CN111686668A - Preparation equipment and preparation process of catalyst for preparing acrolein through propylene oxidation - Google Patents

Preparation equipment and preparation process of catalyst for preparing acrolein through propylene oxidation Download PDF

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Publication number
CN111686668A
CN111686668A CN202010334480.0A CN202010334480A CN111686668A CN 111686668 A CN111686668 A CN 111686668A CN 202010334480 A CN202010334480 A CN 202010334480A CN 111686668 A CN111686668 A CN 111686668A
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catalyst
reactor
distributed
propylene
stirring
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王伯生
朱金明
蒋满俐
王荆
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Yixing Shensheng Catalyst Co ltd
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Yixing Shensheng Catalyst Co ltd
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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/88—Molybdenum
    • B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/8876—Arsenic, antimony or bismuth
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0236—Drying, e.g. preparing a suspension, adding a soluble salt and drying
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
    • C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
    • C07C45/34—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds
    • C07C45/35—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in propene or isobutene
    • 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
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • 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
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Catalysts (AREA)

Abstract

The invention relates to a preparation device and a preparation process of a catalyst for preparing acrolein by propylene oxidation. The catalyst is prepared by taking Mo as a reference, adding Fe, Bi, Co and other elements, carrying out coprecipitation reaction and crystallization or physical compounding by using salts or corresponding oxides of the elements, and then mixing and granulating the crystallized or compounded catalyst powder material and a binder. The geometric shape of the catalyst is mostly spherical, cylindrical or irregular. Under certain temperature conditions, the catalyst is activated by calcination to form a catalyst product.

