CN111889036B - Cyclopentadiene fixed bed catalytic hydrogenation reaction device, system and method - Google Patents
Cyclopentadiene fixed bed catalytic hydrogenation reaction device, system and method Download PDFInfo
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- CN111889036B CN111889036B CN201910368193.9A CN201910368193A CN111889036B CN 111889036 B CN111889036 B CN 111889036B CN 201910368193 A CN201910368193 A CN 201910368193A CN 111889036 B CN111889036 B CN 111889036B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/03—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of non-aromatic carbon-to-carbon double bonds
- C07C5/05—Partial hydrogenation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
- C07C2523/74—Iron group metals
- C07C2523/755—Nickel
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/06—Systems containing only non-condensed rings with a five-membered ring
- C07C2601/10—Systems containing only non-condensed rings with a five-membered ring the ring being unsaturated
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Abstract
The invention discloses a cyclopentadiene fixed bed catalytic hydrogenation reaction device, a system and a method, and belongs to the field of chemical equipment. It includes: the shell is provided with an inner cavity which is sequentially divided into a feeding chamber, at least one reaction chamber and a discharging chamber from top to bottom through a plurality of partition plates; the top wall of the feeding chamber is provided with a raw material inlet, and the bottom wall of the discharging chamber is provided with a product outlet; the side wall of each reaction chamber is provided with a refrigerant inlet and a refrigerant outlet, and the refrigerant outlet is higher than the refrigerant inlet; the device also includes: at least one reaction tube with two ends respectively communicated with the feeding chamber and the discharging chamber, wherein the reaction tube is internally provided with a catalyst and a circulating path; a first distributor located at the feedstock inlet; a second distributor located within the feed chamber and below the first distributor; the side wall of one reaction chamber is provided with a stress buffering structure which protrudes outwards and is in an annular structure coaxial with the shell. The device can avoid the phenomenon of self-polymerization and coking of reaction raw materials, and improve the selectivity and yield of the generated product.
Description
Technical Field
The invention relates to the field of chemical equipment, in particular to a cyclopentadiene fixed bed catalytic hydrogenation reaction device, a cyclopentadiene fixed bed catalytic hydrogenation reaction system and a cyclopentadiene fixed bed catalytic hydrogenation reaction method.
Background
Cyclopentene is an important intermediate of fine chemical products, and can be used as a production raw material of medicines, perfume intermediates, polycycloolefin high-molecular polymers and electronic chemicals. The raw materials have high purity requirement on cyclopentene, and high-purity cyclopentene can be prepared by hydrogenation of cyclopentadiene.
Cyclopentene is currently produced by reacting cyclopentadiene with hydrogen in an adiabatic fixed bed catalytic hydrogenation reactor.
However, the cyclopentadiene hydrogenation reaction is an exothermic reaction, and the fixed bed hydrogenation reactor is an adiabatic reactor, so that the temperature in the fixed bed hydrogenation reactor is high, cyclopentadiene is prone to self-coking, and the problems that the selectivity and yield of cyclopentene are greatly reduced, the catalytic activity of the fixed bed hydrogenation reactor is rapidly reduced, and the like are caused.
Disclosure of Invention
The embodiment of the invention provides a cyclopentadiene fixed bed catalytic hydrogenation reaction device, a cyclopentadiene fixed bed catalytic hydrogenation reaction system and a cyclopentadiene fixed bed catalytic hydrogenation reaction method, which can solve the technical problems. The specific technical scheme is as follows:
in one aspect, an embodiment of the present invention provides a cyclopentadiene fixed bed catalytic hydrogenation reaction apparatus, where the apparatus includes:
the device comprises a shell, a reaction chamber and a discharge chamber, wherein the shell divides an inner cavity into the feed chamber, the at least one reaction chamber and the discharge chamber from top to bottom in sequence through a plurality of partition plates;
the top wall of the feeding chamber is provided with a raw material inlet, and the bottom wall of the discharging chamber is provided with a product outlet;
the side wall of each reaction chamber is provided with a refrigerant inlet and a refrigerant outlet, the refrigerant outlet is higher than the refrigerant inlet, the side wall of one reaction chamber is provided with a stress buffering structure which protrudes outwards, and the stress buffering structure is in an annular structure coaxial with the shell;
the device further comprises: the reaction tubes are positioned in the shell, two ends of each reaction tube are respectively communicated with the feeding chamber and the discharging chamber, and each reaction tube is internally provided with a catalyst and a circulation path;
a first distributor located at the feedstock inlet;
and the second distributor is positioned in the feeding chamber and is arranged below the first distributor.
