CN108014732B - Continuous aging reactor and aging method of aluminum hydroxide - Google Patents

Continuous aging reactor and aging method of aluminum hydroxide Download PDF

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Publication number
CN108014732B
CN108014732B CN201610973912.6A CN201610973912A CN108014732B CN 108014732 B CN108014732 B CN 108014732B CN 201610973912 A CN201610973912 A CN 201610973912A CN 108014732 B CN108014732 B CN 108014732B
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aging
reactor body
reactor
stirring shaft
reaction
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CN108014732A (en
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梁维军
赵旭
宋云华
倪黎
王晓伟
张麦奎
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China Petroleum and Chemical Corp
Sinopec Catalyst Co
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China Petroleum and Chemical Corp
Sinopec Catalyst Co
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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
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/051—Stirrers characterised by their elements, materials or mechanical properties
    • B01F27/054—Deformable stirrers, e.g. deformed by a centrifugal force applied during operation
    • B01F27/0541—Deformable stirrers, e.g. deformed by a centrifugal force applied during operation with mechanical means to alter the position of the stirring elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/21—Mixers with rotary stirring devices in fixed receptacles; Kneaders characterised by their rotating shafts
    • B01F27/2123—Shafts with both stirring means and feeding or discharging means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/86—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis co-operating with deflectors or baffles fixed to the receptacle
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/91—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
    • B01F33/71—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming working at super-atmospheric pressure, e.g. in pressurised vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/211—Measuring of the operational parameters
    • B01F35/2112—Level of material in a container or the position or shape of the upper surface of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/22—Control or regulation
    • B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
    • B01F35/2211—Amount of delivered fluid during a period
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • 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
    • B01J19/0006—Controlling or regulating processes
    • B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
    • 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
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • 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
    • B01J19/06—Solidifying liquids
    • 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
    • B01J19/1806—Stationary reactors having moving elements inside resulting in a turbulent flow of the reactants, such as in centrifugal-type reactors, or having a high Reynolds-number
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
    • 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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
    • B01J35/40—
    • B01J35/615—
    • B01J35/638—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F2035/99—Heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/2204—Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00099—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor the reactor being immersed in the heat exchange medium
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00599—Solution-phase processes
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/0077—Baffles attached to the reactor wall inclined

Abstract

The invention relates to the field of catalysts, and discloses a continuous aging reactor and an aging method of aluminum hydroxide. The continuous aging reactor provided by the invention comprises a reactor body, a feed inlet (3) arranged at the upper part of the reactor body and a discharge outlet (10) arranged at the lower part of the reactor body, wherein a separation plate (14) is arranged on the inner wall of the reactor body, and the separation plate (14) separates the reactor body into more than 2 aging chambers; the middle part of the reactor body is provided with a stirring shaft (12), and paddles (13) are respectively arranged on the stirring shaft (12) corresponding to each aging chamber. The continuous aging reactor and the aging method of the aluminum hydroxide can realize continuous aging of the aluminum hydroxide slurry and prepare the high-purity pseudo-boehmite.

Description

Continuous aging reactor and aging method of aluminum hydroxide
Technical Field
The invention relates to the field of catalysts, in particular to a continuous aging reactor and an aging method of aluminum hydroxide.
Background
Pseudoboehmite is aluminum hydroxide with fine particles, incomplete crystallization and thin fold sheet layers, the water-containing state of the pseudoboehmite is thixotropic gel, the pseudoboehmite has the characteristics of high specific surface area, large pore volume and the like, and the pseudoboehmite with high crystal phase purity is a catalyst carrier with excellent performance. The pseudo-boehmite is used as a hydrogenation catalyst carrier, so that the activity of the catalyst can be improved, and the strength of the catalyst can be improved. The performance of pseudo-boehmite is directly related to the physicochemical properties of specific surface area, pore structure, grain size and the like, so that the physicochemical properties of the pseudo-boehmite need to be adjusted in the preparation process of the pseudo-boehmite so as to meet the application requirements. One of the most commonly used means for adjusting the physicochemical properties is to age the aluminum hydroxide slurry, thereby changing its physicochemical properties such as specific surface area, pore structure and grain size.
