temperature sensor in the reaction barrel senses that the temperature in the reaction barrel is too high, the controller controls the electric telescopic rod to stretch until the opening plug is attached to the opening of the feeding pipe, and simultaneously controls the first air pump to work, and the first air pump can pump the gas generated in the reaction barrel into the liquid storage tank through the first guide pipe; plug up the inlet pipe through utilizing the mouth stopper and can block rolling of catalyst to can prevent the increase of catalyst content, make catalyst and methane reaction produce a large amount of reaction heats, through with the gaseous liquid reserve tank that lets in the reaction barrel, can reduce gaseous temperature, thereby can prevent that the high temperature from causing the influence to the reaction barrel.
S3: when the methane in the reaction barrel completely reacts with the catalyst, the controller controls the second air pump to work, the second air pump can pump the gas completely reacted into the liquid storage tank, and the gas enters the collection tank through the second spiral pipe after flowing into the liquid storage tank; the gas after reaction is introduced into the liquid storage tank, so that the temperature of the gas can be further reduced, and when the gas flows into the collecting tank, the reaction degree of methane and the catalyst can be further improved, so that the purity of the prepared ethylene can be improved;
and S4, when the gas flows into the collecting box, the gas can flow out of the reaction barrel through the gas outlet pipe, and when the gas flows out of the reaction barrel, the gas is recovered to obtain the ethylene.
The invention has the following beneficial effects:
1. according to the invention, the gas groove is arranged, when gas in the first spiral pipe enters the gas groove, the gas in the gas groove can be sprayed to the reaction layer through the uniformly arranged gas holes, and the catalyst above the reaction layer can be blown away in the process, so that the catalyst is prevented from being accumulated, the reaction speed of the catalyst reaction is synchronous, and the catalyst sintering phenomenon is caused.
2. The stirring rod is arranged, the stirring rod which is uniformly arranged can be driven to rotate in the rotating process of the sliding layer, the catalyst on the reaction layer can be stirred in the rotating process of the stirring rod, the catalyst can be flattened to uniform thickness in the process, the reaction speed of the catalyst is ensured, meanwhile, the catalyst can be overturned, the catalyst can be prevented from being kept in a state all the time in the process, the generated reaction heat can damage the reaction layer, the stirring rod is designed elastically, a certain buffering capacity can be provided for the vibration layer in the upward vibration process of the vibration layer, so that the vibration layer is prevented from vibrating too violently, the catalyst falls off the vibration layer, the stirring rod can apply downward pressure to the vibration layer in the downward vibration process of the vibration layer, so that the pressure required by vibration can be provided for the vibration layer, thereby improving the vibration duration of the vibration layer.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a front view of the reaction apparatus of the present invention;
FIG. 3 is a sectional view of a reaction apparatus of the present invention;
FIG. 4 is an enlarged view of a portion of FIG. 3 at A;
FIG. 5 is an enlarged view of a portion of FIG. 3 at B;
in the figure: the reaction barrel comprises a reaction barrel 1, a reaction layer 11, an air tank 12, an air hole 13, a support rod 14, a rotating wheel 15, a sliding layer 16, an arc-shaped groove 17, an electric telescopic rod 18, a port plug 19, a stirring rod 191, a liquid storage tank 192, a temperature sensor 193, a first air pump 194, a first guide pipe 195, a first spiral pipe 196, a vibration layer 197, a conveying pipe 198, a collecting box 199, a second air pump 111, a second guide pipe 121, a second spiral pipe 131, an air outlet pipe 141, a through hole 151, a barrel cover 2, a feeding pipe 21, a feeding cover 22 and an inclined plate 23.
Detailed Description
A reaction apparatus for producing ethylene by oxidative coupling of methane according to one embodiment of the present invention will be described below with reference to FIGS. 1 to 5.
