CN115990437B - Method, system and application for controlling feeding temperature and temperature rise of catalyst bed layer of each section in reactor - Google Patents
Method, system and application for controlling feeding temperature and temperature rise of catalyst bed layer of each section in reactor Download PDFInfo
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Abstract
The invention discloses a method, a system and an application for controlling the feeding temperature and the temperature rise of each section of catalyst bed in a reactor, wherein raw materials I and II are used as raw materials for reaction (particularly exothermic reaction), wherein raw materials II exchange heat with reaction products of each section of the reactor step by step, when the content of components reacting with raw materials II in the raw materials I changes to influence the temperature of each section of the reactor, the quantity of the reaction products removed from each section of heat exchange is controlled, and the quantity of the raw materials I removed from heat exchange is controlled, so as to maintain the temperature change of an inlet of each section of catalyst bed to be not more than +/-2% and the temperature rise change to be not more than +/-10%. Mainly solves the problems of uneven feeding temperature and temperature rise of each section of catalyst bed layer, low product yield and large energy consumption of the device in the prior art.
Description
Technical Field
The invention belongs to the field of chemical technology, and particularly relates to a temperature control method, a system and application for controlling feeding temperature and temperature rise of each section of catalyst bed in a reactor.
Background
In the prior art, when a multi-stage catalytic addition bed is adopted to carry out reaction (especially exothermic reaction), if the composition in the raw material is unstable, the inlet of each stage of catalyst bed in the reactor is difficult to control at the same temperature and the same temperature rise, for example, the technology of preparing ethylbenzene by using dilute ethylene gas phase method is easy to cause.
The technology for preparing ethylbenzene by using dilute ethylene gas phase is to directly add value to convert ethylene and benzene alkylation reaction in catalytic cracking byproducts of petroleum industry such as catalytic dry gas and the like into ethylbenzene as chemical products, effectively utilizes waste resources and reduces carbon emission.
CN1250494C discloses a process flow for preparing ethylbenzene by catalyzing dry gas, which has the advantages of no corrosion to pipeline, high recovery rate of benzene up to 99.5%, and low energy consumption. The catalyst includes water washing tower, hydrocarbonation reactor, coarse separation tower, absorption tower, benzene tower, toluene eliminating tower, ethylbenzene tower, polyethylbenzene eliminating tower, diethylbenzene tower, heat exchanger, machine pump and tank, and the catalyst dry gas is first water washed in the water washing tower to eliminate MDEA carried in the dry gas, then reacted in the hydrocarbonation reactor, the reacted product is heat exchanged in the heat exchanger, the condensed and cooled to 5-20 deg.c, the obtained product is first in the coarse separation tower, the non-condensated gas is then pumped in the absorption tower, the bottom liquid is then pumped in benzene tower, toluene eliminating tower, ethylbenzene tower, polyethylbenzene eliminating tower and diethylbenzene tower to separate out circulating benzene, toluene, ethylbenzene, propyl benzene, heavy component and diethylbenzene successively, and the reacted product is heat exchanged and then fed into benzene tower. The invention is suitable for modifying the existing process flow for preparing ethylbenzene by catalyzing dry gas.
CN101768043a discloses a method for preparing ethylbenzene by reacting dilute ethylene with benzene, which uses dilute ethylene in dry gas of oil refinery as raw material, and enters into alkylation reactor after washing and selectively removing propylene, and then carries out alkylation reaction with benzene in the presence of zeolite catalyst, and the alkylation reaction process adopts dry gas and/or low temperature gas phase benzene to extract heat, so as to reduce reaction temperature rise; after vapor-liquid separation of the hydrocarbonylation reaction product, tail gas is absorbed and discharged through a low temperature device, and the liquid product is sequentially separated into circulating benzene, ethylbenzene, propyl benzene, diethylbenzene and heavy components through a separation system; the diethylbenzene and benzene are mixed and enter an anti-alkylation reactor to carry out anti-alkylation reaction on a molecular sieve catalyst to further convert the diethylbenzene into ethylbenzene. The invention effectively reduces the benzene consumption and energy consumption in the process of preparing ethylbenzene from dilute ethylene, the ethylene conversion rate is not lower than 99%, the total selectivity of the ethylbenzene is not lower than 99%, the recovery rate of benzene carried by tail gas is not lower than 99.5%, and the xylene content in the ethylbenzene is below 800 ppm.
CN107935805A discloses a method for expanding the production of ethylbenzene by dry gas based on the rising ethylene content in raw materials, which belongs to the technical field of ethylbenzene by petrochemical dry gas. The rich solvent in the dry gas refining section is regenerated by combining two steps into one step, so that the back mixing of the circulating dry gas to the fed dry gas is eliminated, the impurity content in the purified dry gas is greatly reduced, and the byproduct content such as toluene, xylene and isopropylbenzene in the alkylation product is also greatly reduced. In the ethylbenzene refining section, the load of the benzene tower is relieved by adopting a method of recycling benzene through the rough separation tower top, the recycling benzene amount is increased, the benzene ratio in the alkylation reaction is ensured not to change before and after the expansion, and meanwhile, the reflux ratio of the ethylbenzene tower is reduced due to the reduction of the impurity amount in the ethylbenzene, and the load of the ethylbenzene tower is ensured. Therefore, by means of the system strategy of gradually eliminating the bottleneck, the production expansion can be realized under the conditions that main equipment is not replaced and unit consumption of the device is not increased.