At present, the main methods for preparing pseudo-boehmite are an aluminum choline hydrolysis method, an aluminum ammonium sulfate pyrolysis method, an aluminum ammonium carbonate pyrolysis method and an aluminum alkoxide method. Besides the aluminum alkoxide method, the purity of the pseudo-boehmite prepared by other methods is difficult to ensure, and the requirement of the catalyst carrier on the purity of the pseudo-boehmite cannot be met. The method for preparing the pseudo-boehmite by the aluminum alkoxide method comprises the following steps of: alcohol reacts with aluminum metal at a certain temperature to generate aluminum alkoxide, the aluminum alkoxide is hydrolyzed to generate alcohol and aluminum hydroxide slurry, and then the aluminum alkoxide is aged to prepare pseudo-boehmite with different physical and chemical properties.
Aiming at the aging process of hydroxide slurry, a kettle-type aging reactor is generally adopted in industry, hydroxide materials are added into the kettle-type aging reactor, and aging treatment is carried out by maintaining certain temperature and pressure, and the processing mode has the defects that the aging process is operated in a batch mode, the production efficiency is lower, meanwhile, due to batch processing, the aging condition of each batch is difficult to keep completely uniform, and the fluctuation of physical properties of products is larger. There is no report on continuous aging of aluminum hydroxide slurry.
Disclosure of Invention
The invention aims to provide a continuous ageing reactor which can realize continuous ageing of aluminum hydroxide slurry and can be used for preparing high-purity pseudo-boehmite.
In order to achieve the above object, a first aspect of the present invention provides a continuous aging reactor, which comprises a reactor body, a feed inlet provided at an upper portion of the reactor body, and a discharge outlet provided at a lower portion of the reactor body, wherein a partition plate is provided on an inner wall of the reactor body, and the partition plate partitions the reactor body into more than 2 aging chambers; the middle part of the reactor body is provided with a stirring shaft, and paddles are respectively arranged on the stirring shaft corresponding to each aging chamber.
In a second aspect of the present invention, there is provided a method for aging aluminum hydroxide, which is carried out in the above-mentioned continuous aging reactor, wherein an aluminum hydroxide slurry is fed into the continuous aging reactor from the feed port, and the aluminum hydroxide slurry is sequentially passed through each aging chamber under stirring by a stirring shaft and discharged from the discharge port, wherein the aging reaction is carried out at a reaction temperature of 25 to 360 ℃, a reaction pressure of 0 to 20MPa, and a reaction time of 0.1 to 72 hours.
Through the technical scheme, the continuous aging reactor and the aging method provided by the invention are designed based on the plug flow model or the plug flow model, an effective aging space is provided for the aging reaction of materials, the aging reaction is continuously carried out, the production efficiency is high, the aging condition can be maintained to be uniform in the aging process, the stability of the product property is good, and the production cost of hydroxide products can be greatly reduced. The continuous aging reactor provided by the invention has the advantages of simple and compact structure and low manufacturing cost.
In addition, the upper end and the lower end of the stirring shaft are respectively provided with a guide sewage disposal device, so that pollutants are prevented from entering an aging system, and the purity of an aging product is ensured.
Furthermore, the invention can accurately control the physicochemical properties of the finally obtained pseudo-boehmite, such as the specific surface area, the pore volume and the like by regulating and controlling the conditions of the aging reaction.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the description serve to explain, without limitation, the invention. In the drawings:
FIG. 1 is a block diagram of a continuous aging reactor according to a preferred embodiment of the present invention.
Description of the reference numerals
1. Transmission part 2, safety valve interface
3. Feed inlet 4, jacket heat-conducting medium inlet
5. Spare feeding port 6, jacket temperature measuring port
7. Jacket 8, jacket heat-conducting medium outlet
9. Mixing shaft blow-down valve 10 and discharge port
11. Spare outlet 12 of jacket and stirring shaft
13. Blade 14, separator plate
15. Liquid level meter interface 16, blow-down tank
17. Emptying port
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, unless otherwise indicated, terms of orientation such as "upper and lower" are used to refer generally to the upper and lower parts of the drawings.