In one possible embodiment, the stress damping structure has an arc-shaped cross section in the axial direction.
In one possible design, in each reaction tube, the upper end and the lower end of the catalyst are respectively provided with a material pressing piece and a supporting piece;
the material pressing part is provided with a first overflowing gap communicated with the flowing path, and the supporting part is provided with a second overflowing gap communicated with the flowing path.
In one possible design, the pressing piece comprises a spring pressing ring, a first large-diameter magnetic ring and a first small-diameter magnetic ring which are sequentially arranged from top to bottom;
and a first overcurrent gap which is communicated is formed among the spring pressing ring, the first large-diameter magnetic ring and the first small-diameter magnetic ring.
In one possible design, the support piece comprises a second large-diameter magnetic ring and a second small-diameter magnetic ring which are sequentially arranged from bottom to top;
and the second overcurrent gap is communicated between the second large-diameter magnetic ring and the second small-diameter magnetic ring.
In one possible design, the press part and the support part are both detachably arranged in the reaction tube.
In one possible design, the first distributor is removably arranged at the raw material inlet;
the second distributor is detachably arranged in the feeding chamber.
In one possible design, the catalyst is in a columnar structure;
the inner diameter of the reaction tube is 10 to 50 times the diameter of the catalyst;
the ratio of the height to the diameter of the shell is 1:1-1.
In one aspect, an embodiment of the present invention provides a cyclopentadiene hydrogenation reaction system, including: any of the cyclopentadiene fixed bed catalytic hydrogenation reaction device, the gas-liquid separator and the circulating pump mentioned above;
the inlet of the cyclopentadiene fixed bed catalytic hydrogenation reaction device is communicated with a raw material input pipeline, and the outlet of the cyclopentadiene fixed bed catalytic hydrogenation reaction device is communicated with the inlet of the gas-liquid separator through a first pipeline;
the gas outlet of the gas-liquid separator is communicated with a hydrogen recovery pipeline, the liquid outlet of the gas-liquid separator is communicated with the inlet of the circulating pump through a second pipeline, the outlet of the circulating pump is communicated with the raw material input pipeline through a third pipeline, and the third pipeline is also communicated with a product output pipeline.
In one aspect, an embodiment of the present invention provides a cyclopentadiene hydrogenation reaction method, which is applied to the above-mentioned cyclopentadiene hydrogenation reaction system, and the method includes:
inputting a mixed raw material of cyclopentadiene, an auxiliary agent and hydrogen into a cyclopentadiene fixed bed catalytic hydrogenation reaction device through a raw material input pipeline, and reacting the mixed raw material in the cyclopentadiene fixed bed catalytic hydrogenation reaction device to obtain a first mixed product of cyclopentene, the auxiliary agent and the hydrogen;
the first mixed product is input into a gas-liquid separator through a first pipeline for gas-liquid separation treatment, and a second mixed product of cyclopentene and an auxiliary agent and hydrogen are obtained;
hydrogen is discharged from a hydrogen recovery pipeline, the second mixed product is input into a circulating pump through a second pipeline, and a third mixed product is obtained after pressurization of the circulating pump;
and the first part of the third mixed product is conveyed to the raw material input pipeline through a third pipeline, is mixed with the mixed raw material and then is conveyed to the cyclopentadiene fixed bed catalytic hydrogenation reaction device, and the second part of the third mixed product is conveyed out through a product output pipeline.
