CN115055124A - Acrylonitrile fluidized bed reaction device and process - Google Patents
Acrylonitrile fluidized bed reaction device and process Download PDFInfo
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- CN115055124A CN115055124A CN202210712467.3A CN202210712467A CN115055124A CN 115055124 A CN115055124 A CN 115055124A CN 202210712467 A CN202210712467 A CN 202210712467A CN 115055124 A CN115055124 A CN 115055124A
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- propylene
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- ammonia
- pipes
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 58
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title abstract description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 198
- 238000009826 distribution Methods 0.000 claims abstract description 147
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 137
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 137
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 102
- -1 alkene nitrile Chemical class 0.000 claims abstract description 4
- 239000011148 porous material Substances 0.000 claims description 20
- 230000003068 static effect Effects 0.000 claims description 16
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 abstract description 11
- 238000007086 side reaction Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 description 20
- 239000007789 gas Substances 0.000 description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 239000006227 byproduct Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000013386 optimize process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- GLAKNHGQBRSLIO-UHFFFAOYSA-N azane;prop-1-ene Chemical group N.CC=C GLAKNHGQBRSLIO-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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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
- B01J8/18—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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/24—Preparation of carboxylic acid nitriles by ammoxidation of hydrocarbons or substituted hydrocarbons
- C07C253/26—Preparation of carboxylic acid nitriles by ammoxidation of hydrocarbons or substituted hydrocarbons containing carbon-to-carbon multiple bonds, e.g. unsaturated aldehydes
-
- 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
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an alkene nitrile fluidized bed reaction device, which comprises a reactor, wherein the reactor comprises a body part and a lower cone part, an ammonia/propylene distributor is arranged on the body part, and the inlet end of the ammonia/propylene distributor is connected with a homomixer for homogenizing ammonia and propylene; an air distributor is arranged in the lower cone part, and an inlet of the air distributor is connected with an air inlet pipe; and a sieve mesh distribution plate is arranged between the body part and the lower cone part. Also provides an acrylonitrile fluidized bed reaction process. The invention reduces the generation of various side reactions, improves the yield of acrylonitrile, reduces the generation probability of the oxazole impurity and creates conditions for the scale enlargement of the acrylonitrile reaction device by innovatively designing the engineering and process conditions of the fluidized bed reaction device.
Description
Technical Field
The invention belongs to the technical field of chemical engineering processes, and relates to an acrylonitrile fluidized bed reaction device and an acrylonitrile fluidized bed reaction process.
Background
The propylene ammoxidation for producing acrylonitrile is a fluidized bed reaction process, and through technical progress for many years, although the conversion rate of propylene reaches more than 98%, because inhibition means for side reaction is deficient, a large amount of byproducts are generated, so that the yield of acrylonitrile is reduced, the production energy consumption is increased, and the product quality of acrylonitrile is seriously influenced by partial byproducts such as oxazole and the like. The yield of the most advanced industrial acrylonitrile fluidized bed reaction device at present is improved to about 80 percent, and the content of the byproduct oxazole is reduced to about 20 ppm.
Chinese patent document CN102372650B proposes an active ingredient containing the following general formula: mo 12 Bi a Fe b Ni c X d Y e Z f Q g K h O x The catalyst solves the problems of low content of Mo element tetrahedral crystal phase structure, low acrylonitrile selectivity and reduced acrylonitrile yield along with the extension of reaction time in the prior art. The catalyst is prepared under optimized process conditions, namely: the mol ratio of the raw materials of propylene/ammonia/air is 1/1.05-1.30/9.2-9.8, the reaction temperature is 420-440 ℃, the reaction pressure is 0.06-0.14 Mpa, and the WWH is 0.06-0.10 h -1 Under the condition, the technical aim that the yield of the acrylonitrile is more than 78 percent is realized.
Chinese patent document CN201210412589.7 proposes a fluidized bed catalyst and a method for preparing unsaturated nitrile by ammoxidation, which mainly solve the problems of low conversion rate of propylene, low selectivity of acrylonitrile, and rapid decrease of acrylonitrile yield caused by low oxygen storage and release capacity and low specific surface area of acrylonitrile catalyst in the prior art. By using silica sol as carrier and active component Mo 12 Bi a Fe b Ni c X d Y e Z f K g O x Wherein Y is two or more rare earth elements which are firstly formed into solid solution and then prepared into the catalyst. The catalyst realizes the technical goal that the yield of acrylonitrile is more than 78 percent under the optimized process condition.
The chinese patent document CN201310727958.6 provides a process for producing acrylonitrile, which is to use a commercial C49MC type catalyst in a fluidized bed reactor with a multi-layer perforated plate distribution plate, and react under the conditions of a molar ratio of propylene to ammonia of 1:1.15, a pressure of 0.06Mpa and a temperature of 435 ℃, so as to achieve the goal of remarkably reducing the conversion rate of oxazole impurity generated in the process of producing acrylonitrile by 0.02 wt% or less. The yield of acrylonitrile is more than 78 percent and the content of oxazole impurity is less than 0.02 percent (weight).