As shown in fig. 1, the continuous aging reactor of the present invention comprises a reactor body, a feed inlet 3 arranged at the upper part of the reactor body, and a discharge outlet 10 arranged at the lower part of the reactor body; a separation plate 14 is arranged on the inner wall of the reactor body, and the separation plate 14 separates the reactor body into more than 2 aging chambers; the middle part of the reactor body is provided with a stirring shaft 12, and blades 13 are respectively arranged on the stirring shaft 12 corresponding to each aging chamber.
According to the present invention, the structure of the reactor body is not particularly limited, and may be appropriately selected according to the reaction requirement, and may be specifically one of a reaction tower, a reaction kettle, and a reaction tube. Among them, a reaction column is preferable.
In the present invention, the feed port 3 is provided at the upper portion of the reactor body, and the discharge port 10 is provided at the lower portion of the reactor body. In the continuous ageing reaction process, materials enter the reactor body through the feed inlet 3, and under the condition that the stirring shaft 12 drives the paddles to rotate, the materials are continuously and uniformly mixed and sequentially pass through each ageing chamber from top to bottom, and finally the aged materials are obtained through the discharge outlet 10.
In the present invention, the material is not particularly limited, and in order to adjust the aging reaction conditions and ensure a sufficient aging time, the material is preferably a material having poor fluidity, such as a slurry material, a gel material, or the like. Examples of the material include slurries of hydroxides such as aluminum hydroxide, magnesium hydroxide, and magnesium aluminum hydrotalcite.
According to the present invention, the structure of the partition plate 14 is not particularly limited as long as the effect of reducing the material lowering speed can be achieved. The partition plate 14 may be an annular structure fixed on the inner wall of the reactor body, or may be an annular or near-annular structure formed by splicing a plurality of partition plates 14. In the case where a plurality of the partition plates 14 are joined together, the shape of each partition plate is not particularly limited, and a slit may be provided between the partition plates 14.
The middle of the annular structure is provided with a shaft hole, and the stirring shaft is arranged in the shaft hole. The size of the shaft hole is not particularly limited and may be specifically selected according to the desired material falling speed, for example, the diameter of the shaft hole may be 20 to 50%, preferably 20 to 40%, more preferably 30 to 40% of the inner diameter of the reactor body.
The partition plate 14 may also have openings for lowering the material in order to adjust the material lowering speed. The openings and the gaps between the plurality of divider plates 14 increase the rate of material descent. The size and dimension of the gap and the opening can be specifically selected according to the aging reaction conditions such as the solid content of the material. Preferably, the total area of the slits and openings is 1-30%, preferably 2-15%, more preferably 4-7% of the area of the divider plate. The gaps and the open holes are preferably distributed symmetrically relative to the center of the stirring shaft, can be uniformly distributed in the axial direction, and can be closer to the center or the periphery. More preferably, the divider plate 14 may have more slits and openings near its center.
Further preferably, in order to uniformly mix the materials during the descending process, the partition plate 14 may be provided in a tapered structure inclined downward from the inner wall, and the materials may be sufficiently mixed by the paddles 13 by descending the materials at a position close to the paddles 13. The inclination angle of the partition plate 14 with respect to the horizontal direction is not particularly limited, and may be, for example, 0 to 30 °, preferably 0.5 to 15 °, more preferably 1 to 10 °
In the present invention, the size of the aging chamber formed by partitioning the reactor body by the partition plate 14 is not particularly limited, and may be the same or different, and it is preferable to make the aging space of each aging chamber the same. In the invention, the aging space refers to a space in the aging chamber for mixing materials to complete an aging reaction.
According to the invention, a transmission part 1 is arranged at the top of the reactor body, and the transmission part 1 is used for driving the stirring shaft 12 to rotate. The transmission member 1 is not particularly limited, and may be capable of rotating the stirring shaft 12. In particular, the transmission component may be a magnetic stirrer. Preferably, the transmission member 1 is sealed in order to ensure the reaction pressure inside the reactor body. The sealing method is not particularly limited, and a transmission seal or a mechanical seal is preferable in order to ensure a good sealing effect. The seal can be specifically selected according to the needs, and the sealing modes can also be combined for use. For example, the sealing means may be a mechanical seal.