The technical scheme provided by the embodiment of the invention has the beneficial effects that at least:
according to the cyclopentadiene fixed bed catalytic hydrogenation reaction device provided by the embodiment of the invention, the side wall of the reaction chamber is provided with the refrigerant inlet and the refrigerant outlet, and the refrigerant is input into the refrigerant inlet, so that heat is exchanged between the refrigerant and the reaction tube, and the reaction tube is cooled, so that the reaction chamber can be cooled, the phenomenon of self-polymerization coking of reaction raw materials is avoided, the selectivity and the yield of generated products are improved, and the catalytic activity of a catalyst is also ensured. Through set up stress buffer structure on the lateral wall of reaction chamber, can absorb the reaction chamber because of the stress that the difference in temperature produced, avoid the casing inflation to damage.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a cyclopentadiene fixed-bed catalytic hydrogenation reaction apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic view of a reaction tube according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a cyclopentadiene hydrogenation reaction system according to an embodiment of the present invention.
Wherein the reference numerals denote:
a 100-cyclopentadiene fixed bed catalytic hydrogenation reaction device,
1-shell, 11-feeding chamber, 111-raw material inlet, 12-reaction chamber, 121-refrigerant inlet, 122-refrigerant outlet, 123-stress buffer structure, 13-discharging chamber, 131-product outlet,
2-a partition board which is arranged on the upper surface of the shell,
3-a reaction tube, wherein the reaction tube is provided with a reaction tube,
4-the first distributor is arranged on the first side of the distributor,
5-a second distributor of the second group of distributors,
6-material pressing piece, 61-spring press ring, 62-first large-diameter magnetic ring, 63-first small-diameter magnetic ring,
7-a catalyst (I) which is prepared by reacting a catalyst,
8-a support member, 81-a second large-diameter magnetic ring, 82-a second small-diameter magnetic ring,
200-a gas-liquid separator, wherein,
300-a circulating pump, wherein the circulating pump is arranged in the shell,
400-a raw material input pipeline, wherein,
500-the first line-up of the first line,
600-a hydrogen recovery line for recovering hydrogen,
700-the second line-up of the second line,
800-a third line-the first line,
900-product output line.
Detailed Description
Unless defined otherwise, all technical terms used in the examples of the present invention have the same meaning as commonly understood by one of ordinary skill in the art. In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
In one aspect, an embodiment of the present invention provides a cyclopentadiene fixed bed catalytic hydrogenation apparatus 100, as shown in fig. 1, the apparatus including: the device comprises a shell 1, wherein an inner cavity of the shell 1 is sequentially divided into a feeding chamber 11, at least one reaction chamber 12 and a discharging chamber 13 from top to bottom through a plurality of partition plates 2; the top wall of the feeding chamber 11 is provided with a raw material inlet 111, and the bottom wall of the discharging chamber 13 is provided with a product outlet 131; the sidewall of each reaction chamber 12 has a coolant inlet 121 and a coolant outlet 122, the coolant outlet 122 is higher than the coolant inlet 121, the sidewall of one reaction chamber 12 has a stress buffering structure 123 protruding outwards, and the stress buffering structure 123 is in an annular structure coaxial with the housing 1. The cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 provided by the embodiment of the invention further comprises: at least one reaction tube 3 positioned in the shell 1 and having two ends respectively communicated with the feeding chamber 11 and the discharging chamber 13, wherein each reaction tube 3 has a catalyst 7 and a flow path therein, see fig. 2; a first distributor 4 located at the feedstock inlet 111; a second distributor 5 located within the inlet chamber 11 and below the first distributor 4.
The flow path in the reaction tube 3 is a gap between the catalyst 7 and the reaction tube 3, and the shape thereof is not particularly limited, and fluid may be allowed to flow therethrough.