The engineering limit that the yield of acrylonitrile is more than 80 percent can not be broken through in the prior art. Therefore, there is a great need in the art to provide a high yield, low oxazole production acrylonitrile fluidized bed reactor and process based on engineering and process innovations.
Disclosure of Invention
The invention aims to provide an acrylonitrile fluidized bed reaction device and a process with high yield and low oxazole output. By innovatively designing engineering and process conditions of the fluidized bed reaction device, the generation of various side reactions is reduced, the yield of acrylonitrile is improved, the generation probability of oxazole impurity is reduced, and conditions are created for the scale expansion of the acrylonitrile reaction device.
One of the purposes of the invention is to provide an alkene nitrile fluidized bed reaction device, which adopts the following technical scheme:
an alkene nitrile fluidized bed reaction device comprises a reactor, wherein the reactor comprises a body part and a lower cone part, an ammonia/propylene distributor is arranged on the body part, and the inlet end of the ammonia/propylene distributor is connected with a homomixer for homogenizing ammonia and propylene; an air distributor is arranged in the lower cone part, and an inlet of the air distributor is connected with an air inlet pipe; and a sieve mesh distribution plate is also arranged between the ammonia/propylene distributor and the air distributor.
Preferably, the cone angle of the lower cone part ranges from 90 degrees to 105 degrees.
Preferably, a lower tangent of the fluidized bed is formed at the joint of the body part and the lower cone part, and the distance between the air distributor and the lower tangent of the fluidized bed is 1/3-1/2 of the cone height of the lower cone part;
the sieve mesh distribution plate is arranged above the lower tangent line of the fluidized bed and is 200 mm-300 mm away from the lower tangent line of the fluidized bed.
Preferably, the ammonia/propylene distributor is positioned 200 mm-600 mm above the sieve mesh distribution plate.
Preferably, the homomixer comprises a shell, the shell is a cylinder, a plurality of propylene distribution pipes and static mixing units are arranged in the shell, the propylene distribution pipes are arranged along the flowing direction of ammonia, and adjacent propylene distribution pipes are connected through a propylene gas transmission branch pipe;
the distance between the tail end of the propylene distribution pipe and the front end of the static mixing unit is 1-3 times of the diameter of the homogenizing mixer; one of the propylene distributing pipes is positioned on the central line of the shell, and the rest propylene distributing pipes are circumferentially and symmetrically distributed outside the central line.
Further, the circumferential diameter of the propylene distribution pipe is 2/3 of the diameter of the homogenizer shell;
any spray holes are uniformly formed in the side wall of the propylene distribution pipe in a triangular arrangement mode, and the diameter of each spray hole is 10-15 mm.
Preferably, the air distributor comprises two main air pipes which are in cross communication at 90 degrees and air branch pipes which are communicated with the main air pipes, the air branch pipes are perpendicular to the main air pipes and are distributed at intervals, and the main air pipes and the air branch pipes are positioned in the same horizontal plane;
the air inlet pipe is connected with the crossing center of the two air main pipes;
the lower side wall of the air branch pipe is provided with distribution holes, the distribution holes are concentrated in an area with an included angle alpha between two sides of a vertical axis, and the value of alpha is 20-45 degrees.
Furthermore, the pipe center distance between adjacent air branch pipes is 2-3 times of the diameter of the air branch pipe.
Further, the diameter of the air distributor is 0.8-0.9 times of the diameter of the section of the cone where the air distributor is located;
furthermore, the distribution holes on the lower side wall of the air branch pipe are consistent in size, the distribution holes are uniformly distributed on the lower side wall of the air branch pipe, and the aperture of each distribution hole is 5-15 mm.
Preferably, the sieve pore distribution plate is a perforated plate with the diameter equivalent to that of the reactor, and the opening rate is 15-35%; the size of the opening is 30-50 mm, and the openings are uniformly distributed on the distribution plate.
Preferably, the ammonia/propylene distributor comprises 4 distribution main pipes which are arranged in a 90-degree crossed manner, 4 fan-shaped areas are defined by the distribution main pipes and the inner wall of the reactor, a plurality of distribution branch pipes are arranged on any one distribution main pipe at intervals and are vertically communicated, and the distribution branch pipes in the adjacent fan-shaped areas are respectively arranged in the vertical direction; the distribution main pipe and the distribution branch pipes are positioned in the same horizontal plane;
any one of the distribution branch pipes is of a reducing structure, the diameter of the connection part of the distribution branch pipe and the distribution main pipe is the largest, and the pipe diameter is smaller as the distance from the main pipe is farther.
Furthermore, two rows of nozzles are arranged on the lower side wall of the distribution branch pipe, the opening shape of the nozzles on the pipe wall is a tapered shape, and the tapered angle beta is 25-35 degrees;
the nozzles are divided into cylinders outside the distribution pipe, the two rows of nozzles are symmetrically distributed along the vertical direction, and the included angle between the two rows of nozzles and the vertical direction is 25-35 degrees.