The circulating benzene enters the heating furnace at low temperature, so that the load of the circulating benzene heating furnace is large, the quenching benzene is directly injected between sections, the total benzene ratio is increased, the load of the benzene tower is increased, and the energy consumption of the device is increased. In addition, the raw materials of the technologies directly enter the reactor at a single temperature after propylene removal, but because the ethylene content of the raw materials is not stable, the ethylene content generally fluctuates up and down by 10 to 60 percent, so that the inlet of each section of catalyst bed in the alkylation reactor is difficult to control at the same temperature and the same temperature rise. Generally, when the ethylene concentration is reduced, the temperature of the first stage bed layer of the reactor is increased, and the inlet temperature of the later stages of bed layers is difficult to reach the design requirement temperature, so that the ethylbenzene yield is reduced; when the concentration of ethylene is increased, the inlet temperature of a bed layer at the later sections of the reactor exceeds the design requirement temperature, the side reaction is increased, the concentration of key impurity dimethylbenzene is increased, and the catalyst deactivation is accelerated.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a method, a system and application for controlling the feeding temperature and the temperature rise of each section of catalyst bed in a reactor. The method takes a raw material I and a raw material II as raw materials to carry out reaction (particularly exothermic reaction), wherein the raw material II exchanges heat with the reaction products of each section of the reactor step by step, when the content of components reacting with the raw material II in the raw material I changes to influence the temperature of each section of the reactor, the quantity of the reaction products of each section of the heat exchange removal is controlled, and the quantity of the raw material I of the heat exchange removal is controlled, so as to maintain the temperature change of an inlet of each section of the catalyst bed layer to be not more than +/-2 percent and the temperature rise change to be not more than +/-10 percent. Mainly solves the problems of uneven feeding temperature and temperature rise of each section of catalyst bed layer, low product yield and large energy consumption of the device in the prior art.
It is an object of the present invention to provide a method for controlling the feed temperature and temperature rise of each section of catalyst bed in a reactor, comprising: carrying out exothermic reaction on a raw material I and a raw material II in a reactor containing N sections of catalyst beds, wherein the raw material I enters the reactor from each section of catalyst bed in N strands respectively and independently, the raw material II enters the reactor from the 1 st section of catalyst bed (in a one-strand manner), reaction products are led out from the lower part of each section of catalyst bed, and the raw material II exchanges heat with each section of reaction products sequentially from bottom to top; wherein:
the reaction products of the 1 st-N-1 st section catalyst bed are recycled to the reactor after heat exchange (preferably recycled to the reactor from the upper part of the next section catalyst bed), and the reaction products of the N th section are extracted after heat exchange;
optionally cooling the heat-exchanged raw material II by adopting a cooling medium after each heat exchange, and finally, introducing the heat-exchanged raw material II into the reactor from a section 1 catalyst bed after optional heating treatment;
the catalyst bed layers of the reactor are a1 st section catalyst bed layer, a2 nd section catalyst bed layer, a3 rd section catalyst bed layer, … th section catalyst bed layer and an N th section catalyst bed layer from top to bottom in sequence.
In the step (2), the heat exchange is performed between the raw material II and the reaction products led out from the N-th section catalyst bed, …, the 3-rd section catalyst bed, the 2-th section catalyst bed and the 1-th section catalyst bed in sequence in a one-stream mode. The raw material I contains a component capable of reacting with the raw material II, and can also contain other components besides the component, and the raw material I preferably contains 1-99 wt% of the component capable of reacting with the raw material II. The reactor is a multistage fixed bed reactor, such as an axial multistage fixed bed reactor. Preferably, feedstock I is dilute ethylene and feedstock II is benzene.
In a preferred embodiment, the feedstock I is apportioned between the segments of the reactor (i.e. each segment of the catalyst bed) and the feed amount is obtained according to formulas (1) and (2):
In the formulas (1) and (2), alpha is the distribution coefficient of the raw material I, and alpha is more than or equal to 0.5 and less than or equal to 1.5; n 1 is the molar feed amount of the component reacting with the raw material II in the first section of raw material I, and mol/h; n Total is the total molar feed amount of the components in the raw material I which react with the raw material II, mol/h; n N is the molar feed amount of the component reacting with the raw material II in the N-th section of raw material I, and mol/h; n N-1 is the molar feed amount of the component in the N-1 th section raw material I which reacts with the raw material II, and mol/h; n is more than or equal to 2.
Preferably, α+.1 is used, as the inventors have experimentally found that the effect is better than α=1 when α+.1.
In a preferred embodiment, the starting material I comprises a component which can react with the starting material II and optionally further components, preferably the starting material I comprises 1 to 99% by weight of a component which can react with the starting material II.
In a preferred embodiment, the feedstock II is cooled at least once after each heat exchange with the 2 nd to N-stage reaction products, which are the reaction products of the 2 nd to N-stage catalyst beds.
Wherein the temperature of the raw material II is controlled by exchanging heat between the cooling medium and the raw material II. The heat exchange efficiency of the heat exchange material II on the residual reaction products can be improved after the heat exchange material II is cooled.
In a further preferred embodiment, the feedstock II after heat exchange with the reaction product of stage 2 is cooled by means of a cooling medium, wherein the reaction product of stage 2 refers to the reaction product exiting from the catalyst bed of stage 2.
In a further preferred embodiment, the cooling is performed in a cooler, on which a temperature control unit is arranged for controlling the flow of the cooling medium in order to control the temperature of the raw material II at the outlet of the cooler.
In a preferred embodiment, the heat treatment is performed in a furnace.
Wherein a gas phase reaction, preferably an exothermic reaction, is carried out in the reactor.
In a preferred embodiment, the temperature of each stage of reaction product after heat exchange is controlled to be 250-450 ℃, and/or the feeding temperature above each stage of catalyst bed is controlled to be 250-450 ℃ independently, and/or the feeding pressure above each stage of catalyst bed is controlled to be 0.5-2.0 MPaG; and/or controlling the temperature of each section of catalyst bed to be 5-30 ℃.
In a further preferred embodiment, the temperature of the reaction product of each stage after heat exchange is controlled to be 300-400 ℃, and/or the feeding temperature above each stage of catalyst bed is controlled to be 300-400 ℃ independently, and/or the feeding pressure above each stage of catalyst bed is controlled to be 0.8-1.5 MPaG; and/or controlling the temperature of each section of catalyst bed to be 10-26 ℃.
For example, the temperature of each stage of reaction product after heat exchange is controlled to 300 ℃, 320 ℃, 340 ℃, 360 ℃, 380 ℃ or 400 ℃, and/or the feed temperature above each stage of catalyst bed is controlled to 300 ℃, 320 ℃, 340 ℃, 360 ℃, 380 ℃ or 400 ℃ independently, and/or the feed pressure above each stage of catalyst bed is controlled to 0.8MPaG, 1MPaG, 1.2MPaG, 1.4MPaG or 1.5MPaG; and/or controlling the temperature of each stage of catalyst bed to be 10 ℃, 12 ℃,14 ℃, 16 ℃, 18 ℃,20 ℃,22 ℃, 24 ℃ or 26 ℃.