It will be appreciated that the feed inlet 111 is located in the top wall of the housing 1 and the product outlet 131 is located in the bottom wall of the housing 1. The refrigerant inlet 121 and the refrigerant outlet 122 are located on a sidewall of the housing 1.
The working principle of the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 provided by the embodiment of the invention is explained as follows:
the mixed raw material of cyclopentadiene, hydrogen and an auxiliary is input to the raw material inlet 111. The mixed raw materials are uniformly distributed by the first distributor 4, enter the feeding chamber 11, and uniformly distributed by the second distributor 5 and enter the reaction tube 3. Under the action of the catalyst 7 in the reaction tube 3, cyclopentadiene reacts with hydrogen to generate cyclopentene, which is output to the discharge chamber 13 from the reaction tube 3 and finally output from the product outlet 131.
In the process of preparing cyclopentene, the temperature in the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 is high, a refrigerant is input through the refrigerant inlet 121 of the reaction chamber 12, heat is exchanged between the refrigerant and the reaction tube 3 to cool the reaction tube 3, and then the refrigerant is output through the refrigerant outlet 122.
According to the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 provided by the embodiment of the invention, the coolant inlet 121 and the coolant outlet 122 are arranged on the side wall of the reaction chamber 12, and the coolant is input into the coolant inlet 121, so that the coolant and the reaction tube 3 exchange heat to cool the reaction tube 3, the reaction chamber 12 can be cooled, the phenomenon of self-coking of reaction raw materials is avoided, the selectivity and yield of the generated product are improved, and the catalytic activity of the catalyst 7 is also ensured. By arranging at least one reaction chamber 12, the temperature of the reaction chamber 12 can be fully and uniformly reduced by the refrigerant. Through setting up first distributor 4 and second distributor 5, do benefit to and carry out the equipartition to mixing the feed gas, guarantee to mix feed gas and the catalyst 7 in the reaction tube 3 abundant contact, improved the productivity.
Through setting up stress buffer structure 123, not only can absorb the stress that reaction chamber 12 produced because of the heat transfer, can also absorb or avoid producing stress because of the temperature difference of reaction tube 3 and casing 1 is big when catalyst 7 in the reaction tube 3 regenerates, and then avoid casing 1 inflation to damage.
As shown in fig. 1, the stress buffering structure 123 is an annular structure coaxial with the housing 1.
The stress buffering structure 123 has a simple structure, can absorb circumferential stress of the housing 1, and has a good stress buffering effect.
In addition, the refrigerant outlet 122 is higher than the refrigerant inlet 121, so that more refrigerant is filled in the reaction chamber 12 to exchange heat with the reaction tube 3 sufficiently.
An example is given for the stress buffering structure 123 in the embodiment of the present invention: the tangential plane of the stress buffering structure 123 along the axial direction is an arc-shaped plane. Thus, the stress buffering structure 123 can stably buffer stress, and avoid the phenomenon of stress concentration at the stress buffering structure 123.
As an example, as shown in fig. 2, in the reaction tube 3, the catalyst 7 is provided at upper and lower ends thereof with a pressure member 6 and a support member 8, respectively; the material pressing part 6 is provided with a first flow gap communicated with the flow path, and the support part 8 is provided with a second flow gap communicated with the flow path.
The catalyst 7 can be effectively fixed in the reaction tube 3 by the pressure feed 6 and the support 8.
The pressing member 6 and the supporting member 8 may be provided in various structures, and the following examples are given in the embodiments of the present invention with respect to the manner in which the pressing member 6 and the supporting member 8 are provided:
as shown in fig. 2, the pressing member 6 includes a spring ring 61, a first large-diameter magnetic ring 62, and a first small-diameter magnetic ring 63, which are sequentially arranged from top to bottom; a first flow gap is formed among the spring pressing ring 61, the first large-diameter magnetic ring 62 and the first small-diameter magnetic ring 63, so that the mixed raw materials can enter the reaction tube 3 through the pressing piece 6. For example, a first through hole communicating the inner cavity of the first small-diameter magnetic ring 63 with the circulation path is formed in the side wall of the first small-diameter magnetic ring 63, and the inner cavity of the spring pressing ring 61, the first large-diameter magnetic ring 62 and the first through hole are communicated with each other to form a first overcurrent gap.
