CN114558527A - Reaction device for producing pyridine base and implementation method thereof - Google Patents
Reaction device for producing pyridine base and implementation method thereof Download PDFInfo
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- CN114558527A CN114558527A CN202110843441.8A CN202110843441A CN114558527A CN 114558527 A CN114558527 A CN 114558527A CN 202110843441 A CN202110843441 A CN 202110843441A CN 114558527 A CN114558527 A CN 114558527A
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- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 title claims abstract description 120
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims description 80
- 238000009826 distribution Methods 0.000 claims description 53
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 38
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 36
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 12
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 230000001172 regenerating effect Effects 0.000 claims 1
- 239000000376 reactant Substances 0.000 abstract description 8
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 150000001299 aldehydes Chemical class 0.000 abstract 1
- 239000002585 base Substances 0.000 description 28
- ITQTTZVARXURQS-UHFFFAOYSA-N 3-methylpyridine Chemical compound CC1=CC=CN=C1 ITQTTZVARXURQS-UHFFFAOYSA-N 0.000 description 22
- 230000008929 regeneration Effects 0.000 description 9
- 238000011069 regeneration method Methods 0.000 description 9
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UJPKMTDFFUTLGM-UHFFFAOYSA-N 1-aminoethanol Chemical compound CC(N)O UJPKMTDFFUTLGM-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000007805 chemical reaction reactant Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- 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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
-
- 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
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/0055—Separating solid material from the gas/liquid stream using cyclones
-
- 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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
-
- 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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1872—Details of the fluidised bed reactor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/08—Preparation by ring-closure
- C07D213/09—Preparation by ring-closure involving the use of ammonia, amines, amine salts, or nitriles
- C07D213/10—Preparation by ring-closure involving the use of ammonia, amines, amine salts, or nitriles from acetaldehyde or cyclic polymers thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
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- B01J2208/00008—Controlling the process
- B01J2208/00539—Pressure
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- 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
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00893—Feeding means for the reactants
- B01J2208/00902—Nozzle-type feeding elements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
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- Combustion & Propulsion (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention discloses a reaction device for producing pyridine base and an implementation method thereof, belonging to the technical field of pyridine base production equipment. The fluidized bed and the riser are integrated, the use amount of aldehydes is reduced, the residence time of reactants is greatly prolonged, the yield of pyridine base is high, the continuous and automatic production is favorably realized, and the energy conservation of the production process is favorably realized.
Description
Technical Field
The invention relates to the technical field of pyridine base production equipment, in particular to a reaction device for producing pyridine base and an implementation method thereof.
Background
Pyridine base is an important chemical raw material, and pyridine and 3-methylpyridine have high chemical and biological reaction activity, so that pyridine and 3-methylpyridine are widely used as raw materials for synthesizing medicines, pesticides, spices, feed additives, rubber auxiliaries, dyes, surfactants, food additives, adhesives, synthetic materials and the like. The prior method for producing pyridine base mainly adopts an aldehyde ammonia method, and the adopted process is a fluidized bed process. At present, a single fluidized bed reactor is generally adopted at home and abroad, the typical structure is that a reactor with equal diameter and a regenerator are arranged in parallel, a raw material feeding distribution ring is arranged in the bottom area of the reactor, the reactor bed layer is generally a dense phase bed layer, a cyclone separator is arranged at the top of the reactor, a reaction product and a catalyst mixture are separated by the cyclone separator at the top of the reactor, a gas-phase product enters a subsequent separation system, and a catalyst returns to the reactor bed layer of the reactor through a dipleg of the cyclone separator. The invention mainly solves the problems of low production capacity and high energy consumption of the pyridine base reactor.