According to the invention, the stirring shaft 12 extends through the reactor body. When the stirring shaft 12 rotates, the blades 13 in each aging chamber are driven to rotate simultaneously, so that the materials are uniformly mixed and gradually move downwards. By providing an integral stirring shaft 12, the operation and maintenance process of the reactor can be simplified.
According to the present invention, the structure and number of the blades 13 are not particularly limited, and mixing of materials can be achieved. The blades 13 may be one or more of a pitched blade turbine blade, a hinged blade, an anchor blade, and a frame blade. More preferably, the blade 13 is a pitched blade turbine blade. Preferably, in order to ensure uniform mixing of the materials, the materials are aged at a uniform temperature, and the number of the blades 13 provided for each aging chamber is 2-8, preferably 4-6. In the present invention, the number of the blades 13 in each aging chamber may be one or more, and in particular, may be reasonably arranged according to the volume of the aging space, generally 1 to 6 groups, and preferably 1 to 2 groups.
According to the invention, the rotational speed of the blade 13 may be chosen according to the specific ageing reaction and the conditions of the material. In order to ensure uniform mixing of the materials, the rotation speed of the blade 13 is preferably 50 rpm or more, preferably 60 rpm or more, more preferably 80 rpm or more, and still more preferably 100 rpm or more. In the aging reaction requiring crystallization, the rotation speed of the blade 13 is preferably 350 rpm or less, more preferably 300 rpm or less, still more preferably 200 rpm or less, still more preferably 150 rpm or less, so as not to damage the formation process of crystal grains of the material
According to the invention, the position of the blade 13 on the stirring shaft 12 can be specifically set according to the needs, so that the uniform mixing of materials can be ensured. Preferably, the position of the paddle 13 on the stirring shaft 12 may be adjusted, so that the mixing effect of the paddle 13 may be controlled more conveniently as required, and the mixing efficiency may be further improved.
According to the present invention, in order to prevent impurities in the stirring shaft 12 from entering the reactor body, the upper and lower ends of the stirring shaft 12 are respectively provided with guide sewage outlets, which are respectively connected with the sewage tank 16 and the stirring shaft sewage valve 9. By providing the guide drain, worn scrap iron in the stirring shaft 12 can be discharged outside the aging reactor, so that the purity of the materials of the aging reaction is ensured.
According to the invention, the side wall of the reactor body is coated with a jacket 7, and the jacket 7 is filled with a heat conducting medium. According to the invention, the upper part of the jacket 7 is provided with a jacket heat conducting medium inlet 4, and the lower part of the jacket 7 is provided with a jacket heat conducting medium outlet 8. The jacket heat-conducting medium inlet 4 is used for adding the heat-conducting medium, and the jacket heat-conducting outlet 8 is used for discharging the heat-conducting medium. In addition, the lower part of the jacket 7 may be provided with a jacket spare outlet 11, as required. The jacket 7 serves for heating and insulating the reactor body. The heat-conducting medium inside the jacket 7 may be specifically selected according to the heating temperature, and the heat-conducting medium in the jacket 7 may be a heat-conducting medium having a certain temperature, such as steam, or may be a heat-conducting medium that can be heated inside the jacket, such as heat-conducting oil. Specifically, an electric heating rod for heating the heat-conducting medium may be further provided inside the jacket 7. By means of the arrangement of the jacket 7, a certain aging temperature can be kept in the reactor body, and the aging reaction is guaranteed.
According to the invention, the jacket 7 is provided with a jacket temperature measuring port 6, and the jacket temperature measuring port 6 is used for measuring the temperature of the heat conducting medium inside the jacket 7 through a temperature measuring device.
According to the present invention, the number of the aging chambers is 2 to 10, preferably 2 to 8, more preferably 3 to 6, in order to secure a reaction time for which the aging reaction is continued.