The spring pressing ring 61 not only can tightly press the first large-diameter magnetic ring 62 and the first small-diameter magnetic ring 63, but also cannot damage the first large-diameter magnetic ring 62 and the first small-diameter magnetic ring 63. Spring clamping ring 61, first big footpath magnetic ring 62, first path magnetic ring 63 not only play the effect that compresses tightly catalyst 7, can also play the effect of filtering mixed raw materials, avoid mixed raw materials to block up reaction tube 3.
The support member 8 includes a second large-diameter magnetic ring 81 and a second small-diameter magnetic ring 82 which are sequentially arranged from bottom to top. A second overflowing gap is formed between the second large-diameter magnetic ring 81 and the second small-diameter magnetic ring 82, so that the mixed raw materials can be output from the reaction tube 3. For example, the sidewall of the second small-diameter magnetic ring 82 is provided with a second through hole communicating the inner cavity and the circulation path thereof, and the second flow gap is formed by the inner cavity of the second large-diameter magnetic ring 81 and the second small-diameter magnetic ring 82 and the second through hole.
The second large-diameter magnetic ring 81 and the second small-diameter magnetic ring 82 can effectively support the catalyst 7 and prevent the catalyst 7 from being separated from the reaction tube 3.
The pressure member 6 and the support member 8 may be welded in the reaction tube 3 so as not to be detachable, and the pressure member 6 and the support member 8 may be detachably provided in the reaction tube 3. Thus, the disassembly, assembly and replacement of the material pressing piece 6 and the supporting piece 8 are facilitated.
For example, the pressing member 6 and the supporting member 8 are both fixed in the reaction tube 3 by friction, and the pressing member 6 and the supporting member 8 can also be clamped in the reaction tube 3.
As an example, the first distributor 4 is detachably provided at the raw material inlet 111; the second distributor 5 is arranged in a removable manner in the inlet chamber 11.
Thus, the first distributor 4 and the second distributor 5 are convenient to disassemble, assemble and replace with the shell 1.
Wherein, the first distributor 4 may be a wire mesh structure. The second distributor 5 may be a trough-type liquid distributor.
In the embodiment of the present invention, the partition plate 2 may be integrally formed with the housing 1, or may be detachably disposed in the housing 1. When baffle 2 can dismantle with casing 1 and be connected, can have the joint groove on casing 1's the inner wall, have joint spare on baffle 2, joint spare joint in the joint inslot to realize baffle 2 and casing 1's being connected.
As an example, the number of the reaction chambers 12 is three, and the side wall of the reaction chamber 12 located in the middle has a stress buffering structure 123.
So, stress buffer structure 123 can effectively play the effect of eliminating the stress, avoids casing 1 to take place stress expansion because of the big difference in temperature with reaction tube 3 bad.
As an example, the number of the reaction tubes 3 is plural, and the plural reaction tubes 3 are all arranged in the vertical direction and are uniformly arranged in the housing 1.
As an example, the catalyst 7 has a columnar structure; the inner diameter of the reaction tube 3 is 10 to 50 times the diameter of the catalyst 7; for example, the amount may be 10 times, 15 times, 20 times, 25 times, 30 times, 35 times, 40 times, 45 times, 50 times, or the like.
Thus, an annular gap (i.e., a flow path) is formed between the reaction tube 3 and the catalyst 7, which is not only beneficial to the circulation of the mixed raw material gas, but also beneficial to the sufficient contact between the mixed raw material gas and the catalyst 7, so that the mixed raw material gas reacts.
The ratio of the height to the diameter of the shell 1 is 1:1-1, for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1.