Wherein each section of reaction product refers to the reaction product of each section of catalyst bed, the feeding temperature above the 1 st section of catalyst bed refers to the temperature after the raw material I and the raw material II entering the 1 st section of catalyst bed are mixed, and the feeding temperature above the 2 nd to N sections of catalyst bed refers to the temperature after the raw material I entering the section of catalyst bed and the reaction product after the heat exchange of the last section of catalyst bed are mixed.
In a preferred embodiment, when the content of the component reacting with the raw material II in the raw material I is changed, the variation in the feeding temperature of each stage of the catalyst bed is controlled to be not more than + -2% (preferably not more than + -1%, e.g., unchanged) and the variation in the temperature rise of each stage of the catalyst bed is controlled to be not more than + -10% (preferably not more than + -8%, e.g., not more than 1%) by adjusting at least one of the flow rate of the reaction product per stage, the flow rate of the raw material II, the heating temperature of the raw material II, and the flow rate of the cooling medium.
Among them, the main reason for the variation in the content of the component reacting with the raw material II in the raw material I is influenced by the upstream reaction thereof.
In a further preferred embodiment, as the amount of components in feedstock I that react with feedstock II increases, the feed temperature change per stage of catalyst bed is controlled to be no more than ±2% (preferably no more than ±1%, e.g., constant) and the temperature rise per stage of catalyst bed is controlled to be no more than ±10% (preferably no more than ±8%, e.g., no more than 1%) by at least one of the following operations: the flow rate of the reaction product led out by each section of catalyst bed layer is increased, the flow rate of the raw material II exchanging heat with each section of reaction product is increased, and the flow rate of the cooling medium is increased.
In a still further preferred embodiment, as the level of components in feedstock I that react with feedstock II is reduced, the feed temperature change per stage catalyst bed is controlled to be no more than ±2% (preferably no more than ±1%, e.g., constant) and the temperature rise per stage catalyst bed is controlled to be no more than ±10% (preferably no more than ±8%, e.g., no more than 1%) by at least one of the following operations: reducing the flow of reaction products led out from each section of catalyst bed, reducing the flow of raw material II exchanging heat with each section of reaction products, and improving the heating treatment temperature before the raw material II enters the 1 st section of catalyst bed.
In the present application, each stage of reaction product refers to a reaction product led out from each stage of catalyst bed.
In a preferred embodiment:
When the mass concentration of the component reacting with the raw material II in the raw material I is increased by 0.1% -60%, the feed temperature change of each catalyst bed is controlled to be not more than +/-2% (preferably not more than +/-1%, such as not changed) and the temperature rise of each catalyst bed is controlled to be not more than +/-10% (preferably not more than +/-8%, such as not more than 1%) by at least one of the following operations: the flow rate of each section of reaction product is increased by 0.1 to 50 percent, the flow rate of the raw material II which exchanges heat with each section of reaction product is respectively and independently increased by 0.1 to 50 percent, and the flow rate of a cooling medium is increased by 0.1 to 100 percent; or alternatively, the first and second heat exchangers may be,
When the mass concentration of the component reacting with the raw material II in the raw material I is reduced by 0.1% -60%, the feed temperature change of each catalyst bed is controlled to be not more than +/-2% (preferably not more than +/-1%, for example, unchanged) and the temperature rise change of each catalyst bed is controlled to be not more than +/-10% (preferably not more than +/-8%, for example, not more than 1%) by at least one of the following operations: the heating treatment temperature (especially the outlet temperature of a heating furnace) is increased by 0.1 to 20 percent, the flow rate of each stage of reaction product is reduced by 0.1 to 80 percent, and the flow rate of the raw material II which exchanges heat with each stage of reaction product is respectively and independently reduced by 0.1 to 80 percent.
In a further preferred embodiment:
When the mass concentration of the component reacting with the raw material II in the raw material I is increased by 5% -30%, the feed temperature change of each catalyst bed is controlled to be not more than +/-2% (preferably not more than +/-1%, such as not changed) and the temperature rise change of each catalyst bed is controlled to be not more than +/-10% (preferably not more than +/-8%, such as not more than 1%) by at least one of the following operations: the flow rate of each section of reaction product is increased by 3-20%, the flow rate of the raw material II which exchanges heat with each section of reaction product is respectively and independently increased by 3-20%, and the flow rate of the cooling medium is increased by 10-50%; for example, the flow rate of each stage of reaction product is increased by 3%, 5%, 8%, 10%, 12%, 15%, 18% or 20%, the flow rate of the raw material II subjected to heat exchange with each stage of reaction product is independently increased by 3%, 5%, 8%, 10%, 12%, 15%, 18% or 20%, and the flow rate of the cooling medium is increased by 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%, respectively;
Or alternatively, the first and second heat exchangers may be,
When the mass concentration of the component reacting with the raw material II in the raw material I is reduced by 5% -30%, the feed temperature change of each catalyst bed is controlled to be not more than +/-2% (preferably not more than +/-1%, such as not changed) and the temperature rise change of each catalyst bed is controlled to be not more than +/-10% (preferably not more than +/-8%, such as not more than 1%) by at least one of the following operations: the heating treatment temperature (especially the outlet temperature of a heating furnace) is increased by 5 to 10 percent, the flow rate of each section of reaction product is reduced by 10 to 60 percent, and the flow rate of the raw material II which exchanges heat with each section of reaction product is respectively and independently reduced by 10 to 60 percent; for example, the heat treatment temperature (especially the furnace outlet temperature) is increased by 5%, 6%, 7%, 8%, 9% or 10%, the flow rate of each stage of the reaction product is reduced by 10%, 20%, 30%, 40%, 50% or 60%, and the flow rate of the raw material II which exchanges heat with each stage of the reaction product is reduced by 10%, 20%, 30%, 40%, 50% or 60%, respectively, independently.
