CN112206722A - Multi-stage adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling, reactor and application thereof - Google Patents
Multi-stage adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling, reactor and application thereof Download PDFInfo
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
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Abstract
The invention relates to a multi-section adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling, a reactor and application thereof, and mainly solves the problems of more side reactions, low catalyst utilization rate and short service life caused by the fact that the reaction temperature and bed temperature rise of each section of catalyst bed layer of the existing multi-section adiabatic fixed bed reactor with strong reaction heat are difficult to accurately control. The invention adopts the following steps: dividing split-flow reaction raw materials into n strands, entering each section of catalyst bed layer of the reactor in a segmented manner, wherein the flow rates from the first strand to the nth strand are respectively F1, F2, … … and Fn, wherein F1 is more than F2 and more than … … is more than Fn; b) the number of the catalyst bed layers is n, the filling heights of each section of catalyst bed layers corresponding to n split-flow reaction raw materials are respectively H1, H2, … … and Hn, wherein H1 is more than H2 and more than … … is more than Hn; wherein n is a natural number, and n is more than or equal to 2. The method can be used in the process of a multi-section adiabatic fixed bed reactor.
Description
Technical Field
The invention relates to the field of adiabatic fixed bed reaction processes, in particular to a multi-section adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling, a reactor and application thereof.
Background
The multistage heat-insulating fixed bed reactor does not exchange any heat with the outside, the catalyst is fixed in the reactor in multiple stages, reactants enter the catalyst bed layer from top to bottom, and the reactor has the advantages of simple equipment structure, difficult abrasion of the catalyst and high reaction rate, so the reactor is widely applied to the field of chemical industry.
However, since the support of the catalyst in the fixed bed is often a poor conductor of heat, and the chemical reaction is accompanied by a certain thermal effect, the reaction result is very sensitively dependent on the temperature conditions. Therefore, for the reaction process with large thermal effect, the heat transfer and temperature control problems become difficult and critical in the fixed bed design.
The adiabatic reactor has no heat exchange with the outside, and for exothermic reaction, the heat released in the reaction process is completely used for heating the temperature of materials in the system; in the case of an endothermic reaction, the system temperature will decrease. If the temperature is increased or decreased beyond a certain range, the effect of the reaction is decreased, and the catalyst is also adversely affected. In order to control the inlet temperature and adiabatic temperature rise (or adiabatic temperature drop) of each catalyst bed in the reactor, the prior art generally adopts the method that reaction raw materials with the temperature different from the feeding temperature at the top are added between each catalyst bed to adjust the inlet temperature and the temperature rise of the bed. However, in the prior art, equal-flow feeding is carried out between sections, reactants of the later section of catalyst bed layer are necessarily more than the former section, so that the temperature of the later section of catalyst bed layer is increased than that of the former section of bed layer, and the temperature of the inlet of each section of bed layer is gradually increased.
Chinese patent CN101147852A discloses a multi-stage layered heat-insulating fixed bed reactor, which mainly solves the problems of uneven distribution of bed layer fluid in the multi-stage heat-insulating fixed bed reactor and long mixing length of fluid between stages in the prior art by adopting the technical scheme of an inlet fluid pre-distributor and a fluid distributor between stages in the multi-stage layered fixed bed reactor. This patent does not relate to bed height and feed rate distribution methods.
Chinese patent CN103664484A discloses a method for preparing ethylbenzene by gas phase alkylation of benzene and ethylene, which mainly solves the problem of influence on catalyst reaction selectivity due to uneven mixing of materials between segments caused by uniform distance between two adjacent catalyst beds in a multi-segment adiabatic fixed bed reactor in the previous literature by adopting a technical scheme that the distance between two adjacent catalyst beds from top to bottom in the reactor is gradually increased in the reaction of preparing ethylbenzene by gas phase alkylation of benzene and ethylene. The patent makes a limitation on the space between catalyst beds (homogenization space), but does not refer to the conditions of the height of the catalyst bed, the relation between the feed amount of raw materials and the height of the catalyst bed, and the like.
Chinese patent CN103739438A discloses a method for producing cumene by liquid phase alkylation of benzene and propylene, which mainly solves the problem of influence on catalyst reaction selectivity due to uneven mixing of materials between sections caused by uniform distance between two adjacent catalyst beds in a multi-section adiabatic fixed bed reactor in the previous literature by adopting a technical scheme that the distance between two adjacent catalyst beds is gradually increased from bottom to top. The patent makes a limitation on the space between catalyst beds (homogenization space), but does not refer to the conditions of the height of the catalyst bed, the relation between the feed amount of raw materials and the height of the catalyst bed, and the like.