The inner diameters of the first large-diameter magnetic ring 62 and the second large-diameter magnetic ring 81 may be 10mm, and the inner diameters of the first small-diameter magnetic ring 63 and the second small-diameter magnetic ring 82 may be 5mm.
As an example, the inlet chamber 11 is connected to the reaction chamber 12 by a flange, and the outlet chamber 13 is connected to the reaction chamber 12 by a flange.
As an example, the material of the reaction tube 3 is a steel tube, for example, the material of the reaction tube 3 may be DN25-DN150 seamless steel tube.
As an example, the reaction chamber 12 has a reaction temperature of-20 ℃ to 50 ℃ and a reaction pressure of 0.1MPa to 10MPa.
As an example, cyclopentadiene with the purity of 98.5% is hydrotreated by using the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 provided by the embodiment of the invention, and the flow rate of cyclopentadiene input into the reaction device is 1t/h. In this reaction apparatus, the outer diameter of the shell 1 was 1.6m, the length was 5m, the inner diameter of the reaction tube 3 was 60mm, each reaction tube 3 was formed by connecting five seamless steel tubes, the number of the reaction tubes 3 was 313, and they were arranged in a regular triangle. The shell 1 is uniformly divided into three reaction chambers 12 by partition plates 2. The reaction tube 3 is filled with a nickel-containing catalyst 2.46m 3 . The pressure in the reaction device is 5Mpa, the operation temperature is minus 10 ℃, and the design temperature is minus 20 ℃ to 450 ℃. The coolant is glycol water solution, the temperature of the glycol water solution entering the coolant inlet 121 is-15 ℃, and the temperature of the glycol water solution output from the coolant outlet 122 is 0 ℃. The percent of selectivity of cyclopentadiene hydrogenation reaction to cyclopentene is 99% and the conversion rate of cyclopentadiene into cyclopentene is 99%.
In one aspect, an embodiment of the present invention provides a cyclopentadiene hydrogenation reaction system, as shown in fig. 3, the system including: any of the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100, the gas-liquid separator 200 and the circulating pump 300 mentioned above. Wherein, the inlet of the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 is communicated with the raw material input pipeline 400, and the outlet is communicated with the inlet of the gas-liquid separator 200 through the first pipeline 500; the gas outlet of the gas-liquid separator 200 is communicated with the hydrogen recovery pipeline 600, the liquid outlet is communicated with the inlet of the circulating pump 300 through the second pipeline 700, the outlet of the circulating pump 300 is communicated with the raw material input pipeline 400 through the third pipeline 800, and the third pipeline 800 is further communicated with the product output pipeline 900.
According to the cyclopentadiene hydrogenation reaction system provided by the embodiment of the invention, the coolant inlet 121 and the coolant outlet 122 are arranged on the side wall of the reaction chamber 12, and a coolant is input into the coolant inlet 121, so that heat is exchanged between the coolant and the reaction tube 3, and the reaction tube 3 is cooled, so that the reaction chamber 12 can be cooled, the phenomenon of self-coking of reaction raw materials is avoided, the selectivity and yield of generated products are improved, the catalytic activity of a catalyst is also ensured, and the efficiency of cyclopentadiene hydrogenation reaction is effectively improved. By providing the stress buffering structure 123 on the sidewall of the reaction chamber 12, the stress generated by the temperature difference in the reaction chamber 12 can be absorbed, and the expansion and damage of the housing 1 can be avoided.
In one aspect, an embodiment of the present invention provides a cyclopentadiene hydrogenation reaction method, which is applied to the above-mentioned cyclopentadiene hydrogenation reaction system, and the method includes:
mixed raw materials of cyclopentadiene, an auxiliary agent and hydrogen are input into the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 through the raw material input pipeline 400, and the mixed raw materials react in the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100 to obtain a first mixed product of cyclopentene, the auxiliary agent and the hydrogen.