As shown in fig. 1 to fig. 5, the reaction apparatus for preparing ethylene by oxidative coupling of methane according to the present invention is characterized in that: comprises a reaction barrel 1; a barrel cover 2 is rotatably connected above the reaction barrel 1; a feeding pipe 21 is fixedly connected to the central line of the barrel cover 2 in the inner wall of the barrel cover 2, and the feeding pipe 21 is in a conical design; a feeding cover 22 is sleeved above the feeding pipe 21; the inner wall of the feeding pipe 21 is fixedly connected with uniformly arranged inclined plates 23, and the inclined plates 23 are arranged in a staggered manner; a reaction layer 11 is fixedly connected in the inner wall of the reaction barrel 1 below the feeding pipe 21; a sliding layer 16 is rotatably connected above the reaction layer 11 through a support rod 14, and the sliding layer 16 is designed in an arc shape; the sliding layer 16 is of smooth design and is not attached to the reaction layer 11; arc-shaped grooves 17 which are uniformly distributed are formed in the inner wall of the sliding layer 16; the upper surface of the sliding layer 16 is fixedly connected with an electric telescopic rod 18 at the central line position of the sliding layer 16, and the electric telescopic rods are electrically connected with a controller through leads; the end surface of the top of the electric telescopic rod 18 is rotatably connected with a port plug 19, and the port plug 19 corresponds to the pipe orifice of the feeding pipe 21; a liquid storage tank 192 is fixedly connected below the reaction layer 11, and cooling liquid is contained in the liquid storage tank 192; a temperature sensor 193 is fixedly connected in the inner wall of the reaction barrel 1 at the left side of the feeding pipe 21, and the temperature sensor 193 is electrically connected with a controller through a lead; a first air pump 194 is fixedly connected in the inner wall of the reaction barrel 1 below the temperature sensor 193; a first conduit 195 is fixedly connected to the left side of the first air pump 194, and the other end of the first conduit 195 extends into the liquid storage tank 192; a first spiral pipe 196 is fixedly connected in the liquid storage tank 192, and the first spiral pipe 196 is communicated with a first conduit 195; the first spiral pipe 196 is made of copper-aluminum alloy; the other end of the first spiral pipe 196 extends out of the liquid storage tank 192 and extends to the upper part of the reaction layer 11;
when the reactor is used, firstly methane gas is introduced into the reaction barrel 1, the catalyst is injected into the feed pipe 21, the feed cover 22 is closed, and the feed pipe 21 is in a conical design, and the inclined plates 23 which are uniformly arranged are fixedly connected in the feed pipe 21, so that the falling speed of the catalyst can be reduced, the catalyst is slowly rolled down in the feeding pipe 21, when the catalyst is rolled down on the sliding layer 16, because the arc-shaped grooves 17 which are uniformly arranged are arranged in the inner wall of the sliding layer 16 and are designed smoothly, the catalyst can uniformly fall down to the upper surface of the reaction layer 11 through the arc-shaped grooves 17 which are uniformly arranged, the catalyst can be prevented from being accumulated to generate a thick layer in the process, so the reaction heat of the catalyst is improved, when the temperature sensor 193 senses that the temperature in the reaction barrel 1 is overhigh, the controller controls the electric telescopic rod 18 to stretch at the moment, the stretching is stopped when the opening plug 19 is contacted with the pipe opening of the feeding pipe 21, the content of the catalyst can be prevented from being increased again in the process, so the reaction speed is accelerated, a large amount of reaction heat is generated, the catalyst is sintered, meanwhile, the phenomenon that the reaction heat generated by the reaction is overhigh temperature, which can cause damage to the reaction barrel 1 can be prevented, in the process of the work of first air pump 194 can be with producing the gaseous first spiral pipe 196 in the first pipe 195 suction liquid reserve tank 192 of a large amount of reaction heat, because the splendid attire has the coolant liquid in the liquid reserve tank 192, thereby can reduce the gaseous temperature in the first spiral pipe 196, because first spiral pipe 196 is made for copper-aluminum alloy, thereby can improve the absorptive capacity of first spiral pipe 196, at the cooling of cooperation coolant liquid to first spiral pipe 196, can further reduce gaseous temperature, thereby prevent gaseous high temperature, accelerate the reaction rate of methane and catalyst, cause the influence to retort 1 and catalyst, can get into reaction layer 11 top through first spiral pipe 196 after gaseous process liquid reserve tank 192, with this circulation.