Compared with a fluidized bed reactor, the riser reactor has low back mixing, can effectively utilize heat and ensure higher catalyst activity. The patent document with Chinese patent No. 200810055443.5 proposes a carbon disulfide fluidized bed production process, the patent adopts a reactor structure mode of coaxially arranging a pre-lifting, a lifting pipe and a settler, reactants are added from a lifting pipe section and mixed with a catalyst from the pre-lifting to react, the reacted products enter the settler after the fast separation of the tail end of a lifting pipe reactor, the reaction products and the catalyst realize gas-solid separation through a cyclone separator in the settler, gas products are led out from a lifting pipe of the cyclone separator, the reactor adopts the lifting pipe reactor as a reaction site, the heat loss caused by back mixing can be effectively reduced, in addition, under the same treatment capacity, the diameter of the lifting pipe reactor is far smaller than that of the fluidized bed reactor due to higher operating gas velocity in the lifting pipe, so the lifting pipe reactor can adopt a nozzle for feeding, but the riser is independently adopted as the reactor, the whole adjusting capacity of the device is small, and the device is not suitable for the changeable market demands of the pyridine bases, so that the design of products with different product distributions is needed. The patent document with Chinese patent number 200810084405.2 proposes a riser and gas-solid circulating bed coupling reaction device, which adopts a method that a riser reactor and a settler are coaxially connected in series, the upper part of the riser reactor extends into the settler, the tail end of the riser reactor is provided with a gas-solid distribution plate, a circulating bed reactor is arranged above the gas-solid distribution plate, in the practical implementation case, the device is suitable for the oil refining industry, the reaction related to the oil refining industry is different from the reaction related to pyridine base synthesis, therefore, different reaction equipment needs to be designed in order to adapt to the pyridine base synthesis reaction, and the feeding of the device adopts a single nozzle form and is not suitable for the reactor with larger diameter.
Disclosure of Invention
The invention aims to provide a reaction device for producing pyridine base and an implementation method thereof, which integrate a fluidized bed and a riser, reduce the usage amount of aldehydes, greatly improve the retention time of reactants, have high pyridine base yield, are beneficial to realizing continuous and automatic production and are beneficial to saving energy in the production process.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a reaction unit of production pyridine alkali, includes catalyst reactor, catalyst reactor's upper end is provided with cyclone, cyclone is connected with the catalyst regenerator, the bottom of catalyst regenerator has catalyst reactor through the pipe connection, catalyst reactor is formed by riser and fluidized bed combination, install the heliciform distributing plate in the riser, and the upper end and the fluidized bed interconnect of riser, the lower extreme of riser is seted up there is the ammonia import, has seted up two openings on the lateral wall of riser, and two openings are connected with feed nozzle and catalyst regenerator respectively.
Further, the height of the riser is 9200mm, and the diameter is 1250 mm; the total height of the fluidized bed is 18590mm, the diameter of the upper part of the fluidized bed is 3800mm, the diameter of the lower part riser is 2400mm, the upper part and the lower part of the fluidized bed are connected through a circular truncated cone, the upper diameter and the lower diameter of the circular truncated cone are 2400mm and 3800mm respectively, and the height of the circular truncated cone is 1800 mm; the total number of the feeding nozzles is 8-12, and the height of the feeding nozzles from the bottom of the riser is 1560 mm.
Further, the height of the catalyst regenerator is 10600mm, the diameter of the catalyst regenerator is 3000mm, and the height of the connection part of the catalyst regenerator and the riser from the bottom of the riser is 800-1000 mm.
Furthermore, the positions of the lifting pipe, 600mm, 400mm and 200mm away from the bottom of the lifting pipe, are respectively welded with a spiral distribution plate, the section of each spiral distribution plate is annular, the thickness of each spiral distribution plate is 8-12mm, the inner diameter of each spiral distribution plate is 1/2 of the radius of the lifting pipe, and the outer diameter of each spiral distribution plate is the same as the radius of the lifting pipe.
Furthermore, the spiral distribution plate is provided with catalyst overflow holes of the distribution plate, the catalyst overflow holes of the distribution plate are in Gaussian distribution, and the diameter of each catalyst overflow hole of the distribution plate is
Furthermore, the opening rate of the overflow holes of the catalyst of the distribution plate on each spiral distribution plate is 54-66%.
Further, an ammonia gas conveying pipeline is arranged at the central position of the riser at the lower part of the fluidized bed.
Furthermore, a support frame is arranged between the spiral distribution plate and the bottom of the riser, an inner barrel is fixedly connected to the upper end of the support frame, the spiral distribution plate is welded to the outer portion of the inner barrel, the riser is fixedly connected to the lower end of the support frame, and the upper end of the ammonia gas conveying pipeline is inserted into the inner barrel.