According to the invention, the reactor body is preferably a pressure-resistant reactor to meet the requirements of aging reaction under certain pressure. The pressure in the reactor body can be generated by liquid phase evaporation in materials, and can be pressurized as required. The pressurization may be performed by filling a gas, and the gas is not particularly limited, and is preferably an inert gas. The inert gas may be helium, argon, nitrogen or other common inert gases.
According to the invention, the top of the reactor body is provided with a safety valve interface 2, said safety valve interface 2 being used for connecting a pressure safety valve. By providing the pressure relief valve, the aging reaction can be safely performed at a higher pressure.
According to the invention, the top of the reactor body is provided with a vent 17. The vent 17 is used to regulate the pressure inside the reactor body.
According to the invention, the side wall of the reactor body is provided with a level gauge interface 15. The liquid level meter is used for detecting the material liquid level inside the reactor body in the continuous aging reaction. Specifically, the liquid level meter can be a tuning fork vibration type liquid level meter, a magnetic levitation type liquid level meter, a differential pressure liquid level meter, an ultrasonic liquid level meter and the like. The arrangement of the level gauge interface 15 may be selected according to the specific level gauge used.
In the present invention, a spare feed port 5 is provided in the middle of the reactor body. The spare feed inlet 5 is used as a material inlet channel, and can be selected according to the requirement, for example, when a shorter ageing time is required.
The aging method of the aluminum hydroxide provided by the invention is carried out in the continuous aging reactor, wherein the aluminum hydroxide slurry enters the continuous aging reactor from the feed inlet 3, and is sequentially led through each aging chamber and discharged from the discharge outlet 10 under the stirring of the stirring shaft, wherein the reaction temperature of the aging reaction is 25-360 ℃, the reaction pressure is 0-20MPa, and the reaction time is 0.1-72 hours.
Preferably, the aging reaction is carried out at a reaction temperature of 60-280 ℃, a reaction pressure of 0.5-10MPa and a reaction time of 0.5-24 hours. The reaction time refers to the time from the inlet 3 to the outlet 10.
In the present invention, the reaction temperature of the aging reaction is controlled by the jacket 7. The reaction pressure can be generated by liquid phase evaporation in the aluminum hydroxide slurry, and can be pressurized according to the requirement. The pressurization may be performed by filling a gas, and the gas is not particularly limited, and is preferably an inert gas. The inert gas may be helium, argon, nitrogen or other common inert gases.
In the present invention, the reaction pressure is a pressure in gauge.
In the present invention, the aging reaction is continuously carried out, and the feed rate of the aluminum hydroxide slurry is not particularly limited, but is preferably 50 to 2000 g/min, more preferably 50 to 1000 g/min, in order to ensure that the aging of aluminum hydroxide proceeds sufficiently. During the reaction, the liquid level in the continuous aging reactor is monitored by a liquid level meter, and the feeding speed can be properly regulated according to the requirement.
The aluminum hydroxide slurry is not particularly limited, and may be, for example, aluminum hydroxide slurry obtained by hydrolysis of aluminum alkoxide during preparation of pseudo-boehmite by an aluminum alkoxide method. The solid content of the aluminum hydroxide slurry is not particularly limited, and in order to ensure that the aging reaction proceeds sufficiently, the solid content of the aluminum hydroxide slurry is preferably 5 to 30% by weight. The aluminum hydroxide slurry may contain water, alcohol, acid, etc.
According to the present invention, the rotation speed of the stirring shaft 12 is not particularly limited, and may be specifically selected as needed. In particular, the rotational speed of the stirring shaft 12 may be used to adjust the size of the resulting pseudo-boehmite grains. In order to ensure uniform mixing of the materials, the rotation speed of the blade 13 is preferably 50 rpm or more, preferably 60 rpm or more, more preferably 80 rpm or more, and still more preferably 100 rpm or more. In order not to damage the crystal grain formation process, the rotation speed of the blade 13 is preferably 350 rpm or less, more preferably 300 rpm or less, still more preferably 200 rpm or less, and still more preferably 150 rpm or less.