Chinese patent CN203061163U discloses the use of a reactor comprising a reactor inlet, outlet, shell, and catalyst bed: the catalyst bed layers are positioned in the reactor and consist of 2 to n catalyst bed layers, the space between every two adjacent catalyst bed layers from top to bottom of the catalyst bed layers is h1, h2, … … and hn, wherein h1 is more than h2 and more than … … is more than hn. The patent makes a limitation on the space between catalyst beds (homogenization space), but does not refer to the conditions of the height of the catalyst bed, the relation between the feed amount of raw materials and the height of the catalyst bed, and the like.
Disclosure of Invention
The invention aims to solve the technical problems that in the prior art, the inlet reaction temperature and bed temperature rise of each section of catalyst bed of a multi-section heat-insulation fixed bed reactor with stronger reaction heat are difficult to accurately control, so that the side reactions are more and the utilization rate of the catalyst is low. The method has the characteristics of accurately controlling the reaction temperature and bed temperature rise of each section of catalyst bed inlet, improving the reaction performance and the catalyst utilization rate and prolonging the service life.
One of the purposes of the invention is to provide a multi-stage adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling, which comprises the following steps:
a) dividing split-flow reaction raw materials into n strands, entering each section of catalyst bed layer of the reactor in a segmented manner, wherein the flow rates from the first strand to the nth strand are respectively F1, F2, … … and Fn, wherein F1 is more than F2 and more than … … is more than Fn;
b) the number of the catalyst bed layers is n, the filling heights of each section of catalyst bed layers corresponding to n split-flow reaction raw materials are respectively H1, H2, … … and Hn, wherein H1 is more than H2 and more than … … is more than Hn;
wherein n is a natural number, n is not less than 2, n is preferably 2-8, and n is more preferably 4-6.
In the technical scheme, the split-flow reaction raw material is one or more reaction substances, and the one or more reaction substances are fed respectively; or the split-flow reaction raw materials are a mixture of several reaction substances, and the mixture is fed together.
And Fi is the flow rate of a certain strand of the split reaction raw material, i is more than or equal to 2 and less than or equal to n, and the split flow rate is gradually increased, namely Fi is more than Fi-1, wherein the Fi is (1.05-2.0) Fi-1, preferably the Fi is (1.1-1.5) Fi-1, and more preferably the Fi is (1.2-1.5) Fi-1.
As a more preferable mode, in the process of the present invention, the flow rate of the reaction raw material for division satisfies the relation (Fi +1/Fi) > (Fi/Fi-1).
And setting Hi as the filling height of a certain section of the catalytic bed layer, wherein i is more than or equal to 2 and less than or equal to n, and the filling height is gradually increased, namely Hi is more than Hi-1, and Hi is (1.05-2.0) Hi-1, preferably Hi is (1.1-1.5) Hi-1, and more preferably Hi is (1.2-1.5) Hi-1.
The reactor of the multi-section adiabatic fixed bed comprises n catalyst beds, preferably n is 2-8, namely 2-8 catalyst beds; more preferably, n is 4-6, i.e. comprises 4-6 catalyst beds.
Preferably, the n split-flow reaction raw materials respectively enter the reactor from the upper part of the corresponding n sections of catalyst beds.
The split-flow reaction raw materials enter the reactor in a subsection mode through the fluid distributor.
The fluid distributor is arranged at the top or bottom inlet of the reactor and between two adjacent catalyst beds. The fluid distributor is not particularly limited, and is a fluid distributor generally used in the art.
The temperature of the raw materials between the catalyst bed sections is the same as or different from that of the raw materials at the top.
The reaction method is used for exothermic or endothermic reactions.
The split-flow reaction raw materials enter each section of catalyst bed layer of the reactor from top to bottom or from bottom to top in a segmented manner.
The second purpose of the invention is the application of the multistage adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling in the reactions of alkylation of aromatic hydrocarbon and olefin, alkylation of aromatic hydrocarbon and alcohol, alcohol dehydration, dehydrogenation of aromatic hydrocarbon and the like.
The invention also aims to provide a reactor for the variable-mass feeding and catalyst gradient-filling multistage adiabatic fixed bed reaction method, which comprises n catalyst beds; the top or bottom inlet of the reactor is provided with a fluid distributor, and a fluid distributor is arranged between two adjacent catalyst bed layers, wherein n is a natural number and is more than or equal to 2.