According to another aspect of the present invention, there is provided an implementation method of a reaction apparatus for producing pyridine base, comprising the steps of:
s101: mixing raw materials of formaldehyde, water and acetaldehyde to form mixed aldehyde, and enabling the mixed aldehyde to enter a bottom lifting pipe from a feeding nozzle;
s102: the catalyst enters the fluidized bed from a fluidized bed start-up line;
s103: ammonia gas enters a riser from an ammonia gas conveying pipeline through a gas controller, and the ammonia gas reacts with mixed aldehyde under the catalytic action of a catalyst;
s104: the catalyst after reaction enters the top of the catalyst regenerator from the top of the fluidized bed, and the catalyst is activated in the catalyst regenerator;
s105: the activated catalyst enters the riser from the bottom of the catalyst regenerator through a regeneration pipe.
Compared with the prior art, the invention has the beneficial effects that:
1. the reaction device for producing pyridine base and the implementation method thereof provided by the invention integrate the fluidized bed and the riser, have compact integral structure, simple structure and easy manufacture, have high yield of pyridine base, are beneficial to realizing continuous and automatic production and are beneficial to saving energy in the production process.
2. The reaction device for producing pyridine base and the implementation method thereof provided by the invention have the advantages that the usage amount of aldehydes is reduced, the production cost is saved, the retention time of reactants is greatly prolonged, and the yield of pyridine base is further increased.
Drawings
FIG. 1 is an overall configuration diagram of a pyridine base production reaction apparatus according to the present invention;
FIG. 2 is a view showing the structure of a riser of the reaction apparatus for producing pyridine base according to the present invention;
FIG. 3 is a structural view of a spiral distribution plate of the reaction apparatus for producing pyridine base according to the present invention;
FIG. 4 is a distribution diagram of catalyst overflow holes of a distribution plate of the reaction apparatus for producing pyridine base according to the present invention;
FIG. 5 is a flow chart of the method for carrying out the reaction apparatus for producing pyridine base according to the present invention.
In the figure: 1. a catalyst reactor; 2. a cyclone separator; 3. a catalyst regenerator; 4. a riser tube; 5. a fluidized bed; 6. a spiral distribution plate; 7. an ammonia inlet; 8. a feed nozzle; 9. catalyst overflow holes of the distribution plate; 10. an ammonia gas delivery line; 11. a support frame.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1 to 4, a reaction apparatus for producing pyridine base comprises a catalyst reactor 1, a cyclone separator 2 is arranged at the upper end of the catalyst reactor 1, the cyclone separator 2 is connected with a catalyst regenerator 3, the bottom end of the catalyst regenerator 3 is connected with the catalyst reactor 1 through a pipeline, the catalyst reactor 1 is formed by combining a riser 4 and a fluidized bed 5, an ammonia gas conveying pipeline 10 is arranged at the central position of the riser 4 at the lower part of the fluidized bed 5, a spiral distribution plate 6 is arranged in the riser 4, the upper end of the riser 4 is connected with the fluidized bed 5, an ammonia inlet 7 is arranged at the lower end of the riser 4, two openings are arranged on the side wall of the riser 4, and the two openings are respectively connected with a feeding nozzle 8 and the catalyst regenerator 3.
Wherein, the height of the riser 4 is 9200mm, and the diameter is 1250 mm; the total height of the fluidized bed 5 is 18590mm, the diameter of the upper part of the fluidized bed is 3800mm, the diameter of the lower part riser 4 is 2400mm, the fluidized bed and the lower part riser are connected through a circular truncated cone, the upper diameter and the lower diameter of the circular truncated cone are 2400mm and 3800mm respectively, and the height of the circular truncated cone is 1800 mm; the height from the feeding nozzle 8 to the bottom of the riser 4 is 1560 mm; the height of the catalyst regenerator 3 is 10600mm, the diameter is 3000mm, and the height of the connection part of the catalyst regenerator 3 and the riser 4 from the bottom of the riser 4 is 900 mm.