By the aging method of aluminum hydroxide provided by the invention, the aging process of aluminum hydroxide is continuously carried out. By arranging the sewage discharging device on the upper part and the lower part of the stirring shaft, the purity of the obtained pseudo-boehmite can be ensured. By controlling the conditions of the aging reaction, a specific surface area of 50-400cm can be obtained 2 Per g, pore volume of 0.3-2.0mL/g, the grain size of the pseudo-boehmite is 1-50nm.
The present invention will be described in detail by examples.
Example 1
This example was performed using the continuous aging reactor shown in fig. 1.
As shown in fig. 1, the continuous aging reactor comprises a reaction tower, a feed inlet 3 arranged at the upper part of the reaction tower and a discharge outlet 10 arranged at the lower part of the reaction tower; a separation plate 14 is arranged on the inner wall of the reaction tower, and the separation plate 14 separates the reaction tower into 6 aging chambers; the middle part of the reaction tower is provided with a stirring shaft 12, and blades 13 are respectively arranged on the stirring shaft 12 corresponding to each aging chamber.
The partition plate 14 has a taper structure with a shaft hole in the middle and inclined downward from the inner wall, the angle of downward inclination of the partition plate 14 relative to the horizontal direction is 3 °, the diameter of the shaft hole is 50% of the inner diameter of the reaction tower, and no opening is provided on the partition plate 14.
The top of the reaction tower is provided with a transmission part 1, and the transmission part 1 is a mechanical seal magnetic stirrer and is used for driving the stirring shaft 12 to rotate.
The stirring shaft 12 penetrates through the reaction tower, and a group of 6-leaf oblique-leaf turbine blades 13 are arranged on the stirring shaft corresponding to each aging chamber. The upper end and the lower end of the stirring shaft 12 are respectively provided with a guide drain outlet, and the guide drain outlets are respectively connected with the drain tank 16 and the stirring shaft drain valve 9.
According to the invention, the side wall of the reaction tower is coated with a jacket 7, and the jacket 7 is filled with heat conduction oil and an electric heating rod for heating the heat conduction oil. The jacket 7 is provided with a jacket temperature measuring port 6, and a thermometer is arranged in the jacket temperature measuring port 6, so that the temperature of the heat conducting medium in the jacket 7 is measured. The upper part of the jacket 7 is provided with a jacket heat-conducting medium inlet 4, and the lower part of the jacket 7 is provided with a jacket heat-conducting medium outlet 8. The jacket heat-conducting medium inlet 4 is used for adding the heat-conducting medium, and the jacket heat-conducting outlet 8 is used for discharging the heat-conducting medium. The lower part of the jacket 7 may also be provided with a jacket reserve outlet 11.
The top of the reaction tower is provided with a safety valve connector 2, and the safety valve connector 2 is connected with a pressure safety valve. The top of the reaction tower is also provided with a vent 17. Two liquid level meter interfaces 15 are arranged on the side wall of the reaction tower, the liquid level meter interfaces 15 are connected with a differential pressure liquid level meter, and the slurry amount in the continuous reaction tower is monitored through the liquid level meter. In this embodiment, a spare feed inlet 5 is also provided in the middle of the reaction tower.
In the aging process of aluminum hydroxide, aluminum hydroxide slurry with the solid content of 10 weight percent enters the continuous aging reactor from the feed inlet 3, the feed rate is 500 g/min, the aluminum hydroxide slurry is discharged from the discharge outlet 10 after reaction, in the process, the aluminum hydroxide slurry is continuously and uniformly mixed and sequentially passes through each aging chamber from top to bottom, and finally aged materials are obtained through the discharge outlet. In addition, the reaction conditions were: the reaction temperature was 90 ℃, the reaction pressure was 1MPa, the reaction time was 2 hours, and the rotational speed of the stirring shaft 12 was 100 rpm.
After the aging reaction, a specific surface area of 203cm was obtained 2 Per g, pore volume of 0.7mL/g, grain size of 5 nm.