The reactor of the multi-section adiabatic fixed bed preferably comprises 2-8 catalyst beds, and more preferably 4-6 catalyst beds.
The fluid distributor is a fluid distributor as is common in the art.
In the prior art, in order to control the inlet temperature and adiabatic temperature rise (or adiabatic temperature drop) of each catalyst bed in a reactor, reaction raw materials with different temperatures are added between each catalyst bed to adjust the inlet temperature and the temperature rise of the bed. However, in the prior art, equal-flow feeding is carried out between sections, reactants of the later section of catalyst bed layer are necessarily more than the former section, so that the temperature of the later section of catalyst bed layer is increased than that of the former section of bed layer, and the temperature of the inlet of each section of bed layer is gradually increased.
The invention adopts a multi-section adiabatic fixed bed reaction method of variable mass feeding and catalyst gradient filling, and the feeding amount of raw materials between catalyst bed sections is gradually increased according to a certain proportion, so that the inlet temperature and the temperature rise of a reaction bed are effectively controlled. The method adopts a catalyst gradient filling method, is matched with variable-mass feeding, can accurately control reaction temperature and temperature rise on one hand, and can improve the utilization rate of the catalyst, reduce the filling amount of the catalyst, prolong the service life of the catalyst and obtain better technical effects on the other hand.
Drawings
FIG. 1 is a schematic diagram of the multi-stage adiabatic fixed bed reaction process with variable mass feed and gradient catalyst loading according to the present invention.
In fig. 1, R is a reactor, C is an undivided reaction raw material fed from the top of the reactor, D is a discharge from the bottom of the reactor, F is a divided reaction raw material, F1 is a first section catalyst bed layer feed, F2 is a second section catalyst bed layer feed, Fn is an nth section catalyst bed layer feed, H1 is a first section catalyst bed layer filling height, H2 is a second section catalyst bed layer filling height, and Hn is an nth section catalyst bed layer filling height.
In the figure 1, the reactor is a multi-section adiabatic fixed bed reactor, the catalyst is filled in n sections (n is more than or equal to 2), the filling heights from top to bottom are respectively H1-Hn, the un-shunted reaction raw material C enters from the top of the reactor, the shunted reaction raw material F is divided into n strands (n is more than or equal to 2), and the n strands enter each section of catalyst bed layer of the reactor from top to bottom in a subsection manner.
Detailed Description
The invention is further illustrated by the following examples.
The "height" in all tables is the catalyst loading height of each catalyst bed.
[ example 1 ]
In a 20-kiloton/annual ethylbenzene device (8000 hours of annual operation), ethylene and benzene are used as raw materials to carry out alkylation reaction to produce ethylbenzene, the reaction is strong heat effect exothermic reaction, the process shown in figure 1 is adopted, the reaction raw materials enter an alkylation reactor from top to bottom, the alkylation reactor is in a multi-section adiabatic fixed bed type and comprises 5 sections of bed layers, the reaction temperature is 388 ℃, the reaction pressure is 1.6MPaG, other operation parameters are shown in table 1, the loading amount of a catalyst is 4.8 tons, the service life of the catalyst is 4 years, and the total selectivity of the reactor is 99.9%.
TABLE 1 alkylation reactor operating parameters
[ example 2 ]
In a 30 ten thousand ton/year cumene device (8000 hours per year), propylene and benzene are used as raw materials to carry out alkylation reaction to produce the cumene, and the reaction is a strong thermal effect exothermic reaction. The overall process is shown in figure 1, but the reaction raw material enters an alkylation reactor from bottom to top, the alkylation reactor is in a multi-section adiabatic fixed bed type, and has 4 sections of beds, the reaction temperature is 138 ℃, the reaction pressure is 2.6MPaG, other operation parameters are shown in table 2, the loading amount of the catalyst is 18 tons, the service life of the catalyst is 8 years, and the selectivity of the isopropylbenzene and the diisopropylbenzene is 99.95%.
TABLE 2 alkylation reactor operating parameters
[ example 3 ]
In a 10-ten-thousand-ton/year ethylbenzene production device (8000 hours of annual operation), dry catalytic gas (dilute ethylene) is used as a raw material, the weight concentration of ethylene is 45%, the alkylation reaction is carried out with benzene, the reaction is a strong heat effect exothermic reaction, the process shown in figure 1 is adopted, the reaction raw material enters an alkylation reactor from top to bottom, the alkylation reactor is in a multi-section adiabatic fixed bed type, 5 sections of bed layers are provided in total, the reaction temperature is 321 ℃, the reaction pressure is 1.0MPaG, other operation parameters are shown in table 3, the loading amount of a catalyst is 10 tons, and the service life of the catalyst is 2 years. The total selectivity of the reactor was 99.8%.