As an embodiment of the present invention, the arc-shaped grooves 17 uniformly arranged in the inner wall of the sliding layer 16 are all arranged in a staggered manner; during operation, the arc-shaped grooves 17 which are uniformly arranged and are formed in the inner wall of the sliding layer 16 are all arranged in a staggered mode, so that the catalyst can be uniformly arranged on the surface of the reaction layer 11 in the process of rolling off the catalyst, the catalyst can be prevented from being distributed unevenly in the process, the reaction speed of the catalyst is different, and the phenomenon of hot spots appears on the reaction layer 11.
As an embodiment of the present invention, a gas groove 12 is opened in the inner wall of the reaction layer 11; the first spiral pipe 196 extends into the gas tank 12; uniformly arranged air holes 13 are formed in the inner wall of the air groove 12, and the air holes 13 are communicated with the cavity above the reaction layer 11; a support rod 14 fixedly connected with the bottom of the sliding layer 16 extends into the air groove 12; the outer surface of one side of the support rod 14 extending into the air groove 12 is fixedly connected with a rotating wheel 15; the lower surface of the sliding layer 16 is fixedly connected with stirring rods 191 which are uniformly arranged; when the catalyst sintering device works, because the first spiral pipe 196 extends into the gas tank 12, after the gas in the first spiral pipe 196 enters the gas tank 12, the gas in the gas tank 12 can be sprayed to the reaction layer 11 through the uniformly arranged gas holes 13, in the process, the catalyst above the reaction layer 11 can be blown away, so that the catalyst is prevented from being accumulated, the reaction speed of the catalyst reaction is synchronous, and the catalyst sintering phenomenon is caused, because the rotating wheel 15 is fixedly connected to the outer surface of one side of the support rod 14 extending into the gas tank 12, the rotating wheel 15 can be impacted in the process of rotating in the gas tank 12, the rotating wheel 15 can drive the sliding layer 16 to rotate after being impacted, the catalyst falling from the feed pipe 21 can be dispersed in the rotating process of the sliding layer 16, so that the catalyst is prevented from being accumulated into blocks to influence the reaction effect, because the uniformly arranged stirring rods 191 are fixedly connected to the lower surface of the sliding layer 16, the stirring rod 191 which is uniformly arranged can be driven to rotate in the rotating process of the sliding layer 16, the catalyst on the reaction layer 11 can be stirred in the rotating process of the stirring rod 191, the catalyst can be flattened to uniform thickness in the process, the reaction speed of the catalyst is guaranteed, meanwhile, the catalyst can be overturned, the catalyst can be prevented from being always kept in one state in the process, and the generated reaction heat can damage the reaction layer 11.
As an embodiment of the present invention, a spring is fixedly connected between every two of the air holes 13; a vibration layer 197 is fixedly connected above each spring, and the vibration layer 197 is mutually attached to the uniformly arranged stirring rods 191; the stirring rod 191 is of an elastic design; when the reactor works, the vibration layer 197 is fixedly connected above the reaction layer 11 through the spring, when the uniformly arranged air holes 13 inject air outwards, the vibration layer 197 can be impacted, the vibration layer 197 can vibrate after the impact on the vibration layer 197, the catalyst above the vibration layer 197 can bounce in the vibration process of the vibration layer 197, the damage to the reaction barrel 1 caused by burning points formed by catalyst accumulation can be further prevented in the process, because the stirring rod 191 and the vibration layer 197 are mutually attached, the vibration layer 197 can be indirectly pressed in the rotation process of the stirring rod 191, the vibration degree of the vibration layer 197 can be limited in the process, the vibration layer 197 is prevented from vibrating to shake the catalyst down to the vibration layer 197 too violently, because the stirring rod 191 is of elastic design, the vibration layer 197 can have certain buffer capacity in the upward vibration process, therefore, the vibrating layer 197 is prevented from vibrating too violently, so that the catalyst falls off the vibrating layer 197, and in the downward vibrating process of the vibrating layer 197, the stirring rod 191 can apply downward pressure to the vibrating layer 197, so that the pressure required by the vibration can be provided for the vibrating layer 197, and the vibrating duration of the vibrating layer 197 is prolonged.