The first mixed product is input into the gas-liquid separator 200 through the first pipeline 500 for gas-liquid separation treatment, and a second mixed product of hydrogen, cyclopentene and an auxiliary agent is obtained.
The hydrogen is discharged from the hydrogen recovery pipeline 600, and the second mixed product is input to the circulation pump 300 through the second pipeline 700, and is pressurized by the circulation pump 300 to obtain a third mixed product.
The first part of the third mixed product is delivered to the raw material input pipeline 400 through the third pipeline 800, and is mixed with the mixed raw material and delivered to the cyclopentadiene fixed bed catalytic hydrogenation reaction device 100, and the second part of the third mixed product is delivered through the product output pipeline 900.
The cyclopentadiene hydrogenation reaction method provided by the embodiment of the invention can avoid the self-polymerization coking phenomenon of reaction raw materials, improve the selectivity and yield of the generated product, ensure the catalytic activity of the catalyst and effectively improve the efficiency of the cyclopentadiene hydrogenation reaction.
All the above optional technical solutions may be combined arbitrarily to form the optional embodiments of the present disclosure, and are not described herein again.
The above description is only an illustrative embodiment of the present invention, and should not be taken as limiting the scope of the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A cyclopentadiene fixed bed catalytic hydrogenation reaction device is characterized by comprising:
the device comprises a shell (1), wherein an inner cavity of the shell (1) is sequentially divided into a feeding chamber (11), three reaction chambers (12) arranged in the vertical direction and a discharging chamber (13) from top to bottom through a plurality of partition plates (2);
the top wall of the feeding chamber (11) is provided with a raw material inlet (111), and the bottom wall of the discharging chamber (13) is provided with a product outlet (131);
a refrigerant inlet (121) and a refrigerant outlet (122) are formed in the side wall of each reaction chamber (12), the refrigerant outlet (122) is higher than the refrigerant inlet (121), a stress buffering structure (123) protruding outwards is formed in the side wall of the reaction chamber (12) in the middle, and the stress buffering structure (123) is of an annular structure coaxial with the shell (1);
the device further comprises: the reaction device comprises at least one reaction tube (3) which is positioned in the shell (1) and two ends of which are respectively communicated with the feeding chamber (11) and the discharging chamber (13), and a catalyst (7) and a circulating path are arranged in each reaction tube (3);
a first distributor (4) located at the feedstock inlet (111), the first distributor (4) being of a wire mesh construction;
a second distributor (5) positioned in the feed chamber (11) and below the first distributor (4), the second distributor (5) being a trough-type liquid distributor;
in each reaction tube (3), the upper end and the lower end of the catalyst (7) are respectively provided with a material pressing piece (6) and a supporting piece (8);
the material pressing part (6) is provided with a first flow gap communicated with the flow path, and the support part (8) is provided with a second flow gap communicated with the flow path;
the material pressing piece (6) comprises a spring pressing ring (61), a first large-diameter magnetic ring (62) and a first small-diameter magnetic ring (63) which are sequentially arranged from top to bottom;
the spring pressing ring (61), the first large-diameter magnetic ring (62) and the first small-diameter magnetic ring (63) form a conducted first overcurrent gap;
the catalyst (7) is in a columnar structure;
the inner diameter of the reaction tube (3) is 10 to 50 times the diameter of the catalyst (7);
the ratio of the height to the diameter of the shell (1) is 1:1-1;
the carrier of the catalyst (7) is aluminum oxide, and the active component comprises nickel or palladium.
2. The device according to claim 1, characterized in that the stress buffering structure (123) is arc-shaped in axial section.
3. The device according to claim 1, characterized in that the support member (8) comprises a second large-diameter magnetic ring (81) and a second small-diameter magnetic ring (82) which are arranged in sequence from bottom to top;
and the second overcurrent gap is formed between the second large-diameter magnetic ring (81) and the second small-diameter magnetic ring (82).
4. The device according to claim 1, characterized in that the press (6) and the support (8) are both detachably arranged in the reaction tube (3).