The invention also aims to provide an acrylonitrile fluidized bed reaction process, which adopts the following scheme:
uniformly distributed air is introduced into the lower cone part of the reactor through an air distributor, and is diffused and ascended to further be uniformly distributed through a sieve pore distribution plate; meanwhile, the propylene and the ammonia enter the ammonia/propylene distributor at the body part of the reactor through the homomixer to be uniformly distributed and then sprayed out, and are fully mixed with the air uniformly distributed by the sieve pore distribution plate, wherein the ratio of the propylene, the ammonia and the air is controlled to be 1/(1.05-1.20)/(8.2-8.8).
Preferably, in the mixing of ammonia and propylene in the homomixer, the ammonia flows as a mixed gas inside the homomixer shell and outside the propylene distribution pipe, and the hollow pipe flow velocity of the ammonia in the homomixer shell is 5-10 m/s; the flow rate of the propylene in the propylene distribution pipe ranges from 6m/s to 15 m/s; the ammonia and the propylene flow out and are mixed in the shell, and then are further mixed uniformly by the static mixing unit;
uniformly mixing ammonia and propylene, then respectively entering an ammonia/propylene distributor through 4 distribution main pipes, flowing out of distribution branch pipes correspondingly connected with the distribution main pipes at the same flow speed of 3-10 m/s, and downwards spraying out of the distribution branch pipes through nozzles at the initial speed of 10-20 m/s to enter a body part;
in the air distributor, control air enters 2 main air pipes from an air inlet pipe through the cross center of the two main air pipes and then enters the branch air pipes, flows out of distribution holes in the lower side walls of the branch air pipes at a speed of 3-6 m/s and enters the lower cone part, is diffused and rises, and is further rectified and uniformly distributed by a sieve mesh distribution plate to be mixed with ammonia/propylene sprayed by the ammonia/propylene distributor.
Further, controlling the linear speed range in the reactor to be 0.5-1.2 m/s;
the pressure of the reactor is controlled between 0.14MPa and 0.16MPa (a).
The reaction temperature is controlled between 420 ℃ and 440 ℃.
The invention can bring the following beneficial effects:
1) the invention adopts an ammonia/propylene homomixer with a special structure to ensure that propylene and ammonia are mixed in a micro scale before entering a reactor; the air distributor with a special structure is adopted to ensure that the air is uniformly distributed on the cross section of the reactor; in the ammonia/propylene distributor, the gas in the distribution branch pipe is kept at a constant speed by a specific structural design, the mixed gas of ammonia and propylene can be better and uniformly distributed on the section of the whole reactor, and a specific jet flow direction and flow speed are formed by utilizing a special injection pore structure of the ammonia-propylene distributor, so that the ascending air can be stirred and mixed, and the rapid mixing with the air is facilitated; the special reactor arrangement is combined, and the specific arrangement of the cone bottom, the air distributor and the ammonia/propylene distributor achieves the uniform mixing of air, ammonia and propylene on the whole reactor interface, and promotes the improvement of the reaction efficiency.
2) By combining the special device and process, the invention can reduce the excess air coefficient, maintain the propylene/ammonia/air ratio of 1/1.05-1.20/8.2-8.8, and reduce the generation of CO while ensuring the improvement of the yield of acrylonitrile 2 CO and oxazole production rates.
Drawings
FIG. 1 is a schematic view showing the structure of a fluidized bed reactor for acrylonitrile according to the present invention.
Fig. 2 is an enlarged structural view of the homomixer of fig. 1.
FIG. 3 is a schematic view showing the arrangement of propylene distribution pipes in FIG. 2.
Fig. 4 is an enlarged structural view of the air distributor of fig. 1.
Fig. 5 is a schematic view showing the distribution of the openings of the air branch pipes in fig. 4.
FIG. 6 is an enlarged view of the ammonia/propylene distributor of FIG. 1.
Fig. 7 is an enlarged view of the corresponding nozzle on the distribution manifold of fig. 6.
The notations in the figures have the following meanings:
1-reactor, 10-body part, 11-lower cone part;
2-ammonia/propylene distributor, 20-distribution main pipe, 21-distribution branch pipe and 22-nozzle;
3-homogenizing mixer, 30-shell, 31-propylene distribution pipe, 32-propylene gas transmission branch pipe and 33-static mixing unit;
4-air distributor, 40-main air pipe, 41-branch air pipe;
5-mesh distribution plate.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
According to an embodiment of the present invention, as shown in fig. 1, an acrylonitrile fluidized bed reactor is provided, which includes a reactor 1, the reactor 1 includes a main body 10 and a lower cone 11, an ammonia/propylene distributor 2 is disposed on the main body 10, and an inlet end of the ammonia/propylene distributor 2 is connected to a homomixer 3 for homogenizing ammonia and propylene; an air distributor 4 is arranged in the lower cone part 11, and an inlet of the air distributor 4 is connected with an air inlet pipe; and a sieve mesh distribution plate 5 is also arranged between the ammonia/propylene distributor 2 and the air distributor 4.
Based on this example, a specific cone-containing reactor 1, air distributor 4 and ammonia/propylene distributor 2 combination was used to achieve uniform mixing of air and ammonia, propylene across the entire reactor interface.