As an embodiment of the invention, the inner wall of the vibration layer 197 is fixedly connected with evenly arranged conveying pipes 198, and the conveying pipes 198 extend to the lower part of the reaction layer 11; a collecting box 199 is fixedly arranged above the liquid storage box 192, and the conveying pipes 198 extend into the collecting box 199; the inner surface of the reaction barrel 1 is fixedly connected with a second air pump 111 on the inner surface of the right side of the reaction barrel 1; the right side of the second air pump 111 is fixedly connected with a second conduit 121, and the second conduit 121 extends into the liquid storage tank 192; the liquid storage tank 192 is fixedly connected with a second spiral pipe 131, and the second spiral pipe 131 is communicated with a second guide pipe 121; the other end of the second spiral pipe 131 extends to the top of the collection box 199; an air outlet pipe 141 is fixedly connected to the inner wall of the right side of the collecting box 199, and the air outlet pipe 141 extends to the outer side of the reaction barrel 1; during operation, as the conveying pipe 198 fixedly connected in the inner wall of the vibration layer 197 is communicated with the collection box 199, the accumulated catalyst on the surface of the vibration layer 197 can be shaken off into the collection box 199 through the conveying pipe 198 in the rotating process of the stirring rod 191, excessive accumulation and over-intense reaction of the catalyst can be prevented in the process, and thus a large amount of reaction heat and catalyst sintering phenomena can be generated, when the methane in the reaction barrel 1 is completely reacted, the controller controls the second air pump 111 to work, the gas above the reaction layer 11 can be pumped into the second spiral pipe 131 in the liquid storage box 192 in the working process of the second air pump 111, the temperature of the reacted gas can be reduced in the process, and thus the flowing degree of the gas is reduced, as the second spiral pipe 131 extends into the collection box 199, when the gas flows into the collection box 199, the catalyst falling from the conveying pipe 198 is stored in the collection box 199, when gas contacts with the catalyst, the gas which is not completely reacted can be catalyzed for the second time, the reaction degree of the gas can be improved in the process, the ethylene which is not completely made by the gas reaction is prevented from being impure, and after the gas reaction, the gas can flow into the outside through the gas outlet pipe 141 and can be collected through the collecting tank.
As an embodiment of the present invention, the first spiral pipe 196 is designed to pass through a collection box 199; the first spiral pipe 196 penetrates through the inner wall of one side of the collection box 199, and is provided with uniformly arranged through holes 151; in operation, since the first spiral pipe 196 penetrates the outer surface of one side of the collection box 199 to be provided with the uniformly arranged through holes 151, the gas passing through the first spiral pipe 196 can flow into the collection box 199 through the uniformly arranged through holes 151, and the gas can continuously react when contacting the catalyst in the collection box 199, the preparation efficiency of ethylene can be improved in the process, and the sintering phenomenon caused by excessive heat emitted by the catalyst can be prevented.
A process for preparing ethylene by oxidative coupling of methane, which is suitable for a reaction device for preparing ethylene by oxidative coupling of methane as claimed in any one of claims 1-6, and comprises the following steps:
s1: firstly, introducing methane gas into a reaction barrel, then injecting a catalyst into a feed pipe, and starting to react to prepare ethylene when the methane gas and the catalyst are opened;
s2: when a temperature sensor in the reaction barrel senses that the temperature in the reaction barrel is too high, the controller controls the electric telescopic rod to stretch until the opening plug is attached to the opening of the feeding pipe, and simultaneously controls the first air pump to work, and the first air pump can pump the gas generated in the reaction barrel into the liquid storage tank through the first guide pipe; plug up the inlet pipe through utilizing the mouth stopper and can block rolling of catalyst to can prevent the increase of catalyst content, make catalyst and methane reaction produce a large amount of reaction heats, through with the gaseous liquid reserve tank that lets in the reaction barrel, can reduce gaseous temperature, thereby can prevent that the high temperature from causing the influence to the reaction barrel.