A spiral distribution plate is welded at the position of the riser 4, which is 600mm, 400mm and 200mm away from the bottom, the section of the spiral distribution plate 6 is annular, the thickness of the spiral distribution plate is 8-12mm, the inner diameter of the spiral distribution plate is 1/2 of the radius of the riser 4, and the outer diameter of the spiral distribution plate is the same as the radius of the riser 4; the spiral distribution plate 6 is provided with a distribution plate catalyst overflow hole 9, the distribution plate catalyst overflow hole 9 is in Gaussian distribution, and the aperture of the distribution plate catalyst overflow hole 9 is
The aperture ratio of the catalyst overflow hole 9 of the distribution plate on each spiral distribution plate 6 is 60 percent; a supporting frame 11 is arranged between the spiral distribution plate 6 and the bottom of the riser 4, the upper end of the supporting frame 11 is fixedly connected with an inner barrel 12, the spiral distribution plate 6 is welded outside the inner barrel 12, the lower end of the supporting frame 11 is fixedly connected with the riser 4, and the upper end of the ammonia gas conveying pipeline 10 is inserted into the inner barrel 12.
Referring to fig. 5, in order to better show the flow of the implementation method of the reaction device for producing pyridine base, this embodiment now proposes an implementation method of the reaction device for producing pyridine base, which includes the following steps:
s101: mixing raw materials of formaldehyde, water and acetaldehyde to form mixed aldehyde, and enabling the mixed aldehyde to enter a bottom lifting pipe 4 from 8-12 feeding nozzles 8;
s102: the catalyst enters the fluidized bed 5 from the start-up line of the fluidized bed 5;
s103: ammonia enters a riser 4 from an ammonia conveying pipeline 10 through a gas controller, and reacts with mixed aldehyde under the catalytic action of a catalyst;
s104: the reacted catalyst enters the top of the catalyst regenerator 3 from the top of the fluidized bed 5, and the catalyst is activated in the catalyst regenerator 3;
s105: the activated catalyst enters a riser 4 from the bottom of a catalyst regenerator 3 through a regeneration pipe.
Example one
In the embodiment, when 8-nozzle feeding is adopted, the flow rates of formaldehyde, water and acetaldehyde are 3714, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2851kg/h, the top pressure of the reactor is 172kPa, and the temperature of the reactor is 460 ℃. The regeneration circulation quantity of the catalyst is 35t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 570 ℃.
Example two
When the 12-nozzle feeding is adopted in the embodiment, the flow rates of formaldehyde, water and acetaldehyde are 3714, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2851kg/h, the top pressure of the reactor is 172kPa, and the temperature of the reactor is 470 ℃. The regeneration circulation quantity of the catalyst is 35t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 580 ℃.
EXAMPLE III
In the embodiment, when the 10-nozzle feeding is adopted, the flow rates of formaldehyde, water and acetaldehyde are 3714, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2851kg/h, the top pressure of the reactor is 172kPa, and the temperature of the reactor is 470 ℃. The regeneration circulation quantity of the catalyst is 35t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 600 ℃.
Example four
In the embodiment, when the 10-nozzle feeding is adopted, the flow rates of formaldehyde, water and acetaldehyde are 3714, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2898kg/h, the top pressure of the reactor is 172kPa, and the temperature of the reactor is 480 ℃. The regeneration circulation quantity of the catalyst is 35t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 600 ℃.
EXAMPLE five
When the 12-nozzle feeding is adopted in the embodiment, the flow rates of formaldehyde, water and acetaldehyde are 3714, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2851kg/h, the top pressure of the reactor is 175kPa, and the temperature of the reactor is 480 ℃. The regeneration circulation quantity of the catalyst is 35t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 590 ℃.
Example six
In the embodiment, when the 10-nozzle feeding is adopted, the flow rates of formaldehyde, water and acetaldehyde are 3735, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2851kg/h, the top pressure of the reactor is 172kPa, and the temperature of the reactor is 480 ℃. The regeneration circulation quantity of the catalyst is 35t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 600 ℃.
EXAMPLE seven
When the 12-nozzle feeding is adopted in the embodiment, the flow rates of formaldehyde, water and acetaldehyde are 3714, 6314 and 5090kg/h respectively, the feeding flow rate of ammonia is 2851kg/h, the top pressure of the reactor is 172kPa, and the temperature of the reactor is 470 ℃. The regeneration circulation quantity of the catalyst is 36t/h, the top pressure of the regenerator is 180kPa, and the temperature of the regenerator is 600 ℃.