A lower tangent line L of the fluidized bed is formed at the joint of the body part 10 and the lower cone part 11, and as a preferred embodiment, the cone angle a of the lower cone part 11 ranges from 90 degrees to 105 degrees; if the cone angle is too small, the aim of small-scale uniform diffusion of air at the lower tangent of the fluidized bed, namely the lower tangent L of the reactor cannot be fulfilled; if the cone angle is too large, it will not only have a small effect on the uniform distribution of air over the entire cross-section of the fluidized bed, but also be detrimental to the static free flow during the unloading of the catalyst from the reactor 1. Preferably, the distance between the air distributor 4 and the lower tangent L of the fluidized bed is 1/3-1/2 of the taper height of the lower taper part 11; so that the uniformly distributed air can enter the body part 10 of the reactor at a constant speed. The sieve mesh distribution plate 5 is arranged above the lower tangent L of the fluidized bed and is at a vertical distance of 200-300 mm from the lower tangent L of the fluidized bed; facilitating further uniform entry of air into the body portion 10. The ammonia/propylene distributor 2 is positioned 200 mm-600 mm above the sieve mesh distribution plate 5, so that the uniformly mixed ammonia/propylene uniformly enters the body part 10 and is mixed with the uniformly distributed air interface.
As another preferred embodiment, referring to fig. 2 and 3, the homomixer 3 includes a housing 30, the housing 30 is a cylinder, a plurality of (e.g. more than 4) propylene distribution pipes 31 and static mixing units 33 are disposed in the housing 30, the propylene distribution pipes 31 are arranged along the flow direction of ammonia, and adjacent propylene distribution pipes 31 are connected by a propylene gas transmission branch pipe 32;
the distance between the tail end of the propylene distribution pipe 31 and the front end of the static mixing unit 33 is 1-3 times of the diameter of the homomixer 3; one of the propylene distributing pipes 31 is located on the center line of the shell, and the rest propylene distributing pipes 3 are symmetrically distributed in a circle outside the center line.
More preferably, the diameter of the circumference of the propylene distribution pipe 31 is 2/3 of the diameter of the homogenizer shell 30; the side wall of any propylene distribution pipe 31 is uniformly provided with jet holes in a triangular arrangement, and the diameter of each jet hole is 10-15 mm; the number of the openings is controlled so that the exit velocity of propylene is 20 to 40 m/s. In addition, the static mixing unit 33 is a conventional static mixing structure, and is formed by cross arrangement of a normal rotation unit and a different rotation unit; the number of the static mixing units is not less than 4.
Accordingly, in the mixing of ammonia and propylene, ammonia as a gas to be mixed flows through the homomixer case 30 from the inside to the outside of the propylene distribution pipe 31, and the empty pipe flow rate of ammonia in the homomixer case 30 is controlled to be 5 to 10 m/s; the flow rate of propylene in the propylene distribution pipe 31 ranges from 6 to 15 m/s. Therefore, the structure and the mixing process of the homomixer 3 can ensure that the propylene and the ammonia are uniformly mixed within less than 1s, and the maximum concentration difference of the two gases in the same section after mixing is less than 0.5 percent.
As a further preferred embodiment, referring to fig. 4 and 5, the air distributor 4 includes two main air pipes 40 that are cross-connected at 90 °, and a plurality of air branch pipes 41 connected to the main air pipes 40, wherein the air branch pipes 41 are uniformly spaced and distributed perpendicular to the main air pipes 40, and the main air pipes 40 and the air branch pipes 41 are located in the same horizontal plane;
the air inlet pipe is connected with the crossing center (as the inlet of the air distributor 4) of the two main air pipes 40, and the pipe center distance d between the adjacent air branch pipes 41 is 2-3 times of the diameter of the air branch pipes;
the air distributor 4 is in a disc shape, and the diameter of the air distributor is 0.8-0.9 times of the diameter of the section of the lower cone part 11;
the lower side wall of the air branch pipe 4 is provided with distribution holes, the distribution holes are concentrated in an area with included angles on two sides of a vertical axis as b, and the range value of the angle b is 20-45 degrees.
When in application, the distribution holes are controlled to be consistent and uniformly distributed, and the aperture is 5-15 mm. The air outflow speed from the distribution holes is controlled to be 3-6 m/s, the diffusion flow pattern of the air is enhanced, and flow field stripping caused by high flow speed is reduced.
In the embodiment, through the innovation of the structure and the distribution flow rate and the position of the air distributor 4 in the lower cone part 11, the flow rate is uniform when the air rises to the bottom end of the lower tangent line L of the reactor, the speed difference between different points of the same section is less than 5 percent, and the microcosmic uniformity is achieved after the air is uniformly distributed by the sieve pore distribution plates 5.
In another preferred embodiment, the sieve pore distribution plate 5 is an open pore plate with a diameter equivalent to that of the reactor 1, and the open pore ratio is 15-35%; if the open porosity is too low, the effect on the distribution is insignificant, and the pressure drop is too large, if the open porosity is too high, it does not act to homogenize the air distribution. The sieve pore size of sieve pore distributing plate 5 is 30 ~ 50mm to according to triangle-shaped or rectangle equipartition on the distributing plate. Here, the mesh distribution plate 5 serves to further uniformly distribute and rectify the air in the case where the air flow rate is substantially uniform.