TABLE 3 alkylation reactor operating parameters
[ example 4 ]
A60-kiloton/year ethylbenzene plant (8000 hours of annual operation) adopts the process shown in the figure 1, raw materials are crude cracked gas (ethylene weight concentration is 70%), reaction raw materials enter an alkylation reactor from top to bottom, the alkylation reactor is in a multi-section adiabatic fixed bed type and comprises 6 sections of bed layers, the reaction temperature is 320 ℃, the reaction pressure is 2.0MPaG, other operation parameters are shown in a table 4, the loading amount of a catalyst is 55 tons, the service life of the catalyst is 2 years, and the total selectivity of the reactor is 99.75%.
TABLE 4 alkylation reactor operating parameters
[ example 5 ]
The process of the device for producing p-xylene by alkylating 20 ten thousand tons of toluene and methanol per year (8000 hours of annual operation) adopts the process of the figure 1, the raw materials are toluene and methanol, the reaction is a medium thermal effect exothermic reaction, the reactor is in a multi-section adiabatic fixed bed type, the reaction raw materials enter the toluene and methanol alkylation reactor from top to bottom, the reactor is in a multi-section adiabatic fixed bed type, 4 sections of beds are totally adopted, the reaction temperature is 460 ℃, the reaction pressure is 1.5MPaG, other operation parameters are shown in a table 5, the loading amount of the catalyst is 20 tons, the service life of the catalyst is 3 years, the conversion rate of the methanol is 100 percent, and the selectivity of the xylene is 80 percent.
TABLE 5 reactor operating parameters
[ example 6 ]
A certain 28 ten thousand tons/year ethanol dehydration ethylene production device (annual operation time is 8000 hours) adopts the process of figure 1, the raw material is ethanol, the ethanol dehydration reaction is a moderate heat effect endothermic reaction, the reactor is a multi-section adiabatic fixed bed type, the reaction raw material enters the ethanol dehydration reactor from top to bottom, the reactor is a multi-section adiabatic fixed bed type, the total number of the beds is 4, the reaction temperature is 440 ℃, the reaction pressure is 0.3MPaG, other operation parameters are shown in a table 6, the loading amount of the catalyst is 108 tons, the service life of the catalyst is 2 years, the ethanol conversion rate is 99.0 percent, and the ethylene selectivity is 96.0 percent.
TABLE 6 reactor operating parameters
[ COMPARATIVE EXAMPLE 1 ]
In a 20-ten-thousand-ton/year ethylbenzene production device (8000 hours of annual operation), ethylene and benzene are used as raw materials to carry out alkylation reaction to produce ethylbenzene, the reaction is strong heat effect exothermic reaction, the reaction raw materials enter an alkylation reactor from top to bottom, the alkylation reactor is in a multi-section adiabatic fixed bed type and comprises 6 sections of bed layers, the distances between every two adjacent catalyst bed layers are 1500mm, 1650mm, 1820mm, 2000mm and 2200mm respectively, the reaction temperature is 388 ℃, the reaction pressure is 1.6MPaG, other operation parameters are shown in a table 7, the catalyst loading is 5.6 tons, the service life of the catalyst is 2 years, and the total selectivity of the reactor is 99.75%.
TABLE 7 alkylation reactor operating parameters
[ COMPARATIVE EXAMPLE 2 ]
In a 30 ten thousand ton/year cumene device (8000 hours per year), propylene and benzene are used as raw materials to carry out alkylation reaction to produce the cumene, and the reaction is a strong thermal effect exothermic reaction. The reaction raw material enters the alkylation reactor from bottom to top, and the reaction temperature rise is controlled by adopting a mode that part of reaction outlet liquid is returned to the bed layers of each section of the catalyst after being cooled, so that the feeding amount of each section is larger. The alkylation reactor is a multi-section adiabatic fixed bed type, 4 sections of beds are provided, the distance between two adjacent catalyst beds is 2900mm, 3050mm and 3200mm respectively, the reaction temperature is 138 ℃, the reaction pressure is 2.6MPaG, other operation parameters are shown in Table 8, the loading amount of the catalyst is 20 tons, the service life of the catalyst is 5 years, and the selectivity of the isopropyl benzene and the diisopropyl benzene is 99.78%.