Example 2
The aging reaction of aluminum hydroxide was carried out according to the method of example 1, except that the reaction temperature was 120 deg.c, the reaction pressure was 2MPa, the reaction time was 4 hours, and the rotation speed of the stirring shaft 12 was 120 rpm.
After the aging reaction is completed, the specific surface area of 164cm is obtained 2 Per g, pore volume of 1.1mL/g, grain size of 8 nm.
As can be seen from the above examples, the continuous aging reactor and the aging method of aluminum hydroxide provided by the invention can be used for the aging reaction of aluminum hydroxide slurry, and the finally prepared pseudo-boehmite is suitable for being used as a catalyst carrier. And the worn scrap iron in the stirring shaft is discharged through the guide drain outlet, so that the purity of the pseudo-boehmite is improved.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.

Claims (15)

1. A method for aging aluminum hydroxide, characterized in that the method is carried out in a continuous aging reactor, the reactor comprises a reactor body, a feed inlet (3) arranged at the upper part of the reactor body and a discharge outlet (10) arranged at the lower part of the reactor body,
a separation plate (14) is arranged on the inner wall of the reactor body, and the separation plate (14) separates the reactor body into more than 2 aging chambers;
a stirring shaft (12) is arranged in the middle of the reactor body, paddles (13) are respectively arranged on the stirring shaft (12) corresponding to each aging chamber,
the separation plate (14) is of a cone structure which is inclined downwards from the inner wall, and the inclination angle of the separation plate (14) relative to the horizontal direction is 1-10 degrees;
the upper end and the lower end of the stirring shaft (12) are respectively provided with a guide sewage outlet;
a standby feed inlet (5) is arranged in the middle of the reactor body;
the aluminum hydroxide slurry enters the continuous aging reactor from the feed inlet (3), and sequentially passes through all aging chambers and is discharged from the discharge outlet (10) under the stirring of a stirring shaft, wherein the reaction temperature of the aging reaction is 60-280 ℃, the reaction pressure is 0.5-10MPa, and the reaction time is 0.5-24 hours;
the rotating speed of the blade (13) is 50-350 rpm.
2. The aging method as claimed in claim 1, wherein the rotation speed of the stirring shaft (12) is 50-350 revolutions per minute.
3. The aging process according to claim 1 or 2, wherein the solid content of the aluminium hydroxide slurry is 5-30 wt%.
4. The aging method as claimed in claim 1, wherein the partition plate (14) is of an annular structure, or a plurality of partition plates (14) are spliced to form an annular structure with a shaft hole in the middle.
5. The aging method according to claim 4, wherein the diameter of the shaft hole is 20 to 50% of the inner diameter of the reactor body.
6. The aging method as claimed in claim 1, wherein said partition plate (14) has an opening therein.
7. The aging process as claimed in claim 1, wherein the stirring shaft (12) extends through the reactor body.
8. Ageing method according to claim 7, wherein the top of the reactor body is provided with a transmission member (1), the transmission member (1) being adapted to drive the stirring shaft (12) in rotation.
9. The aging method according to claim 1, wherein the number of said paddles (13) provided for each aging chamber is 2-8 leaves.
10. The aging method according to claim 9, wherein said blade (13) is a pitched blade turbine blade.
11. The aging method as claimed in claim 9, wherein the position of the blade (13) on the stirring shaft (12) is adjustable.
12. The aging process as claimed in claim 1, wherein the reactor body side wall is jacketed (7).
13. Aging method according to claim 12, wherein the jacket (7) is filled with a heat conducting medium.
14. The aging method according to claim 1, wherein the number of the aging chambers is 2 to 10.
15. The aging method according to claim 1, wherein the reactor body is one of a reaction tower, a reaction kettle, or a reaction tube.