In a preferred embodiment, the heat exchange treatment is performed in a heat exchanger, preferably N heat exchangers are used for the heat exchange treatment of each reaction product, more preferably, the raw material II sequentially passes through the N heat exchangers from bottom to top and is used for sequentially exchanging heat with the N-th to 1-th reaction products.
In a further preferred embodiment, a bypass line I is provided at the reaction product inlet of the section of each heat exchanger, on which bypass line I a flow regulating valve is provided; and/or a bypass pipeline II is arranged at the inlet of the raw material II of each heat exchanger, and a flow regulating valve is arranged on the bypass pipeline II.
In a further preferred embodiment, the flow of each stage of reaction product is controlled independently of the flow of its corresponding bypass line I and/or the flow of the feed II heat exchanged with each stage of reaction product is controlled by the flow of the bypass line II on each heat exchanger.
Preferably, the flow rate of each reaction product is increased by decreasing the flow rate of the bypass line I (adjusting the bypass I flow rate adjusting valve opening), and the flow rate of each reaction product is decreased by increasing the flow rate of the bypass line I (adjusting the bypass I flow rate adjusting valve opening); and/or the flow rate of the raw material II entering each heat exchanger is increased by reducing the flow rate of the bypass pipeline II (adjusting the valve opening of the bypass II flow rate adjusting valve), and the flow rate of the raw material II entering each heat exchanger is reduced by increasing the flow rate of the bypass pipeline II (adjusting the valve opening of the bypass II flow rate adjusting valve).
It is a second object of the present invention to provide a system for controlling the temperature and temperature rise of each catalyst bed in a reactor, preferably for carrying out one of the methods of the present invention, the system comprising a reactor comprising N catalyst beds, a feed I inlet being provided above each catalyst bed, a product outlet for the reaction product of the reaction zone being provided below each catalyst bed, a product recycle inlet for the reaction product of the previous reaction zone being provided above the 2 nd to N catalyst beds, the product outlets for the reaction products of the 1 st to N-1 th stages being connected to the product recycle inlet for the reaction product of the previous stage by a recycle conduit, the recycle conduit being provided with a heat exchanger.
In a preferred embodiment, a feed II inlet is provided above the 1 st stage catalyst bed of the reactor, preferably at the top of the reactor.
In a preferred embodiment, a feed withdrawal line is provided below the nth stage catalyst bed, preferably at the bottom of the reactor.
In a further preferred embodiment, a heat exchanger is provided on the material withdrawal line.
In a preferred embodiment, all heat exchangers are connected via a feed II feed pipe which further extends to the feed II inlet of the reactor, forming a feed channel for feed II.
In this way, the raw material II passes through all heat exchangers step by step, and heat exchange with each section of reaction product is realized.
In a further preferred embodiment, a heating device (preferably a heating furnace) is arranged on the feed pipe for the raw material II after the last heat exchanger in the flow direction of the raw material II.
In a further preferred embodiment, at least one cooling device is arranged on the feed II feed line between all heat exchangers, preferably between the heat exchanger of the 1 st stage catalyst bed and the heat exchanger of the 2 nd stage catalyst bed.
In the present invention, the material I may be described as a material I, and the material II may be described as a material II.
In a preferred embodiment, a bypass line I is provided at the reaction product inlet of the section of each heat exchanger, on which bypass line I a flow regulating valve is provided.
In a further preferred embodiment, a bypass line II is provided at the inlet of the feed II to each heat exchanger, on which bypass line II a flow control valve is provided.
It is a further object of the present invention to provide the use of the process according to one of the objects of the present invention or of the system according to two of the objects of the present invention in a gas or liquid phase exothermic reaction, in particular in the production of ethylbenzene from dilute ethylene.
In a preferred embodiment, when applied to the production of ethylbenzene from dilute ethylene, the process for producing ethylbenzene from dilute ethylene comprises: carrying out exothermic reaction in a reactor containing N sections of catalyst beds by taking dilute ethylene and benzene as raw materials, wherein the dilute ethylene enters the reactor from each section of catalyst bed in N strands respectively and independently, benzene enters the reactor from the 1 st section of catalyst bed (in a one-strand manner), reaction products are led out from the lower part of each section of catalyst bed, and the benzene exchanges heat with each section of reaction products in sequence from bottom to top; wherein:
the reaction products of the 1 st-N-1 st section catalyst bed are recycled to the reactor after heat exchange (preferably recycled to the reactor from the upper part of the next section catalyst bed), and the reaction products of the N th section are extracted after heat exchange;
Optionally cooling the heat-exchanged benzene by adopting a cooling medium after each heat exchange, and finally, introducing the benzene into the reactor from the section 1 catalyst bed after optional heating treatment;
the catalyst bed layers of the reactor are a1 st section catalyst bed layer, a2 nd section catalyst bed layer, a3 rd section catalyst bed layer, … th section catalyst bed layer and an N th section catalyst bed layer from top to bottom in sequence.
In a preferred embodiment, the molar ratio of benzene to ethylene is from 2 to 7 and the weight space velocity of ethylene is from 0.3 to 2.0h -1.
In the present invention:
When the ethylene concentration in the dilute ethylene increases by 0.1-60% due to upstream fluctuation mass concentration, reducing the opening of a bypass valve of a reaction product to reduce the flow rate of the bypass reaction product by 0.1-50%, reducing the opening of a flow rate regulating valve of a benzene bypass to reduce the flow rate of the benzene bypass by 0.1-50%, and increasing the flow rate of a cooling medium by 0.1-100%; when the ethylene concentration in the dilute ethylene is reduced by 0.1-60% due to upstream fluctuation mass concentration, the outlet temperature of the heating device is increased by 0.1-20%, and meanwhile, the opening of the reaction product bypass flow regulating valve is increased, so that the reaction product bypass flow is increased by 0.1-80%, and the opening of the benzene bypass flow regulating valve is increased, so that the benzene bypass flow is increased by 0.1-80%.