As still another preferred embodiment, the structure of the ammonia/propylene distributor 2 is shown in FIGS. 6 and 7; wherein fig. 6 shows the arrangement of the distribution pipes and fig. 7 shows the distribution of the nozzles on the distribution pipes.
The ammonia/propylene distributor 2 comprises 4 distribution main pipes 20 which are arranged in a 90-degree crossed manner, the distribution main pipes 20 and the inner wall of the reactor 1 enclose 4 fan-shaped areas, any one distribution main pipe 20 is vertically communicated with a plurality of distribution branch pipes 21 at a certain interval, and the distribution branch pipes 21 in the adjacent fan-shaped areas are respectively distributed in the vertical direction; the distribution main pipe 20 and the distribution branch pipes 21 are positioned in the same horizontal plane;
any one of the distribution branch pipes 21 is of a reducing structure, the diameter of the connection part of the distribution branch pipe 21 and the distribution main pipe 20 is the largest, and the pipe diameter of the direction far away from the distribution main pipe 20 is reduced, so that the flow velocity of gas in the distribution branch pipes 21 is kept the same, and the flow velocity is within the range of 3-10 m/s.
Preferably, two rows of nozzles 22 are arranged on the lower side wall of the distribution branch pipe 21, the opening shape of the nozzle 22 on the pipe wall is a tapered shape, and the tapered angle beta is 25-35 degrees;
the part of the nozzle 22, which is positioned outside the distribution pipe, is cylindrical, the diameter of the nozzle is 15-20 mm, the length of the nozzle is 20-50 mm, two rows of nozzles are taken as axes in the vertical direction, and the nozzles are respectively distributed at two sides of the axes by an included angle alpha, wherein the included angle alpha is 25-35 degrees; and the two rows of nozzles 22 are alternately distributed along the extending direction of the distribution branch pipe 21. So as to stir and divide the air on the scale as small as possible, and to maintain the initial speed of the gas sprayed from the nozzle 22 within 10-20 m/s, thereby enabling the propylene-ammonia mixed gas to perform cross cutting and mixing on the rising air at a certain angle, and increasing the mixing uniformity of the three gases.
In combination with the above, the ammonia/propylene distributor 2 of the present embodiment functions to: guarantee ammonia, propylene mist evenly distributed in whole reaction cross-section to cut the mixture to the rising air, accomplish the homogeneous mixing between messenger's propylene, ammonia, the air three.
According to the embodiment, an acrylonitrile fluidized bed reaction process can be further implemented, wherein uniformly distributed air is introduced into the lower cone part 11 of the reactor 1 through the air distributor 4, is diffused and ascended, and is further uniformly distributed through the sieve pore distribution plate 5; meanwhile, the propylene and the ammonia enter the ammonia/propylene distributor 2 of the reactor body part 10 through the homomixer 3, are uniformly distributed and then sprayed out, and are mixed with the air uniformly distributed by the sieve pore distribution plate, wherein the ratio of the propylene, the ammonia and the air is controlled to be 1/(1.05-1.20)/(8.2-8.8).
Preferably, in the mixing of ammonia and propylene in the homomixer 3, ammonia flows as a gas to be mixed in the homomixer case 30 through the inner propylene distribution pipe 31 and the outer propylene distribution pipe 31, and the empty pipe flow velocity of ammonia in the homomixer case 30 is 5 to 10 m/s; the flow rate of propylene in the propylene distribution pipe 31 ranges from 6 to 15 m/s; then, the mixture is further mixed uniformly by a static mixing unit 33;
ammonia and propylene are uniformly mixed and then respectively enter an ammonia/propylene distributor 2 through 4 distribution main pipes 20, flow out of distribution branch pipes 21 correspondingly connected with the distribution main pipes 20 at the same flow speed of 3-10 m/s, and are downwards sprayed out through nozzles at the initial speed of 10-20 m/s to enter a body part 10;
in the air distributor 4, control air enters the 2 main air pipes 40 from an air inlet pipe through the intersection center of the two main air pipes 40, then enters the air branch pipe 41, flows out of the distribution holes in the lower side wall of the air branch pipe 41 at a speed of 3-6 m/s, enters the lower cone part 11, is diffused and ascended, is further rectified and uniformly distributed through the sieve pore distribution plate 5, and then is fully mixed with ammonia/propylene sprayed out of the ammonia/propylene distributor 2.
The homomixer structure and the mixing process can ensure that the propylene and the ammonia are uniformly mixed within less than 1s, and the maximum concentration difference of the two gases in the same cross section is less than 0.5 percent after mixing; the air distribution and the ammonia inlet/propylene distribution of a specific process are combined, so that the propylene-ammonia mixed gas performs cross cutting mixing on the rising air at a certain angle, and the mixing uniformity of the three gases is further increased. Therefore, under the specific proportioning condition of the invention, the full synergy of proportioning and microcosmic mass transfer effect is achieved, the energy consumption of the air compressor is saved, the side reaction caused by oxygen content is fully reduced, and the reaction efficiency and precision of the invention are improved.
In addition, the linear speed range in the reactor is controlled to be 0.5-1.2 m/s, and the catalyst can be suitable for acrylonitrile fluidized bed catalysts with different particle size distributions.