S3: when the methane in the reaction barrel completely reacts with the catalyst, the controller controls the second air pump to work, the second air pump can pump the gas completely reacted into the liquid storage tank, and the gas enters the collection tank through the second spiral pipe after flowing into the liquid storage tank; the gas after reaction is introduced into the liquid storage tank, so that the temperature of the gas can be further reduced, and when the gas flows into the collecting tank, the reaction degree of methane and the catalyst can be further improved, so that the purity of the prepared ethylene can be improved;
and S4, when the gas flows into the collecting box, the gas can flow out of the reaction barrel through the gas outlet pipe, and when the gas flows out of the reaction barrel, the gas is recovered to obtain the ethylene.
The specific working process is as follows:
when the device is used, firstly methane gas is introduced into the reaction barrel 1, meanwhile, a catalyst is injected into the feed pipe 21, the feed cover 22 is closed, the feed pipe 21 is in a conical design, and the feed pipe 21 is fixedly connected with the inclined plates 23 which are uniformly arranged, so that the rolling speed of the catalyst can be slowed down, the catalyst can slowly roll down in the feed pipe 21, when the catalyst rolls down on the sliding layer 16, the inner wall of the sliding layer 16 is provided with the uniformly arranged arc-shaped grooves 17 and is smoothly designed, the catalyst can uniformly fall onto the upper surface of the reaction layer 11 through the uniformly arranged arc-shaped grooves 17, when the temperature sensor 193 senses that the temperature in the reaction barrel 1 is too high, the controller controls the electric telescopic rod 18 to stretch, when the opening plug 19 is in contact with the pipe opening of the feed pipe 21, the controller controls the first air pump 194 to work, and in the working process of the first air pump 194, gas which generates a large amount of reaction heat can be pumped into the first guide pipe 195 through the first guide pipe In the first spiral pipe 196 in the liquid reserve tank 192, because the splendid attire has the coolant liquid in the liquid reserve tank 192, thereby can reduce the temperature of gaseous in the first spiral pipe 196, because first spiral pipe 196 is made for the copper-aluminum alloy, thereby can improve the absorptive capacity of first spiral pipe 196, at the cooling of cooperation coolant liquid to first spiral pipe 196, can further reduce gaseous temperature, thereby prevent gaseous high temperature, accelerate the reaction rate of methane and catalyst, cause the influence to retort 1 and catalyst, can get into reaction layer 11 top through first spiral pipe 196 after gaseous process liquid reserve tank 192, with this circulation.
The principles, principal features and advantages of the invention have been shown and described. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. A reaction device for preparing ethylene by oxidative coupling of methane is characterized in that: comprises a reaction barrel (1); a barrel cover (2) is rotatably connected above the reaction barrel (1); a feeding pipe (21) is fixedly connected to the center line of the barrel cover (2) in the inner wall of the barrel cover (2), and the feeding pipe (21) is in a conical design; a feeding cover (22) is sleeved above the feeding pipe (21); the inner wall of the feeding pipe (21) is fixedly connected with uniformly arranged sloping plates (23), and the sloping plates (23) are arranged in a staggered manner; a reaction layer (11) is fixedly connected in the inner wall of the reaction barrel (1) below the feeding pipe (21); a sliding layer (16) is rotatably connected above the reaction layer (11) through a support rod (14), and the sliding layer (16) is designed in an arc shape; the sliding layer (16) is designed to be smooth and is not attached to the reaction layer (11); arc-shaped grooves (17) which are uniformly distributed are formed in the inner wall of the sliding layer (16); the upper surface of the sliding layer (16) is fixedly connected with an electric telescopic rod (18) at the central line position of the sliding layer (16), and the electric telescopic rods are electrically connected with a controller through leads; the end surface of the top of the electric telescopic rod (18) is rotatably connected with a port plug (19), and the port plug (19) corresponds to the pipe orifice of the feeding pipe (21); a liquid storage tank (192) is fixedly connected below the reaction layer (11), and cooling liquid is contained in the liquid storage tank (192); a temperature sensor (193) is fixedly connected in the inner wall of the reaction barrel (1) at the left side of the feeding pipe (21), and the temperature sensor (193) is electrically connected with a controller through a lead; a first air pump (194) is fixedly connected in the inner wall of the reaction barrel (1) below the temperature sensor (193); the left side of the first air pump (194) is fixedly connected with a first conduit (195), and the other end of the first conduit (195) extends into the liquid storage tank (192); a first spiral pipe (196) is fixedly connected in the liquid storage tank (192), and the first spiral pipe (196) is communicated with a first conduit (195); the first spiral pipe (196) is made of copper-aluminum alloy; the other end of the first spiral pipe (196) extends out of the liquid storage tank (192) and extends to the upper part of the reaction layer (11).