The data of the raw materials for the reaction in the first to seventh examples are counted, and the pyridine yield, the 3-methylpyridine yield and the total pyridine yield obtained by calculating acetaldehyde after the reaction are counted, wherein the statistics are shown in the following table 1:
TABLE 1 yield data for each reaction starting material and reaction
From the above data, the pyridine yield in example one is 45.12%; the yield of 3-methylpyridine is 28.88%, and the total yield of pyridine is 74.00% calculated according to acetaldehyde; the pyridine yield in example two is 46.26%; the yield of 3-methylpyridine is 30.91 percent, and the total yield of pyridine is 77.17 percent according to the calculation of acetaldehyde; the yield of pyridine in the third example is 45.53%; the yield of 3-methylpyridine is 29.78 percent, and the total yield of pyridine is 75.31 percent according to the calculation of acetaldehyde; the pyridine yield in example four is 46.12%; the yield of 3-methylpyridine is 29.92 percent, and the total yield of pyridine is 76.04 percent according to the acetaldehyde; example five pyridine yield 46.37%; the yield of 3-methylpyridine is 29.92%, and the total yield of pyridine is 76.29% according to the calculation of acetaldehyde; in example six; the yield of pyridine in example seven is 47.22%; the yield of 3-methylpyridine was 30.35%, and the total yield of pyridine was 77.57% based on acetaldehyde.
According to the statistical data of the first and second embodiments, under the condition that the flow rates of formaldehyde, water and acetaldehyde are not changed after the number of the feeding nozzles is increased, the reactants are dispersed more, the contact among the reactants is full, the yield of pyridine is increased from 45.12 percent to 46.26 percent, the yield of 3-methylpyridine is increased from 28.88 percent to 30.91 percent, the total yield of pyridine is increased from 74.00 percent to 77.17 percent, and according to the second to seventh examples, at the reaction temperature of 470-480, the yield of pyridine base can be improved by slightly increasing the flow rate of reactants or increasing the number of 8 feeding nozzles, from the data in examples five and six, it can be seen that the pyridine yield is reduced from 46.78% to 46.37%, the 3-methylpyridine yield is reduced from 30.12% to 29.92%, and the total pyridine yield is reduced from 76.90% to 76.29% after the formaldehyde feed flow is reduced.
In summary, the following steps: according to the reaction device for producing pyridine base and the implementation method thereof, the fluidized bed 5 and the riser 4 are integrated, the device is compact in overall structure, simple in structure and easy to manufacture, the yield of pyridine base is high, continuous and automatic production is facilitated, and energy conservation in the production process is facilitated; the usage amount of aldehydes is reduced, the production cost is saved, the retention time of reactants is greatly improved, and the yield of pyridine base is further increased.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (9)
1. The reaction device for producing pyridine base comprises a catalyst reactor (1), wherein a cyclone separator (2) is arranged at the upper end of the catalyst reactor (1), the cyclone separator (2) is connected with a catalyst regenerator (3), the bottom end of the catalyst regenerator (3) is connected with the catalyst reactor (1) through a pipeline, and the reaction device is characterized in that: the catalyst reactor (1) is formed by combining a lifting pipe (4) and a fluidized bed (5), a spiral distribution plate (6) is installed in the lifting pipe (4), the upper end of the lifting pipe (4) is connected with the fluidized bed (5), an ammonia inlet (7) is formed in the lower end of the lifting pipe (4), two openings are formed in the side wall of the lifting pipe (4), and the two openings are respectively connected with a feeding nozzle (8) and a catalyst regenerator (3).
2. A reaction unit for the production of pyridine bases according to claim 1, characterized in that the riser (4) has a height of 9200mm and a diameter of 1250 mm; the total height of the fluidized bed (5) is 18590mm, the diameter of the upper part of the fluidized bed is 3800mm, the diameter of the lower part riser (4) is 2400mm, the upper part and the lower part of the fluidized bed are connected through a circular truncated cone, the upper diameter and the lower diameter of the circular truncated cone are 2400mm and 3800mm respectively, and the height of the circular truncated cone is 1800 mm; the total number of the feeding nozzles (8) is 8-12, and the height of the feeding nozzles from the bottom of the riser (4) is 1560 mm.