Description

Preparation equipment and preparation process of catalyst for preparing acrolein through propylene oxidation
Technical Field
The invention relates to the technical field of production of acrolein catalysts prepared by propylene oxidation, in particular to a preparation device and a preparation process of the acrolein catalysts prepared by propylene oxidation.
Background
The catalyst is suitable for gas phase oxidation of propylene or isobutylene (tert-butyl alcohol) in the presence of air or molecular oxygen to produce acrolein or methacrolein. The raw material gas for reaction is composed of propylene or isobutylene, air or oxygen and water vapor in a certain proportion, and is carried out in a tubular fixed bed reactor filled with a catalyst. The reactor is heated by molten salt or heat conducting oil, and the acrolein or methacrolein production can be realized by tail gas circulation or a one-time system process.
The prior acrolein or methylacrolein catalyst mostly adopts static box drying or spray drying of slurry after multi-component coprecipitation reaction. Thus, the labor and the time are wasted, and the production efficiency is low. And the generated phase state of the catalyst component is incomplete, so that the catalytic performance of the catalyst is directly influenced. Secondly, the catalyst production repeatability is relatively low, and the catalyst manufacturing cost is undoubtedly increased.
Disclosure of Invention
The invention aims to provide equipment and a process for preparing an acrolein catalyst by propylene oxidation, which are used for solving the problems in the prior production of the acrolein or methacrolein catalyst in the background art. A brand-new preparation device and a preparation process of a catalyst for preparing acrolein by propylene oxidation are provided. Two reactors (A and B) are used to complete the precipitation reaction of the catalyst components and the crystallization of the precipitate. Not only improving the production efficiency of the catalyst and the product yield. And simultaneously, the production cost of the catalyst is reduced.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation device and a preparation process of a catalyst for preparing acrolein by propylene oxidation comprise a base and a catalyst component introducing pipeline, wherein a bracket is welded at the upper end of the base, and the inner wall of the bracket is welded with a reactor A, two sides of the reactor A are provided with catalyst component leading-in pipelines or feeding pipelines, the middle part of the upper end of the reactor A is provided with a stirring mechanism, a first discharge pipeline is arranged at the bottom of the lower end of the reactor A, an electromagnetic valve is distributed on the outer wall of one side of the first discharge pipeline, the other side of the first discharging pipeline is communicated with a reactor B, the bottom of the lower end of the reactor B is provided with a second discharging mechanism, and the tail end of the second discharging mechanism is distributed with a flange plate, the bottom of the lower end of the flange plate is provided with a hot air device, and the lower extreme branch of desicator is equipped with gas heater, the distribution of one side of desicator has defeated material baffle, and the other side of defeated material baffle distributes and has the material collecting box. Particularly, the device of the reactor A is adopted to not only solve the coprecipitation reaction of each component of the catalyst, but also well solve the crystallization problem of each component after precipitation through the reactor B.
Preferably, a welding integrated structure is arranged between the base and the support, and the support is vertically distributed.
Preferably, the reactor A and the reactor B form a communication structure through a first discharge pipeline, and the reactor A and the reactor B are parallel to each other.
Preferably, the dryer forms a communicating structure with the material accumulating box through the material conveying guide plate, and the material conveying guide plate is distributed in an inclined shape.
Preferably, the rabbling mechanism is including servo motor, mounting bracket, sealed dish, (mixing) shaft and stirring leaf, and servo motor's lower extreme bottom settles and have the mounting bracket, the laminating of the lower extreme inner wall of mounting bracket has sealed dish, servo motor's terminal key-type connection has the (mixing) shaft, and the lower extreme both sides distribution of (mixing) shaft has the stirring leaf.
Preferably, the stirring shaft is distributed along the vertical central axis of the reactor, and the stirring blades are distributed along two sides of the outer wall of the stirring shaft, so that the crystallization time and temperature of the mixture led into the reactor B after the precipitation reaction are well controlled.
Preferably, the catalyst performance test comprises the following process steps:
1) the catalyst performance test was carried out on a tubular fixed bed reactor.
2) And (3) heating by using molten salt.
3) The catalyst is diluted by inert balls and filled in different sections with different concentrations, and the distribution of the imported materials is controlled by the resistance drop of the catalyst bed. The airspeed is 800-1500 h-1The raw material gas consists of propylene or isobutene, air (oxygen) and water (circulating gas), and the concentration of a reactant is generally controlled to be 6.5-10 vol.%, and O is2/C=1.6 to 2.2, H2O/C=1.4 to 3.5. If a cyclic process is used, H2O/C=Can be reduced to 0.8-1.0 percent, and the circulating gas amount is 25-30 percent.
Preferably, the length of the tube type fixed bed reactor is 3.5m, and the diameter is 25.4 mm.