The pressure of the reactor is controlled between 0.14MPa and 0.16MPa (a). The pressure is too high to favor the acrylonitrile synthesis (molar increase) reaction and, conversely, does not provide sufficient back-up pressure for downstream processing.
The reaction temperature is dependent on the optimum reaction temperature of the catalyst and is controlled between 420 ℃ and 440 ℃ in order to reduce the formation of by-products.
Based on the innovative engineering device and the process provided by the embodiment, under the same catalyst condition, the yield of acrylonitrile can be improved by 3 to 5 percent, the generation rate of oxazole is reduced by less than 20ppm, and the energy consumption of a reaction device is reduced by about 3 percent.
The reason is that in the acrylonitrile reaction device, byproducts generated under the condition of uniformly distributing propylene, ammonia and oxygen are mainly hydrocyanic acid and acetonitrile, and the yield of the two byproducts is mainly determined by the selectivity of the catalyst and is controlled by the selection of the catalyst as shown in reaction formulas (7) and (8). But CO 2 The generation of CO is largely caused by the uneven distribution of propylene, ammonia, oxygen and excess oxygen (or local excess oxygen), and the excess oxygen due to the high oxygen ratio causes a large amount of oxygen to attack propylene to generate, as shown in reaction formulas (3), (4), (5) and (6). The oxazole impurity is formed by the reaction of acrylonitrile with oxygen due to excess oxygen, as shown in equation (9). The present invention achieves the above-mentioned properties by deeply and microscopically uniformly mixing and distributing propylene, ammonia, and oxygen to suppress the occurrence of these side reactions, particularly, the reaction formulae (3), (4), (5), (6), and (9).
Main reaction of an acrylonitrile device:
C 3 H 6 +NH 3 +3/2O 2 →C 3 H 3 N+3H 2 O (1)
side reaction:
NH 3 +3/4O 2 →1/2N 2 +3/2H 2 O (2)
C 3 H 6 +9/2O 2 →CO 2 +3H 2 O (3)
C 3 H 6 +3O 2 →2CO+3H 2 O (4)
C 3 H 6 +3/2O 2 →C 3 H 4 O 2 +H 2 O (5)
C 3 H 6 +O 2 →C 3 H 4 O+H 2 O (6)
C 3 H 6 +3NH 3 +3/2O 2 →3HCN+6H 2 O (7)
C 3 H 6 +3/2NH 3 +3/2O 2 →3/2C 2 H 3 N+3H 2 O (8)
2C 3 H 3 N+3/2O 2 →2C 3 H 3 NO (9)
several application examples are provided below for further proof of effectiveness:
comparative example 1
The device comprises the following steps: on the basis of the device provided by the invention, the following differences are formed: mixing propylene and ammonia by adopting a conventional static mixer outside the reactor; the cone angle a of the reactor lower cone 11 is 90 °, the air duct enters directly into the lower cone 11 (without distributor); only a sieve plate is arranged 200mm above the lower tangent line of the reactor, the opening rate of the sieve plate is 15 percent, and the pore size is 35 mm; an ammonia/propylene distributor (adopting a distributor structure with a traditional structure) is arranged at the position of 800mm above the lower tangent line of the reactor.
The molar ratio of the raw materials is as follows: propylene/ammonia/air ═ 1/1.2/9.5
Catalyst: the catalyst is a commercial catalyst taking molybdenum and bismuth as main activities, and the particle size distribution of the catalyst is as follows: d 50 ＝44μm。
Catalyst reaction pressure of components: 0.16MPa (a), reaction temperature: 435 ℃, fluidized bed linear speed: 0.7 m/s.
The molar ratios of the starting materials and the reaction results are shown in Table 1.
Example 1
The device comprises the following steps: the homomixer 3 of the invention is adopted outside the reactor to mix propylene and ammonia, and the characteristic parameters of the homomixer 3 are as follows: the diameter of the jet hole is 10mm, and the outlet speed of the propylene is 30 m/s; the number of the static mixing units 33 is 4; the reactor adopts the structure of the invention; the cone angle a of the lower cone part 11 is 100 degrees, air is distributed into the lower cone part 11 through the air distributor 4, the air distributor 4 is away from the cone height of 1/3 degrees of the lower tangent line of the reactor, the distribution holes are concentrated on the lower side wall of the distribution branch pipe 41 and in a symmetrical area forming an included angle b of 30 degrees with the vertical direction, the aperture of each distribution hole is 10mm, and the flowing speed of the air from the distribution holes is 4 m/s; a sieve pore distribution plate 5 is arranged at the position 100mm above a lower tangent line L of the reactor, the opening rate of the sieve pore plate is 18 percent, and the pore size is 35 mm; the ammonia/propylene distributor 2 is arranged at the position 800mm above the lower tangent line of the reactor, the ammonia/propylene distributor 2 adopts the structure of the invention, the taper angle beta of the nozzles 22 is 30 degrees, the diameter of the nozzles is 20mm, the length of the nozzles is 30mm, the symmetrical included angle alpha of the two rows of nozzles along the vertical direction is 30 degrees, the flow velocity of ammonia/propylene gas in each distribution branch pipe 21 is 4m/s, and the ejection velocity of the ammonia/propylene gas from the nozzles 22 is 15 m/s.