Preferably, when the mass concentration of ethylene in the dilute ethylene is increased by 5% -30%, the opening of a reaction product bypass valve is reduced, so that the flow rate of the bypass reaction product is reduced by 3% -20%, and meanwhile, the opening of a benzene bypass flow rate regulating valve is reduced, so that the flow rate of the benzene bypass is reduced by 3% -20%, and the flow rate of a cooling medium is increased by 10% -50%; when the ethylene concentration in the dilute ethylene is reduced by 5% -30% due to upstream fluctuation mass concentration, the outlet temperature of the heating furnace is increased by 5% -10%, meanwhile, the opening of a reaction product bypass flow regulating valve is increased, the reaction product bypass flow is increased by 10% -60%, and the opening of a benzene bypass flow regulating valve is increased, so that the benzene bypass flow is increased by 10% -60%.
Wherein the dilute ethylene is derived from FCC dry gas, DCC dry gas, crude cracked gas, and the like.
In the prior art, dilute ethylene is generally fed into an alkylation reactor in multiple strands at a single temperature of 10-40 ℃ after propylene removal. Part of low-temperature benzene from the benzene tower is taken as interstage quenching benzene, and the other part of the low-temperature benzene is heated in a circulating benzene heating furnace and then mixed with 1 st dilute ethylene at a1 st stage bed inlet to reach the reaction required temperature, and enters a reactor for reaction. The low-temperature dilute ethylene and the quenching benzene from the 2 nd section to the N th section are mixed with high-temperature reaction gas from the catalyst bed layer of the previous section, and the reaction temperature is reduced to the required temperature and enters the catalyst bed layer of the next section. The temperature and the feeding amount designed according to the ethylene content in the dilute ethylene ensure that the temperature change of the inlet of each section of catalyst bed layer is not more than +/-2 percent and the temperature rise change is not more than +/-10 percent, and can ensure that higher ethylbenzene yield and high utilization rate of the catalyst can be obtained. Because the ethylene content in the catalytic dry gas of the refinery is unstable, the ethylene content generally fluctuates about 10-60%, so that the inlet of each section of catalyst bed in the alkylation reactor is difficult to control at almost unchanged temperature due to the great change of the ethylene concentration, the temperature rise of the catalyst bed is also greatly different, when the ethylene concentration in the catalytic dry gas is lower than a design value, the inlet temperature of the reactor bed is lower than the design requirement temperature, and the ethylbenzene yield is reduced; when the concentration of ethylene in the catalytic dry gas is higher than a design value, the inlet temperature of a reactor bed layer exceeds the design requirement temperature, the side reaction is increased, and the catalyst deactivation is accelerated. In addition, because the circulating benzene enters the heating furnace at low temperature, the load of the circulating benzene heating furnace is large, and the quenching benzene is directly injected between sections, so that the total benzene ratio is increased, the load of the benzene tower is increased, and the energy consumption of the device is increased.
When the method or the system is adopted to prepare ethylbenzene from dilute ethylene, low-temperature benzene from the benzene tower is subjected to heat exchange with each section of reaction product step by step, the temperature of the benzene is increased step by step, and the heat released by alkylation reaction is fully recovered before the benzene enters a circulating benzene heating furnace, so that the heat load of the heating furnace is greatly reduced, meanwhile, the use of quenching benzene among sections is avoided, the benzene ratio is reduced, and the load of the benzene tower is reduced. All heat exchange equipment is provided with a reaction product outlet temperature control device, and when the concentration of ethylene in the raw material is changed, the change of the inlet temperature of each section of the catalyst is not more than +/-2% and the change of the bed temperature rise is not more than +/-10% by adjusting the feeding temperature of benzene in the reactor and/or the outlet temperature of each reaction product. When the ethylene concentration in the raw material is lower than the design value, the temperature of the circulating benzene entering the reactor is increased through a heating furnace and/or the bypass flow of the reaction product is increased, so that the inlet temperature of each section of bed layer is ensured to reach the design temperature; when the ethylene concentration is higher than the design value, the inlet temperature of each section of bed layer can be ensured not to exceed the design requirement temperature by reducing the benzene bypass flow and/or increasing the cooling medium flow.
By adopting the method, the alkylation reaction system is adapted to the ethylene concentration change of dilute ethylene in a wider range, the temperature and the temperature rise of the inlet of the bed layer are precisely controlled, the reaction heat is effectively recovered, the styrene ratio is reduced, the load of a heating furnace and a benzene tower is reduced, the ethylbenzene yield is improved by 5-20%, the comprehensive energy consumption is reduced by 10-50%, and a better technical effect is obtained.
The endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. In the following, the individual technical solutions can in principle be combined with one another to give new technical solutions, which should also be regarded as specifically disclosed herein.
Compared with the prior art, the invention has the following beneficial effects:
(1) The low-temperature raw material II (such as benzene) is subjected to heat exchange with each section of reaction product step by step, the temperature of the raw material II (such as benzene) is increased step by step, the heat released by the reaction is fully recovered before the raw material II enters the heating device, so that the heat load of the heating device is greatly reduced, meanwhile, the use of quenching raw material II (such as benzene) between sections is avoided, the benzene ratio is reduced in the process of preparing ethylbenzene from dilute ethylene, and the load of a benzene tower is reduced.
(2) By adopting the method or the system, the reaction system (such as an alkylation reaction system) adapts to the concentration change of components (such as ethylene) in a wider range of the raw material I, the inlet temperature and the temperature rise of a bed layer are precisely controlled, and the reaction heat is effectively recovered;
(3) In the process of preparing ethylbenzene from dilute ethylene, the styrene ratio is reduced (high styrene ratio can cause low ethylbenzene yield), the load of a heating furnace and a benzene tower is reduced, the ethylbenzene yield can be improved by 5-20%, the comprehensive energy consumption is reduced by 10-50%, and a better technical effect is obtained.
Drawings
FIG. 1 shows a schematic diagram of the system of the present invention;
Fig. 2 shows a schematic diagram of a system according to the prior art.
1-Reactor, 2-heating device, 3-heat exchanger, 4-cooler, 5-raw material I inlet, 6-product outlet, 7-product circulation inlet, 8-circulation pipeline, 9-material extraction pipeline, 10-raw material II inlet, 11-raw material II inlet pipe, 12-cooling medium, a-raw material I (such as dilute ethylene), b-raw material II (such as benzene), c-h are the 1 st-N section catalyst beds in turn.