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Publication number Priority date Publication date Assignee Title
CN112694108A (en) * 2019-10-23 2021-04-23 中国石油化工股份有限公司 Method for continuously preparing aluminum sol and aluminum sol prepared by method
CN117258743B (en) * 2023-11-17 2024-03-19 山东天力科技工程有限公司 Para-aramid continuous polymerization system and method

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1250746A (en) * 1998-10-13 2000-04-19 中国石油化工集团公司 Process for preparing artificial diasporite and gamma-alumina
CN1398787A (en) * 2002-05-31 2003-02-26 中国石油化工集团公司 Prepn of gamma-alumina
CN1694916A (en) * 2002-09-23 2005-11-09 通用电气公司 Continuous manufacture of silicone copolymers via multi-stage blade-mixed plug flow tubular reactor
CN201410377Y (en) * 2008-12-04 2010-02-24 柳州市柳化集团大力透明质酸有限公司 Agitating shaft Sealing device for enamel depositing tank
CN104445309A (en) * 2013-09-17 2015-03-25 中国石油化工股份有限公司 High-purity aluminium oxide and preparation method thereof
CN104907031A (en) * 2015-05-14 2015-09-16 徐以撒 Low-backmixing middle-speed reactor being capable of continuous feeding and operation method therefor
CN205095662U (en) * 2015-05-28 2016-03-23 湖北绿色家园精细化工股份有限公司 Continuous solid body dissolving device
CN205127945U (en) * 2015-10-19 2016-04-06 赛鼎工程有限公司 Agitation reactor with porous stratified sheet
CN105922444A (en) * 2016-06-27 2016-09-07 顾宏谦 Layering stirrer
CN206103907U (en) * 2016-10-28 2017-04-19 中国石油化工股份有限公司 Continuous ageing reactor

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG11201610190WA (en) * 2014-06-16 2017-01-27 Bayer Ag Reaction chamber for a chemical reactor, and chemical reactor constructed therefrom

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1250746A (en) * 1998-10-13 2000-04-19 中国石油化工集团公司 Process for preparing artificial diasporite and gamma-alumina
CN1398787A (en) * 2002-05-31 2003-02-26 中国石油化工集团公司 Prepn of gamma-alumina
CN1694916A (en) * 2002-09-23 2005-11-09 通用电气公司 Continuous manufacture of silicone copolymers via multi-stage blade-mixed plug flow tubular reactor
CN201410377Y (en) * 2008-12-04 2010-02-24 柳州市柳化集团大力透明质酸有限公司 Agitating shaft Sealing device for enamel depositing tank
CN104445309A (en) * 2013-09-17 2015-03-25 中国石油化工股份有限公司 High-purity aluminium oxide and preparation method thereof
CN104907031A (en) * 2015-05-14 2015-09-16 徐以撒 Low-backmixing middle-speed reactor being capable of continuous feeding and operation method therefor
CN205095662U (en) * 2015-05-28 2016-03-23 湖北绿色家园精细化工股份有限公司 Continuous solid body dissolving device
CN205127945U (en) * 2015-10-19 2016-04-06 赛鼎工程有限公司 Agitation reactor with porous stratified sheet
CN105922444A (en) * 2016-06-27 2016-09-07 顾宏谦 Layering stirrer
CN206103907U (en) * 2016-10-28 2017-04-19 中国石油化工股份有限公司 Continuous ageing reactor

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
成大先等.《机械设计图册 第4卷 系统和整机的结构与组合》.北京：化学工业出版社,2000,第899-900页. *
拟薄水铝石孔结构调控的研究进展;张哲;白立光;沈冲;赵晓东;;化学推进剂与高分子材料(04);全文 *
拟薄水铝石胶溶性能的影响因素;胡涛;张君屹;;石化技术与应用(01);全文 *
杨玉旺 ; 戴清 ; 许岩 ; 刘敬利 ; 于海斌 ; 郭郢 ; 费家明 ; .老化条件对氢氧化铝性质的影响.无机盐工业.2010,(第11期),全文. *
老化条件对氢氧化铝性质的影响;杨玉旺;戴清;许岩;刘敬利;于海斌;郭郢;费家明;;无机盐工业(11);全文 *
谭蔚等.《化工设备设计基础 第3版》.天津：天津大学出版社,2014,第214-215页. *
邹仁鋘等.《基本有机化工反应工程》.北京：化学工业出版社,1981,第59页. *

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