Preferably, the catalyst preparation comprises the following process steps:
1) 220 g of analytically pure ammonium molybdate is accurately weighed and dissolved in 400ml of purified water at 40 ℃ to obtain solution A.
2) Then 60.4 g of analytically pure cobalt nitrate, 35.7 g of analytically pure ferric nitrate and 50.3 g of analytically pure nickel nitrate are accurately weighed and dissolved in 65ml of water to obtain B1 solution, and 65.3 g of analytically pure bismuth nitrate is accurately weighed and dissolved in 60ml of water acidified by adding 15ml of nitric acid to obtain B2 solution.
3) Adding the solution A, the solution B1 and the solution B2 into the reactor A at the same time, raising the temperature to 75 ℃, and carrying out precipitation reaction under the stirring condition.
4) Then the precipitate produced in reactor A is passed into reactor B for crystallization and drying, and the obtained powder material is kneaded with 15 g of binder and extruded into particles phi 5X 5 mm. Calcining for 8 hours at 550 ℃ by adopting a muffle furnace to obtain a finished catalyst. The atomic ratio is as follows: Mo12Co2.5Ni1.0Fe0.8Bi2.8.
The performance test results of the obtained catalyst are as follows: conversion of propylene: 98.8 percent; acrolein yield: 85.5% mol; yield of acrylic acid: 8.1% mol; acetaldehyde yield: 1.1% mol; carbon oxide yield: 3.8% mol.
Compared with the prior art, the invention has the following beneficial effects:
(1) the reactor is simple and convenient to set, and the precipitation reaction, crystallization and drying are integrally completed. The activity and selectivity of the prepared catalyst exceed those of most of the catalysts at present, and particularly, the stability and the product percent of pass of the catalyst are greatly improved. The production cost of the catalyst is reduced.
(2) The catalyst is prepared by taking Mo element as a reference, adding Fe, Bi, Co and other elements, and carrying out coprecipitation reaction or physical compounding by using salts or corresponding oxides of the elements, wherein the geometric shape of the catalyst is mostly spherical, cylindrical or special-shaped. Under certain temperature conditions, the catalyst is activated by calcination to form a catalyst product.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing acrolein catalyst by propylene oxidation and a process for preparing the same according to the present invention;
FIG. 2 is a schematic diagram showing an external structure of an apparatus for preparing a catalyst for acrolein by propylene oxidation and a process for preparing the same according to the present invention;
FIG. 3 is a schematic diagram of a partially enlarged structure at A in FIG. 1 of a catalyst preparation apparatus for preparing acrolein by propylene oxidation and a preparation process thereof according to the present invention.
In the figure: 1. a base; 2. a support; 3. a, a reactor; 4. a catalyst introduction pipe; 5. a feed conduit; 6. a first discharge conduit; 7. an electromagnetic valve; 8. b, a reactor; 9. a stirring mechanism; 901. a servo motor; 902. a mounting frame; 903. sealing the disc; 904. a stirring shaft; 905. stirring blades; 10. a second discharge mechanism; 11. a flange plate; 12. a hot air device; 13. a heater; 14. a material conveying guide plate; 15. a material accumulation box.
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. 1-3, the present invention provides a technical solution: a propylene oxidation acrolein catalyst preparation equipment and its preparation technology, including the base 1, the support 2, A reactor 3, the catalyst import pipeline 4, the feed line 5, the first discharge pipeline 6, the electromagnetic valve 7, B reactor 8, the stirring mechanism 9, the servo motor 901, the mounting rack 902, the seal disc 903, the stirring shaft 904, the stirring blade 905, the second discharge mechanism 10, the flange 11, the hot air device 12, the heater 13, the material conveying guide plate 14 and the material accumulation box 15, the upper end of the base 1 is welded with the support 2, and the inner wall of the support 2 is welded with the A reactor 3, the base 1 and the support 2 are welded with an integrated structure, the support 2 is vertically distributed, the whole base 1 and the support 2 are used as the support structure of the equipment, the support structure is connected together by welding, the connection strength is high, the structure is stable, and the whole support 2 is used as the vertical fixed structure equipment of the A reactor 3 and the B reactor 8, the brackets 2 are vertically distributed, so that the limiting treatment can be effectively carried out;
catalyst component leading-in pipelines 4 and 5 are arranged at two sides of the upper end of the A reactor 3, a stirring mechanism 9 is arranged in the middle of the upper end of the A reactor 3, and the bottom of the lower end of the A reactor 3 is provided with a first discharging pipeline 6, the stirring mechanism 9 comprises a servo motor 901, a mounting frame 902, a sealing disc 903, a stirring shaft 904 and a stirring blade 905, a mounting frame 902 is arranged at the bottom of the lower end of the servo motor 901, a sealing disc 903 is attached to the inner wall of the lower end of the mounting frame 902, a stirring shaft 904 is connected with the tail end key of the servo motor 901, stirring blades 905 are distributed on two sides of the lower end of the stirring shaft 904, the stirring shaft 904 is distributed along the vertical central axis of the A reactor 3, the stirring blades 905 are distributed along two sides of the outer wall of the stirring shaft 904, when a user needs to stir the reactor a, the servo motor 901 can be turned on, the servo motor 901 drives the stirring shaft 904, and the stirring shaft 904 drives the stirring blade 905 to perform stirring operation.