3. The reaction device for producing pyridine base as claimed in claim 1, wherein the height of the catalyst regenerator (3) is 10600mm, the diameter is 3000mm, and the height of the connection between the catalyst regenerator (3) and the riser (4) is 800-1000mm from the bottom of the riser (4).
4. The reaction device for producing pyridine bases according to claim 1, wherein a spiral distribution plate is welded on the riser (4) at a distance of 600mm, 400mm and 200mm from the bottom, the section of the spiral distribution plate (6) is circular, the thickness of the spiral distribution plate is 8-12mm, the inner diameter of the spiral distribution plate is 1/2 of the radius of the riser (4), and the outer diameter of the spiral distribution plate is the same as the radius of the riser (4).
5. The reaction device for producing pyridine base according to claim 1, wherein the spiral distribution plate (6) is provided with distribution plate catalyst overflow holes (9), the distribution plate catalyst overflow holes (9) are in Gaussian distribution, and the diameter of the distribution plate catalyst overflow holes (9) is equal to
6. A reaction unit for producing pyridine bases according to claim 1, wherein the perforated ratio of the overflow holes (9) of the catalyst of the distribution plate on each spiral distribution plate (6) is 54-66%.
7. A reaction apparatus for producing pyridine base according to claim 1, characterized in that ammonia gas delivering line (10) is provided at the center of riser (4) at the lower part of fluidized bed (5).
8. The reaction device for producing pyridine base according to claim 1, wherein a support frame (11) is disposed between the spiral distribution plate (6) and the bottom of the riser (4), an inner tube (12) is fixedly connected to the upper end of the support frame (11), the spiral distribution plate (6) is welded to the outer portion of the inner tube (12), the riser (4) is fixedly connected to the lower end of the support frame (11), and the upper end of the ammonia gas delivery pipeline (10) is inserted into the inner tube (12).
9. A method for implementing a reaction apparatus for producing pyridine base according to any one of claims 1 to 8, comprising the steps of:
s101: mixing raw materials of formaldehyde, water and acetaldehyde to form mixed aldehyde, and enabling the mixed aldehyde to enter a bottom lifting pipe (4) from a feeding nozzle (8);
s102: the catalyst enters the fluidized bed (5) from the start-up line of the fluidized bed (5);
s103: ammonia gas enters the riser (4) from an ammonia gas conveying pipeline (10) through a gas controller, and reacts with the mixed aldehyde under the catalytic action of the catalyst;
s104: the reacted catalyst enters the top of the catalyst regenerator (3) from the top of the fluidized bed (5), and the catalyst is activated in the catalyst regenerator (3);
s105: the activated catalyst enters a lifting pipe (4) from the bottom of a catalyst regenerator (3) through a regenerating pipe.
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| CN102730636A (en) * | 2012-07-03 | 2012-10-17 | 重庆大学 | Hydrogen production method by steam reforming in combined reactor and device thereof |
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| CN108636303A (en) * | 2018-05-23 | 2018-10-12 | 安徽国星生物化学有限公司 | A kind of recirculating fluidized bed prepares the consersion unit of pyridine base |
| CN111606771A (en) * | 2020-06-11 | 2020-09-01 | 中国石油化工股份有限公司 | Methanol and light hydrocarbon coupling cracking device and method |
| CN113041963A (en) * | 2021-03-25 | 2021-06-29 | 洛阳智邦石化设备有限公司 | Promote catalyst distribution plate structure in advance |
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| CN102899078A (en) * | 2011-07-29 | 2013-01-30 | 中国石油化工股份有限公司 | Catalytic cracking method for producing propylene |
| CN102730636A (en) * | 2012-07-03 | 2012-10-17 | 重庆大学 | Hydrogen production method by steam reforming in combined reactor and device thereof |
| CN108636303A (en) * | 2018-05-23 | 2018-10-12 | 安徽国星生物化学有限公司 | A kind of recirculating fluidized bed prepares the consersion unit of pyridine base |
| CN111606771A (en) * | 2020-06-11 | 2020-09-01 | 中国石油化工股份有限公司 | Methanol and light hydrocarbon coupling cracking device and method |
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