2. The reaction device for preparing ethylene by oxidative coupling of methane according to claim 1, wherein: the arc-shaped grooves (17) which are uniformly arranged and are arranged in the inner wall of the sliding layer (16) are all arranged in a staggered mode.
3. The reaction device for preparing ethylene by oxidative coupling of methane according to claim 1, wherein: an air groove (12) is formed in the inner wall of the reaction layer (11); the first spiral pipe (196) extends into the gas tank (12); uniformly arranged air holes (13) are formed in the inner wall of the air groove (12), and the air holes (13) are communicated with a cavity above the reaction layer (11); a support rod (14) fixedly connected with the bottom of the sliding layer (16) extends into the air groove (12); the outer surface of one side of the support rod (14) extending into the air groove (12) is fixedly connected with a rotating wheel (15); the lower surface of the sliding layer (16) is fixedly connected with stirring rods (191) which are uniformly arranged.
4. The reaction device for preparing ethylene by oxidative coupling of methane according to claim 3, wherein: a spring is fixedly connected between every two air holes (13); a vibration layer (197) is fixedly connected above each spring, and the vibration layer (197) is mutually attached to uniformly arranged stirring rods (191); the stirring rod (191) is of an elastic design.
5. The reaction device for preparing ethylene by oxidative coupling of methane according to claim 4, wherein: conveying pipes (198) which are uniformly distributed are fixedly connected in the inner wall of the vibration layer (197), and the conveying pipes (198) extend to the lower part of the reaction layer (11); a collecting box (199) is fixedly arranged above the liquid storage box (192), and conveying pipes (198) extend into the collecting box (199); the inner surface of the reaction barrel (1) is fixedly connected with a second air pump (111) on the inner surface of the right side of the reaction barrel (1); a second conduit (121) is fixedly connected to the right side of the second air pump (111), and the second conduit (121) extends into the liquid storage tank (192); the second spiral pipe (131) is fixedly connected in the liquid storage tank (192), and the second spiral pipe (131) is communicated with the second guide pipe (121); the other end of the second spiral pipe (131) extends to the top of the collection box (199); an air outlet pipe (141) is fixedly connected to the inner wall of the right side of the collecting box (199), and the air outlet pipe (141) extends to the outer side of the reaction barrel (1).
6. The reaction device for preparing ethylene by oxidative coupling of methane according to claim 5, wherein: the first spiral pipe (196) is designed to pass through a collection box (199); the first spiral pipe (196) penetrates through the inner wall of one side of the collecting box (199) and is provided with uniformly distributed through holes (151).
7. A preparation process for preparing ethylene by oxidative coupling of methane is characterized by comprising the following steps: the process is suitable for a reaction device for preparing ethylene by oxidative coupling of methane according to any one of claims 1 to 6, and comprises the following steps:
s1: firstly, introducing methane gas into a reaction barrel, then injecting a catalyst into a feed pipe, and starting to react to prepare ethylene when the methane gas and the catalyst are opened;
s2: when a temperature sensor in the reaction barrel senses that the temperature in the reaction barrel is too high, the controller controls the electric telescopic rod to stretch until the opening plug is attached to the opening of the feeding pipe, and simultaneously controls the first air pump to work, and the first air pump can pump the gas generated in the reaction barrel into the liquid storage tank through the first guide pipe;
s3: when the methane in the reaction barrel completely reacts with the catalyst, the controller controls the second air pump to work, the second air pump can pump the gas completely reacted into the liquid storage tank, and the gas enters the collection tank through the second spiral pipe after flowing into the liquid storage tank;
and S4, when the gas flows into the collecting box, the gas can flow out of the reaction barrel through the gas outlet pipe, and when the gas flows out of the reaction barrel, the gas is recovered to obtain the ethylene.
CN202010304816.9A 2020-04-17 2020-04-17 Reaction device and process for preparing ethylene by oxidative coupling of methane Active CN111450779B (en)

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