The outer wall of one side of the first discharging pipeline 6 is distributed with an electromagnetic valve 7, the other side of the first discharging pipeline 6 is communicated with a B reactor 8, the A reactor 3 forms a communicating structure through the first discharging pipeline 6 and the B reactor 8, the A reactor 3 and the B reactor 8 are parallel to each other, when the catalyst is produced, A liquid obtained by synchronously dissolving quantitative molybdenum salt in quantitative pure water and B liquid obtained by dissolving corresponding salts such as quantitative Fe, Bi, Co and the like are led into the A reactor 3 for precipitation reaction, then led into the B reactor 8 for crystallization, and then the thick substance is led into the hot air device 12 for drying, so that the obtained powder material is dried
The bottom of the lower end of the reactor B8 is provided with a second discharging mechanism 10, the tail end of the second discharging mechanism 10 is distributed with a flange plate 11, the bottom of the lower end of the flange plate 11 is distributed with a hot air device 12, the lower end of the hot air device 12 is distributed with a heater 13, one side of the hot air device 12 is distributed with a material conveying guide plate 14, the other side of the material conveying guide plate 14 is distributed with a material accumulation box 15, the hot air device 12 and the material accumulation box 15 form a communicating structure through the material conveying guide plate 14, the material conveying guide plate 14 is distributed in an inclined shape, when the hot air device 12 produces catalyst products, the products can be guided into the material accumulation box 15 through the material conveying guide plate 14, the materials can be collected conveniently, and the. And adding a forming agent into the obtained powder for granulation. Activating at 250-600 ℃ to obtain a catalyst product;
the catalyst performance test comprises the following process steps:
1 catalyst performance testing was conducted on a tubular fixed bed reactor.
2, heating by using molten salt.
3 the catalyst is diluted by inert balls and filled in a plurality of sections with different concentrations, and the distribution of the imported materials is controlled by the resistance drop of the catalyst bed. The airspeed is 800-1500 h-1The raw material gas consists of propylene or isobutene, air oxygen and water circulating gas, the concentration of a reactant is generally controlled to be 6.5-10 vol.%, and O is2/C=1.6 to 2.2, H2O/C=1.4 to 3.5. If a cyclic process is used, H2O/C=Can be reduced to 0.8-1.0 percent, and the circulating gas amount is 25-30 percent.
The length of the tube of the tubular fixed bed reactor is 3.5m and the diameter is 25.4 mm.
The preparation of the catalyst comprises the following process steps:
1 accurately weighing 220 g of analytically pure ammonium molybdate, and dissolving in 400ml of purified water at 40 ℃ to obtain solution A.
2, accurately weighing 60.4 g of analytically pure cobalt nitrate, 35.7 g of analytically pure ferric nitrate and 50.3 g of analytically pure nickel nitrate, dissolving the materials in 65ml of water to obtain a B1 solution, and accurately weighing 65.3 g of analytically pure bismuth nitrate, dissolving the materials in 60ml of water acidified by adding 15ml of nitric acid to obtain a B2 solution.
3 adding the A liquid, the B1 liquid and the B2 liquid into the A reactor at the same time, raising the temperature to 75 ℃, carrying out precipitation reaction under the stirring condition, and crystallizing in the B reactor.
4 the powder obtained in the B reactor was then kneaded with 15 g of a binder and granulated by extrusion into particles phi 5X 5 mm. Calcining for 8 hours at 550 ℃ by adopting a muffle furnace to obtain a finished catalyst. The atomic ratio is as follows: Mo12Co2.5Ni1.0Fe0.8Bi2.8.
The catalyst performance test results are as follows:
conversion of propylene: 98.8 percent;
acrolein yield: 85.5% mol;
yield of acrylic acid: 8.1% mol;
acetaldehyde yield: 1.1% mol;
carbon oxide yield: 3.8% mol
The working principle of the embodiment is as follows: when the equipment and the process for preparing the acrolein catalyst by propylene oxidation are used, a certain amount of solution A in which molybdenum salt is dissolved in a certain amount of purified water and a certain amount of solution B in which corresponding salts such as Fe, Bi, Co and the like are dissolved are synchronously led into a reactor A3 for precipitation reaction, then led into a reactor B8 for crystallization, and then the thick matter is led into a hot air device 12 for drying, and the obtained powder is added with a forming agent for granulation. Activating at 250-600 ℃ to obtain a catalyst product, and simultaneously testing the performance of the catalyst;
the catalyst performance test comprises the following process steps:
1 catalyst performance testing was conducted on a tubular fixed bed reactor.
2, heating by using molten salt.
3 the catalyst is diluted by inert balls and filled in a plurality of sections with different concentrations, and the distribution of the imported materials is controlled by the resistance drop of the catalyst bed. The airspeed is 800-1500 h-1Raw gasConsists of propylene or isobutene, air oxygen and water circulating gas, and the concentration of a reactant is generally controlled to be 6.5-10 vol.%, and O2/C=1.6 to 2.2, H2O/C=1.4 to 3.5. If a cyclic process is used, H2O/C=Can be reduced to 0.8-1.0 percent, and the circulating gas amount is 25-30 percent.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.