5. The apparatus according to any of the claims 1 to 4, wherein the first distributor (4) is removably arranged at the raw material inlet (111);
the second distributor (5) is detachably arranged in the feeding chamber (11).
6. A cyclopentadiene hydrogenation reaction system, comprising: the cyclopentadiene fixed bed catalytic hydrogenation reaction device (100), the gas-liquid separator (200), the circulation pump (300) according to any one of claims 1 to 5;
the inlet of the cyclopentadiene fixed bed catalytic hydrogenation reaction device (100) is communicated with a raw material input pipeline (400), and the outlet of the cyclopentadiene fixed bed catalytic hydrogenation reaction device is communicated with the inlet of the gas-liquid separator (200) through a first pipeline (500);
the gas outlet of the gas-liquid separator (200) is communicated with a hydrogen recovery pipeline (600), the liquid outlet of the gas-liquid separator is communicated with the inlet of the circulating pump (300) through a second pipeline (700), the outlet of the circulating pump (300) is communicated with the raw material input pipeline (400) through a third pipeline (800), and the third pipeline (800) is further communicated with a product output pipeline (900).
7. A cyclopentadiene hydrogenation reaction method, which is applied to the cyclopentadiene hydrogenation reaction system according to claim 6, comprising:
inputting a mixed raw material of cyclopentadiene, an auxiliary agent and hydrogen into a cyclopentadiene fixed bed catalytic hydrogenation reaction device (100) through a raw material input pipeline (400), wherein the mixed raw material reacts in the cyclopentadiene fixed bed catalytic hydrogenation reaction device (100) to obtain a first mixed product of cyclopentene, the auxiliary agent and the hydrogen;
the first mixed product is input into a gas-liquid separator (200) through a first pipeline (500) for gas-liquid separation treatment to obtain a second mixed product of cyclopentene and an auxiliary agent and hydrogen;
hydrogen is discharged from a hydrogen recovery pipeline (600), the second mixed product is input into a circulating pump (300) through a second pipeline (700), and a third mixed product is obtained after pressurization is carried out on the second mixed product by the circulating pump (300);
a first part of the third mixed product is output to the raw material input pipeline (400) through a third pipeline (800), and is mixed with the mixed raw material and then is input to the cyclopentadiene fixed bed catalytic hydrogenation reaction device (100), and a second part of the third mixed product is output through a product output pipeline (900).
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| CN1597080A (en) * | 2002-01-11 | 2005-03-23 | 三菱化学株式会社 | Vapor phase catalytic oxidation method using multipipe reactor |
| US7500999B2 (en) * | 2004-09-01 | 2009-03-10 | Praxair Technology, Inc. | Catalytic reactor |
| CN1911877A (en) * | 2005-08-09 | 2007-02-14 | 中国石化上海石油化工股份有限公司 | Method of preparing cyclopentene by continuous hydrogenation of cyclopentadiene |
| CN102688725B (en) * | 2012-07-02 | 2014-04-09 | 西南石油大学 | Hot plate type reactor |
| CN202962427U (en) * | 2012-12-11 | 2013-06-05 | 江苏永大化工机械有限公司 | Ethylene glycol hydrogenation reactor |
| CN103566837B (en) * | 2013-11-13 | 2015-09-30 | 山西大学 | A kind of outer circulation reaction unit being applicable to hydrogenation exothermic reaction |
| CN103566836A (en) * | 2013-11-25 | 2014-02-12 | 南京国昌化工科技有限公司 | Uniform-temperature hydrogenation reactor |
| CN106673938B (en) * | 2015-11-09 | 2019-04-12 | 中国石油化工股份有限公司 | A method of cyclopentene is produced by cyclopentadiene selective hydrogenation |
| CN205253072U (en) * | 2015-12-31 | 2016-05-25 | 庆阳永欣石油化工有限公司 | Preparation hydrogenation dicyclopentadiene petroleum resin's hydrogenation cauldron |
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