The molar ratio of the raw materials is as follows: propylene/ammonia/air ═ 1/1.2/8.5;
catalyst: same as in comparative example 1;
the reaction pressure, reaction temperature and fluidized bed linear velocity were the same as in comparative example 1.
The reaction results are shown in Table 1.
Example 2
The procedure was as in example 1 except that the taper angle a of the lower reactor cone 11 in the apparatus was 90 °.
The reaction results are shown in Table 1.
Example 3
The procedure of example 1 was repeated, except that the number of the static mixing units 33 in the ammonia/propylene homomixer 2 was 5.
The reaction results are shown in Table 1.
Example 4
The same procedure as in example 1 was repeated, except that the diameter of the distribution holes in the air distributor 4 in the apparatus was 15mm, and the velocity of air flowing out from the distribution holes was 3 m/s.
The reaction results are shown in Table 1.
Example 5
Ammonia/propylene distributor in the removal apparatus 2: the nozzle 22 was the same as in example 1 except that the tapered angle β of the injection hole was 25 °, the nozzle diameter was 16mm, the length was 30mm, and the velocity of the ammonia/propylene gas injected from the nozzle was 20 m/s.
And the reaction results are shown in Table 1.
Example 6
The same procedure as in example 6 was repeated, except that the nozzles of the two rows of the ammonia/propylene distributor 2 in the apparatus were vertically symmetrical at an angle of 35 °.
The reaction results are shown in Table 1.
Example 7
The procedure was as in example 1 except that the ammonia/propylene distributor 2 was placed 600mm above the lower tangent of the reactor.
The reaction results are shown in Table 1.
Example 8
Except the raw material proportion: the procedure of example 1 was repeated except that the ratio of propylene/ammonia/air was 1/1.2/8.2.
The reaction results are shown in Table 1.
Example 9
Except the raw material proportion: the procedure was repeated except that propylene/ammonia/air was changed to 1/1.15/8.2, which was the same as in example 1.
The reaction results are shown in Table 1.
Example 10
Except the raw material proportion: the procedure of example 1 was repeated except that the ratio of propylene/ammonia/air was 1/1.3/8.8.
Example 11
The procedure was as in example 1 except that the feed ratio was 1/1.05/8.2.
The reaction results are shown in Table 1.
TABLE 1 reaction results of the examples
It should be noted that the above embodiments can be freely combined as necessary. The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. An alkene nitrile fluidized bed reaction device is characterized in that:
the reactor comprises a reactor, wherein the reactor comprises a body part and a lower cone part, the body part is provided with an ammonia/propylene distributor, and the inlet end of the ammonia/propylene distributor is connected with a homomixer for homogenizing ammonia and propylene; an air distributor is arranged in the lower cone part, and an inlet of the air distributor is connected with an air inlet pipe; and a sieve mesh distribution plate is also arranged between the ammonia/propylene distributor and the air distributor.
2. The acrylonitrile fluidized bed reactor as claimed in claim 1, wherein:
the cone angle range of the lower cone part is 90-105 degrees; and/or the presence of a gas in the gas,
the joint of the body part and the lower cone part forms a lower tangent of the fluidized bed, and the distance between the air distributor and the lower tangent of the fluidized bed is 1/3-1/2 of the cone height of the lower cone part; the sieve mesh distribution plate is arranged above the lower tangent line of the fluidized bed and is 200-300 mm away from the lower tangent line of the fluidized bed; and/or the presence of a gas in the gas,
the ammonia/propylene distributor is positioned 200 mm-600 mm above the sieve pore distribution plate.
3. The acrylonitrile fluidized bed reactor as claimed in claim 1, wherein:
the homogenizing mixer comprises a cylindrical shell, a plurality of propylene distribution pipes and a static mixing unit are arranged in the shell, the propylene distribution pipes are arranged along the flowing direction of ammonia, and adjacent propylene distribution pipes are connected through a propylene gas transmission branch pipe;
the distance between the tail end of the propylene distribution pipe and the front end of the static mixing unit is 1-3 times of the diameter of the homomixer; one of the propylene distributing pipes is positioned on the central line of the shell, and the rest propylene distributing pipes are circumferentially and symmetrically distributed outside the central line.
4. An acrylonitrile fluidized bed reactor as claimed in claim 3, wherein:
the circumferential diameter of the propylene distribution pipe is 2/3 of the diameter of the homogenizer shell;
the side wall of any propylene distribution pipe is uniformly provided with jet holes in a triangular arrangement, and the outlet speed of propylene is 20-40m/s through the jet holes.
5. The acrylonitrile fluidized bed reactor as claimed in claim 1, wherein:
the air distributor comprises two air main pipes which are in cross communication at an angle of 90 degrees and air branch pipes which are communicated with the air main pipes, wherein the air branch pipes are perpendicular to the air main pipes and are distributed at intervals, and the air main pipes and the air branch pipes are positioned in the same horizontal plane; the air inlet pipe is connected with the crossing center of the two air main pipes;
the lower side wall of the air branch pipe is provided with distribution holes, the distribution holes are concentrated in an area with included angles on two sides of a vertical axis as b, and the angle b value is 20-45 degrees.