Claims (10)

1. A preparation equipment of acrolein catalyst by propylene oxidation comprises a reactor A for catalyst component precipitation reaction and a reactor B for crystallization drying of precipitated products, a base (1) and a pipeline (4) for introducing catalyst components, and is characterized in that: the device comprises a base (1), a support (2) is welded at the upper end of the base (1), an A reactor (3) is welded at the inner wall of the support (2), a catalyst leading-in pipeline (4) is arranged on one side of the upper end of the A reactor (3), feed pipelines (5) are arranged on two sides of the upper end of the A reactor (3), a stirring mechanism (9) is arranged in the middle of the upper end of the A reactor (3), a first discharge pipeline (6) is arranged at the bottom of the lower end of the A reactor (3), an electromagnetic valve (7) is distributed on the outer wall of one side of the first discharge pipeline (6), a B reactor (8) is communicated with the other side of the first discharge pipeline (6), a second discharge mechanism (10) is arranged at the bottom of the lower end of the B reactor (8), a flange plate (11) is distributed at the tail end of the second discharge mechanism (10), a hot air device (12) is arranged at, and the lower end of the hot air device (12) is provided with a gas heater (13), one side of the hot air device (12) is distributed with a material conveying guide plate (14), and the other side of the material conveying guide plate (14) is distributed with a material accumulating box (15).
2. The apparatus for preparing a catalyst for acrolein production by oxidation of propylene according to claim 1, wherein: the components of the catalyst are fully subjected to precipitation reaction in the reactor A and crystallization drying in the reactor B, the base (1) and the support (2) are of a welding integrated structure, and the support (2) is vertically distributed.
3. The apparatus for preparing a catalyst for acrolein production by oxidation of propylene according to claim 1, wherein: the reactor A (3) enters the reactor B through a communicating structure formed between the first discharging pipeline (6) and the reactor B (8), and the reactor A (3) and the reactor B (8) are parallel to each other.
4. The apparatus for preparing a catalyst for acrolein production by oxidation of propylene according to claim 1, wherein: the hot air device (12) and the material accumulating box (15) form a communicating structure through the material conveying guide plate (14), and the material conveying guide plate (14) is distributed in an inclined shape.
5. The apparatus for preparing a catalyst for acrolein production by oxidation of propylene according to claim 1, wherein: stirring mechanism (9) are including servo motor (901), mounting bracket (902), sealed dish (903), (mixing) shaft (904) and stirring leaf (905), and the lower extreme bottom of servo motor (901) settles and have mounting bracket (902), the laminating of the lower extreme inner wall of mounting bracket (902) has sealed dish (903), the end key-type connection of servo motor (901) has (mixing) shaft (904), and the lower extreme both sides distribution of (mixing) shaft (904) has stirring leaf (905).
6. The apparatus for preparing a catalyst for acrolein production by oxidation of propylene according to claim 5, wherein: the stirring shaft (904) is distributed along the vertical central axis of the reactor A (3), and the stirring blades (905) are distributed along two sides of the outer wall of the stirring shaft (904).
7. The process according to claim 1, wherein the catalyst comprises: the catalyst performance test comprises the following process steps:
1) the catalyst performance test is carried out on a tubular fixed bed reactor;
2) heating by adopting molten salt;
3) the catalyst is diluted by adopting inert balls and filled in a plurality of sections of different concentrations, the distribution of the inlet materials is controlled by the resistance drop of a catalyst bed layer, and the airspeed is 800-1500 h-1The raw material gas consists of propylene or isobutene, air (oxygen) and water (circulating gas), and the concentration of a reactant is generally controlled to be 6.5-10 vol.%, and O is2/C=1.6 to 2.2, H2O/C=1.4 to 3.5, and if a circulation process is adopted, H2O/C=Can be reduced to 0.8-1.0 percent, and the circulating gas amount is 25-30 percent.
8. The process according to claim 7, wherein the catalyst comprises: the length of the tube type fixed bed reactor is 3.5m, and the diameter is 25.4 mm.
9. The process according to claim 1, wherein the catalyst comprises: the preparation method of the catalyst comprises the following process steps:
1) accurately weighing 220 g of analytically pure ammonium molybdate, and dissolving in 400ml of purified water at 40 ℃ to obtain solution A;
2) then accurately weighing 60.4 g of analytically pure cobalt nitrate, 35.7 g of analytically pure ferric nitrate and 50.3 g of analytically pure nickel nitrate, dissolving in 65ml of water to obtain B1 solution, and accurately weighing 65.3 g of analytically pure bismuth nitrate, dissolving in 60ml of water acidified by adding 15ml of nitric acid to obtain B2 solution;
3) adding the A liquid, B1 and B2 liquid into the A reactor at the same time, heating to 75 ℃, carrying out precipitation reaction under the condition of stirring, finishing the crystallization drying process through the B reactor, kneading the powder with 15 g of binder, extruding and granulating to form phi 5 × 5mm particles, and calcining for 8 hours at 550 ℃ by adopting a muffle furnace to obtain the finished catalyst, wherein the atomic ratio of Mo to Mo is12Co2.5Ni1.0Fe0.8Bi2.8。
10. The process according to claim 9, wherein the catalyst comprises: the performance test result of the obtained catalyst is as follows: conversion of propylene: 98.8 percent; acrolein yield: 85.5% mol; yield of acrylic acid: 8.1% mol; acetaldehyde yield: 1.1% mol; carbon oxide yield: 3.8% mol.
CN202010334480.0A 2020-04-24 2020-04-24 Preparation equipment and preparation process of catalyst for preparing acrolein through propylene oxidation Pending CN111686668A (en)

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