When the method is applied to the preparation of ethylbenzene by ethylene, each section of reaction product is cooled in a heat exchanger through benzene instead of directly adding quenched benzene to be mixed with each section of product, firstly, the benzene ratio is reduced, 50% of heating furnace load is reduced, secondly, the benzene and the reaction product are both provided with bypasses, and through bypass flow control, the temperature change of an inlet of a bed layer can be precisely controlled to be not more than +/-2% and the temperature rise change to be not more than +/-10%, so that the method can be used in the industrial production of ethylbenzene by dilute ethylene.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
In addition, the specific features described in the following embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention can be made, so long as the concept of the present invention is not deviated, and the technical solution formed thereby is a part of the original disclosure of the present specification, and also falls within the protection scope of the present invention.
[ Example 1]
Raw material I is dilute ethylene which is derived from crude cracked gas; raw material II is benzene.
The main working conditions and the running conditions of a device (the operation time is 8000 h) for preparing ethylbenzene by using 40 ten thousand tons/year crude pyrolysis gas are shown in Table 1 by adopting the process technology of FIG. 1.
The ethylene design concentration of the device is 50%, the total styrene ratio is 3.5, the number of sections is 6, the ethylene distribution coefficient alpha=1.15, the working condition 2 is a normal operation working condition, the inlet temperature and the temperature rise of each section are the same, the working condition 1 and the working condition 3 are the same because of the fluctuation of upstream raw material gas, so that the ethylene concentration is respectively increased to 55% and reduced to 40%, when the device runs to the working condition 1, the opening of a reaction product bypass valve is reduced, the flow of a bypass reaction product is reduced by 8%, meanwhile, the opening of a benzene bypass flow regulating valve is reduced, the flow of a benzene bypass is reduced by 12%, and the flow of a cooling medium is increased by 20%; when the device is operated to the working condition 3, the outlet temperature of the heating furnace is increased by 5%, meanwhile, the opening of the reaction product bypass flow regulating valve is increased, so that the reaction product bypass flow is increased by 25%, and the opening of the benzene bypass flow regulating valve is increased, so that the benzene bypass flow is increased by 30%.
TABLE 1
[ Example 2]
Raw material I is dilute ethylene and is derived from DCC dry gas; raw material II is benzene.
The main working conditions and the running conditions of a device for preparing ethylbenzene by using 10 ten thousand tons/year dry gas (8000 hours of operation) adopting the process technology of FIG. 1 are shown in Table 2.
The ethylene design concentration of the device is 30%, the total styrene ratio is 4.5, the number of sections is 4, the ethylene distribution coefficient alpha=1.2, the device operates stably under the working condition 1, when the ethylene concentration of the device is increased to 35%, the opening of a reaction product bypass valve is reduced, so that the flow rate of the bypass reaction product is reduced by 5%, the opening of a benzene bypass flow rate regulating valve is reduced, the flow rate of the benzene bypass is reduced by 9%, and the flow rate of a cooling medium is increased by 10%; when the ethylene concentration of the device is reduced to 25%, the outlet temperature of the heating furnace is increased by 3%, and meanwhile, the opening of the reaction product bypass flow regulating valve is increased, so that the reaction product bypass flow is increased by 20%, and the opening of the benzene bypass flow regulating valve is increased, so that the benzene bypass flow is increased by 20%.
TABLE 2
| Project | Working condition 1 |
| Ethylene concentration (wt%) | 30 |
| Total flow of raw material I (t/h) | 11 |
| Ethylene weight space velocity | 1.2 |
| Benzene mole ratio | 4.5 |
| Number of segments | 4 |
| Reactor section operating pressure MPaG | 1.0 |
| Raw material II (Low temperature benzene) temperature °C | 220 |
| The feeding temperature of each section is DEG C | 330，330，330，330 |
| The temperature of the reaction products of each stage after heat exchange is lower than that of the reaction products of each stage | 352.3，352.5，352.4，352.5 |
| Each segment Wen Sheng | 22.3，22.5，22.4，22.5 |
| Heating furnace load kW | 1560 |
| Ethylbenzene yield% | 99.6 |
| Catalyst utilization% | 97.9 |
| Period month of catalyst regeneration | 16 |
[ Example 3]
Raw material I is dilute ethylene and is derived from FCC dry gas; raw material II is benzene.
The main working conditions and the running conditions of a device for preparing ethylbenzene by using 12 ten thousand tons/year dry gas (8000 hours of operation) adopting the process technology of FIG. 1 are shown in Table 2.
The ethylene design concentration of the device is 20%, the total styrene ratio is 4, the number of sections is 4, the ethylene distribution coefficient alpha=0.9, and the device runs stably under the working condition 1.
TABLE 3 Table 3
| Project | Working condition 1 |
| Ethylene concentration (wt%) | 20 |
| Total flow of raw material I (t/h) | 19.8 |
| Ethylene weight space velocity | 0.8 |
| Benzene mole ratio | 4 |
| Number of segments | 4 |
| Reactor section operating pressure MPaG | 1.1 |
| Raw material II (Low temperature benzene) temperature °C | 240 |
| The feeding temperature of each section is DEG C | 332，332，332，332 |
| The temperature of the reaction products of each stage after heat exchange is lower than that of the reaction products of each stage | 350.3，350.5，350.4，350.5 |
| Each segment Wen Sheng | 18.3，18.5，18.4，18.5 |
| Heating furnace load kW | 1400 |
| Ethylbenzene yield% | 99.6 |
| Catalyst utilization% | 97.9 |
| Period month of catalyst regeneration | 16 |
[ Example 4]
The initial state of operating condition 2 for the normal operation of the device according to example 1 differs only in that the feed material I is not distributed according to α, but is distributed equally, i.e. α=1, and the device operates as shown in table 5.