TABLE 8 alkylation reactor operating parameters
[ COMPARATIVE EXAMPLE 3 ]
In a 10 ten thousand ton/year ethylbenzene plant (8000 hours per year), catalytic dry gas (dilute ethylene) is used as a raw material, and the concentration of ethylene in the catalytic dry gas is 45%. The alkylation reactor is a multi-section adiabatic fixed bed type, 5 sections of beds are totally formed, the catalyst beds are arranged at equal intervals, reaction raw materials enter the alkylation reactor from top to bottom, the reaction temperature is 321 ℃, the reaction pressure is 1.0MPaG, other operation parameters are shown in a table 9, the loading amount of the catalyst is 12 tons, the service life of the catalyst is 1.5 years, and the total selectivity of the reactor is 95.5%.
TABLE 9 alkylation reactor major Structure and reaction parameters
Claims (12)
1. A multi-section adiabatic fixed bed reaction method with variable mass feeding and catalyst gradient filling is characterized by comprising the following steps:
a) dividing split-flow reaction raw materials into n strands, entering each section of catalyst bed layer of the reactor in a segmented manner, wherein the flow rates from the first strand to the nth strand are respectively F1, F2, … … and Fn, wherein F1 is more than F2 and more than … … is more than Fn;
b) the number of the catalyst bed layers is n, the filling heights of each section of catalyst bed layers corresponding to n split-flow reaction raw materials are respectively H1, H2, … … and Hn, wherein H1 is more than H2 and more than … … is more than Hn;
wherein n is a natural number, n is not less than 2, n is preferably 2-8, and n is more preferably 4-6.
2. The method of claim 1, wherein the method comprises the steps of:
the split-flow reaction raw material is one or more reaction substances or a mixture of several reaction substances.
3. The method of claim 1, wherein the method comprises the steps of:
and Fi is the flow rate of a certain strand of the split reaction raw material, i is more than or equal to 2 and less than or equal to n, wherein Fi is (1.05-2.0) Fi-1, preferably Fi is (1.1-1.5) Fi-1, and more preferably Fi is (1.2-1.5) Fi-1.
4. The method of claim 1, wherein the method comprises the steps of:
and Hi is the filling height of a certain section of the catalytic bed layer, i is more than or equal to 2 and less than or equal to n, wherein Hi is (1.05-2.0) Hi-1, preferably Hi is (1.1-1.5) Hi-1, and more preferably Hi is (1.2-1.5) Hi-1.
5. The method of claim 1, wherein the method comprises the steps of:
and the n split-flow reaction raw materials respectively enter the reactor from the upper part of the corresponding n sections of catalyst bed layers.
6. The method of claim 5, wherein the mass-variable feed and catalyst gradient loading multistage adiabatic fixed bed reaction is characterized in that:
the split-flow reaction raw materials enter the reactor in a subsection mode through the fluid distributor.
7. The method of claim 1, wherein the method comprises the steps of:
the temperature of the raw materials between the catalyst bed sections is the same as or different from that of the raw materials at the top.
8. The method of claim 1, wherein the method comprises the steps of:
the reaction method is used for exothermic or endothermic reactions.
9. The method of claim 1, wherein the method comprises the steps of:
the split-flow reaction raw materials enter each section of catalyst bed layer of the reactor from top to bottom or from bottom to top in a segmented manner.
10. Use of the variable mass feed and catalyst gradient packed multistage adiabatic fixed bed reaction process of any of claims 1-9 in alkylation of aromatics with olefins, alkylation of aromatics with alcohols, dehydration of alcohols, dehydrogenation of aromatics.
11. A reactor for use in a multi-stage adiabatic fixed bed reaction process with variable mass feed and gradient loading of catalyst as claimed in any one of claims 1 to 9, characterized in that the reactor comprises n catalyst beds; the top or bottom inlet of the reactor is provided with a fluid distributor, and a fluid distributor is arranged between two adjacent catalyst bed layers, wherein n is a natural number and is more than or equal to 2.
12. The reactor according to claim 11, characterized in that the reactor of the multi-stage adiabatic fixed bed comprises 2 to 8 catalyst beds, preferably 4 to 6 catalyst beds.
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Cited By (1)
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CN115430365A (en) * | 2022-11-09 | 2022-12-06 | 北京弗莱明科技有限公司 | Method for preparing 2,2' -bipyridyl by using near-isothermal reaction device |
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