6. The acrylonitrile fluidized bed reactor as claimed in claim 1, wherein:
the ammonia/propylene distributor comprises 4 distribution main pipes which are arranged in a 90-degree crossed manner, 4 fan-shaped areas are enclosed by the distribution main pipes and the inner wall of the reactor, a plurality of distribution branch pipes are arranged on any one distribution main pipe at intervals and are vertically communicated, and the distribution branch pipes in the adjacent fan-shaped areas are respectively arranged in the vertical direction; the distribution main pipe and the distribution branch pipes are positioned in the same horizontal plane;
any one of the distribution branch pipes is of a reducing structure, and the diameter of the distribution branch pipe at the joint with the distribution main pipe is the largest, and the pipe diameter of the distribution branch pipe is smaller as the distribution branch pipe is farther away from the distribution main pipe.
7. The acrylonitrile fluidized bed reactor as claimed in claim 6, wherein:
two rows of nozzles are arranged on the lower side wall of the distribution branch pipe, the opening shape of each nozzle on the pipe wall is tapered, and the tapered angle beta is 25-35 degrees;
the nozzle is divided into the cylinder type outside the distribution pipe, and two rows of nozzles are along vertical direction symmetric distribution, and is 25 ~ 35 with the contained angle alpha of vertical direction.
8. A fluidized bed reaction process for acrylonitrile, the reaction apparatus of any one of claims 1-7, wherein:
uniformly distributed air is introduced into the lower cone part of the reactor through an air distributor, and the air is diffused and ascended to be further uniformly distributed through a sieve pore distribution plate; meanwhile, the propylene and the ammonia enter the ammonia/propylene distributor at the body part of the reactor through the homomixer to be uniformly distributed and then sprayed out to be mixed with the air uniformly distributed by the sieve pore distribution plate, wherein the ratio of the propylene, the ammonia and the air is controlled to be 1/(1.05-1.20)/(8.2-8.8).
9. The acrylonitrile fluidized bed reaction process of claim 8, wherein:
in the mixing of ammonia and propylene in the homomixer, ammonia as a mixed gas flows inside the homomixer shell and outside the propylene distribution pipe, and the flow velocity of the ammonia in the empty pipe in the homomixer shell is 5-10 m/s; the flow rate of the propylene in the propylene distribution pipe ranges from 6m/s to 15 m/s; the ammonia and the propylene flow out and are mixed in the shell, and then are further mixed uniformly by the static mixing unit;
uniformly mixing ammonia and propylene, then respectively entering an ammonia/propylene distributor through 4 distribution main pipes, flowing out of the distribution branch pipes correspondingly connected with the distribution main pipes at the same flow speed of 3-10 m/s, and spraying out of the distribution branch pipes through a nozzle at an initial speed of 10-20 m/s to enter a body part;
in the air distributor, control air enters 2 main air pipes from an air inlet pipe through the cross center of the two main air pipes and then enters the branch air pipes, flows out of distribution holes in the lower side walls of the branch air pipes at a speed of 3-6 m/s and enters the lower cone part, is diffused and rises, and is further rectified and uniformly distributed by a sieve mesh distribution plate to be mixed with ammonia/propylene sprayed by the ammonia/propylene distributor.
10. The acrylonitrile fluidized bed reaction process according to claim 8 or 9, characterized in that:
controlling the linear speed range in the reactor to be 0.5-1.2 m/s; and/or;
the pressure of the reactor is controlled to be 0.14-0.16 MPa (a); and/or;
the reaction temperature is controlled between 420 ℃ and 440 ℃.
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| CN106492712A (en) * | 2015-09-06 | 2017-03-15 | 中国石油化工股份有限公司 | Feed distributor |
| CN106955644A (en) * | 2016-01-08 | 2017-07-18 | 中国石油化工股份有限公司 | The feed distributor of the fluidized-bed reactor reacted for ammoxidation |
| CN109772234A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | Unstripped gas feed system for ammoxidation of propylene reactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172440A (en) * | 1995-02-01 | 1998-02-04 | 旭化成工业株式会社 | Fluidized-bed reactor and reaction process using the same |
| EP0761298A2 (en) * | 1995-08-24 | 1997-03-12 | Praxair Technology, Inc. | Sparger for direct oxygen injection into a reactant stream for a fluidized bed reactor |
| CN1383911A (en) * | 2001-03-21 | 2002-12-11 | 波克股份有限公司 | Structure of distributor for partial hydrocarbon oxidizing reactor in fluidized bed |
| US20100326966A1 (en) * | 2009-06-26 | 2010-12-30 | Institute Of Nuclear Energy Research Atomic Energy Council, Executive Yuan | Multi-Gas Mixer and Device for Supplying Gas Mixture to Plasma Torch |
| CN106492712A (en) * | 2015-09-06 | 2017-03-15 | 中国石油化工股份有限公司 | Feed distributor |
| CN106955644A (en) * | 2016-01-08 | 2017-07-18 | 中国石油化工股份有限公司 | The feed distributor of the fluidized-bed reactor reacted for ammoxidation |
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