TABLE 4 Table 4
| Project | Working condition 2 |
| Ethylene concentration (wt%) | 50 |
| Total flow of raw material I (t/h) | 29.7 |
| Ethylene weight space velocity | 1 |
| Benzene mole ratio | 3.5 |
| Number of segments | 6 |
| Reactor section operating pressure MPaG | 1.2 |
| Raw material II (Low temperature benzene) temperature °C | 213 |
| The feeding temperature of each section is DEG C | 320.0，321.0，321.8，322.6，323.5，324.0 |
| The temperature of the reaction products of each stage after heat exchange is lower than that of the reaction products of each stage | 345.0，346.5，347.9，348.9，350.4，351.4 |
| Each segment Wen Sheng | 25.0，25.5，26.1，26.3，26.9，27.4 |
| Heating furnace load kW | 3350 |
| Ethylbenzene yield% | 98.0 |
| Catalyst utilization% | 93.0 |
| Period month of catalyst regeneration | 12 |
Comparative example 1
Raw material I is derived from the same as in example 1; raw material II is benzene.
The main working conditions and the operating conditions of a device (the operation time is 8000 h) for preparing ethylbenzene by using 40 ten thousand tons/year crude pyrolysis gas are shown in Table 2 by adopting the process technology of FIG. 2.
The ethylene design concentration of the device is 55%, the total styrene ratio is 5, the number of sections is 6, the ethylene feed quantity of the first section accounts for 30% of the total ethylene feed quantity, the rest 70% of ethylene enters each section of reactor according to equal proportion, the working condition 1 is a normal operation working condition, the inlet temperature and the temperature rise of each section are the same, the working condition 2 and the working condition 3 are due to the fluctuation of upstream feed gas, the ethylene concentration is respectively reduced to 50% and 40%, inert components in the feed gas are increased, the cold quantity brought by the feed gas is increased, the inlet temperature and the reaction temperature rise of each section are reduced, but the process has no adjusting means, and the ethylbenzene yield is reduced when the ethylene concentration is changed.
TABLE 5
The invention has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the invention. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, and these fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (27)
1. A method of controlling the feed temperature and temperature rise of each stage of catalyst bed in a reactor comprising: carrying out exothermic reaction on a raw material I and a raw material II in a reactor containing N sections of catalyst beds, wherein the raw material I enters the reactor from each section of catalyst bed independently in N strands, the raw material II enters the reactor from the 1 st section of catalyst bed, reaction products are led out from the lower part of each section of catalyst bed, and the raw material II exchanges heat with each section of reaction products sequentially from bottom to top; the reaction products of the 1 st to N-1 st section catalyst bed are recycled to the reactor after heat exchange, and the reaction products of the N th section are extracted after heat exchange; optionally cooling the heat-exchanged raw material II by adopting a cooling medium after each heat exchange, and finally, introducing the heat-exchanged raw material II into the reactor from a section 1 catalyst bed after optional heating treatment;
When the content of the components reacting with the raw material II in the raw material I is changed, controlling the feeding temperature change of each section of catalyst bed layer to be not more than +/-2% and the temperature rise change of each section of catalyst bed layer to be not more than +/-10% by adjusting at least one of the flow rate of each section of reaction product, the flow rate of the raw material II, the heating temperature of the raw material II and the flow rate of a cooling medium;
the catalyst bed layers of the reactor are a1 st section catalyst bed layer, a2 nd section catalyst bed layer, a3 rd section catalyst bed layer, … th section catalyst bed layer and an N th section catalyst bed layer from top to bottom in sequence.
2. The method of claim 1, wherein the step of determining the position of the substrate comprises,
The raw material II is cooled by a cooling medium at least once after each heat exchange with the 2~N th stage reaction product, wherein the 2~N th stage reaction product refers to the reaction product of the 2~N th stage catalyst bed.
3. The method according to claim 1, characterized in that the raw material I comprises components which can react with the raw material II and optionally other components besides these.
4. The method according to claim 3, wherein the raw material I contains 1 to 99wt% of a component capable of reacting with the raw material II.
5. The process according to claim 1, characterized in that the feedstock I is apportioned between the segments of the reactor, the feed amounts of which are obtained according to formula (1) and formula (2):
In the formulas (1) and (2), alpha is the distribution coefficient of the raw material I, and alpha is more than or equal to 0.5 and less than or equal to 1.5; n 1 is the molar feed amount of the component reacting with the raw material II in the first section of raw material I, and mol/h; n Total is the total molar feed amount of the components in the raw material I which react with the raw material II, mol/h; n N is the molar feed amount of the component reacting with the raw material II in the N-th section of raw material I, and mol/h; n N-1 is the first The molar feed amount of the components in the section raw material I which react with the raw material II and mol/h; n is more than or equal to 2.
6. The method of claim 1, wherein the step of determining the position of the substrate comprises,
When the content of the component reacting with the raw material II in the raw material I is increased, the feeding temperature change of each section of catalyst bed layer is controlled to be not more than +/-2% and the temperature rise change of each section of catalyst bed layer is controlled to be not more than +/-10% through at least one of the following operations: the flow of the reaction product led out of each section of catalyst bed layer is improved, the flow of the raw material II exchanging heat with each section of reaction product is improved, and the flow of a cooling medium is improved;
Or alternatively
When the content of the component reacting with the raw material II in the raw material I is reduced, the feeding temperature change of each section of catalyst bed layer is controlled to be not more than +/-2% and the temperature rise change of each section of catalyst bed layer is controlled to be not more than +/-10% through at least one of the following operations: reducing the flow of reaction products led out from each section of catalyst bed, reducing the flow of raw material II exchanging heat with each section of reaction products, and improving the heating treatment temperature before the raw material II enters the 1 st section of catalyst bed.
7. The method of claim 6, wherein when the mass concentration of the component reacting with the raw material II in the raw material I is increased by 0.1% -60%, the feed temperature change of each section of catalyst bed is controlled to be not more than + -2% and the temperature rise change of each section of catalyst bed is controlled to be not more than + -10% by at least one of the following operations: the flow rate of each section of reaction product is increased by 0.1% -50%, the flow rate of the raw material II which exchanges heat with each section of reaction product is respectively and independently increased by 0.1% -50%, and the flow rate of the cooling medium is increased by 0.1% -100%;
Or alternatively
When the mass concentration of the components reacting with the raw material II in the raw material I is reduced by 0.1% -60%, the feeding temperature change of each section of catalyst bed is controlled to be not more than +/-2% and the temperature rise change of each section of catalyst bed is controlled to be not more than +/-10% through at least one of the following operations: the heating treatment temperature is increased by 0.1% -20%, the flow rate of each section of reaction product is reduced by 0.1% -80%, and the flow rate of the raw material II exchanging heat with each section of reaction product is respectively and independently reduced by 0.1% -80%.
8. The method of claim 6, wherein the heat exchange treatment is performed in a heat exchanger.
9. The method according to claim 8, characterized in that a bypass line I is provided at the inlet of the reaction product of the section of each heat exchanger, on which bypass line I a flow regulating valve is provided; and/or a bypass pipeline II is arranged at the inlet of the raw material II of each heat exchanger, and a flow regulating valve is arranged on the bypass pipeline II.
10. The process according to claim 9, wherein the flow of each stage of reaction product is controlled independently of the flow of its corresponding bypass conduit I and/or the flow of the feed II exchanging heat with each stage of reaction product is controlled by the flow of the bypass conduit II on each heat exchanger.
11. The method according to any one of claims 1 to 10, wherein the temperature rise of each catalyst bed is controlled to be 5 to 30 ℃.
12. The method of claim 11, wherein the temperature rise of each catalyst bed is controlled to be 10-26 ℃.
13. A system for controlling the feeding temperature and temperature rise of each section of catalyst bed in a reactor, which is used for carrying out the method of one of claims 1 to 12, the system comprises a reactor containing N sections of catalyst beds, a raw material I inlet is arranged above each section of catalyst bed, a product outlet of the reaction product of each section is arranged below each section of catalyst bed, a product circulation inlet of the reaction product of the previous section is arranged above the 2~N th section of catalyst bed, the product outlet of the reaction product of the 1 to N-1 th section is connected with the product circulation inlet of the reaction product of the previous section through a circulation pipeline to form a circulation loop, and a heat exchanger is arranged on the circulation pipeline.
14. The system of claim 13, wherein the system further comprises a controller configured to control the controller,
A raw material II inlet is arranged above a section 1 catalyst bed layer of the reactor; and/or the number of the groups of groups,
A material extraction pipeline is arranged below the Nth section catalyst bed layer.
15. The system of claim 14, wherein the system further comprises a controller configured to control the controller,
The top of the reactor is provided with a raw material II inlet; and/or the number of the groups of groups,
A material extraction pipeline is arranged at the bottom of the reactor.
16. The system of claim 14, wherein a heat exchanger is provided on the material extraction line.
17. The system of claim 13, wherein all heat exchangers are connected by a feed II feed pipe which further extends to the feed II inlet of the reactor forming a feed channel for feed II.
18. The system according to claim 17, characterized in that a heating device is arranged on the feed pipe for the feed II after the last heat exchanger in the flow direction of the feed II.
19. The system according to claim 17, characterized in that at least one cooling device is arranged on the feed II feed pipe between all heat exchangers.
20. The system of claim 17, wherein a cooling device is disposed between the heat exchanger of the stage 1 catalyst bed and the heat exchanger of the stage 2 catalyst bed.
21. A system according to any one of claims 13 to 20, wherein a bypass conduit I is provided at the inlet of the reaction product of the stage of each heat exchanger, and a flow regulating valve is provided on said bypass conduit I.
22. The system of claim 21, wherein a bypass line II is provided at the feed II inlet of each heat exchanger, and a flow regulating valve is provided on the bypass line II.
23. Use of the method according to any one of claims 1 to 12 or the system according to any one of claims 13 to 22 in a gas-phase or liquid-phase exothermic reaction.
24. The use according to claim 23, in the manufacture of ethylbenzene from dilute ethylene.
25. The use according to claim 23, wherein when applied to the preparation of ethylbenzene from dilute ethylene, the use of dilute ethylene as feed I and benzene as feed II is carried out, wherein the molar ratio of benzene to ethylene is 2-7 and the ethylene weight space velocity is 0.3-2.0。
26. The use according to any one of claims 23 to 25, wherein, when applied to the production of ethylbenzene from dilute ethylene,
Controlling the temperature of each section of reaction product after heat exchange to be 250-450 ℃; and/or the number of the groups of groups,
Controlling the feeding temperature above each section of catalyst bed layer to be 250-450 ℃ independently; and/or the number of the groups of groups,
Controlling the feeding pressure above each section of catalyst bed to be 0.5-2.0 MPaG; and/or the number of the groups of groups,
And controlling the temperature rise of each section of catalyst bed layer to be 5-30 ℃.
27. The use according to claim 26, wherein, when applied in the production of ethylbenzene from dilute ethylene,
Controlling the temperature of each section of reaction product after heat exchange to be 300-400 ℃; and/or the number of the groups of groups,
Controlling the feeding temperature above each section of catalyst bed layer to be 300-400 ℃ respectively and independently; and/or the number of the groups of groups,
Controlling the feeding pressure above each section of catalyst bed to be 0.8-1.5 MPaG; and/or the number of the groups of groups,
And controlling the temperature rise of each section of catalyst bed layer to be 10-26 ℃.
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| CN109499261A (en) * | 2018-12-03 | 2019-03-22 | 四川天科技股份有限公司 | The removing system and method for CO in a kind of used in proton exchange membrane fuel cell hydrogen |
| CN110218590A (en) * | 2019-05-22 | 2019-09-10 | 湖南衡钢百达先锋能源科技有限公司 | A kind of blast furnace gas sulfur method and system |
| CN112619396A (en) * | 2019-10-08 | 2021-04-09 | 中国石油化工股份有限公司 | Device and method for quickly removing hydrogen sulfide gas |
| CN212329208U (en) * | 2020-04-20 | 2021-01-12 | 深圳市睿维盛环保科技有限公司 | Semi-movable gas-collecting hood push rod assembly |
| CN212403458U (en) * | 2020-04-24 | 2021-01-26 | 西南化工研究设计院有限公司 | Device for preparing hydrogen for fuel cell from yellow phosphorus tail gas |
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| CN105233653A (en) * | 2015-10-13 | 2016-01-13 | 中国石油化工股份有限公司 | Hydrogen sulfide absorbing device |
| CN105858604A (en) * | 2016-03-31 | 2016-08-17 | 四川天采科技有限责任公司 | Full-temperature-range pressure-swing adsorption method for removing hydrogen sulfide from hydrogen rich gas source |
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