CN108014732A - A kind of aging method of continuous ageing reactor and aluminium hydroxide - Google Patents
A kind of aging method of continuous ageing reactor and aluminium hydroxide Download PDFInfo
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- CN108014732A CN108014732A CN201610973912.6A CN201610973912A CN108014732A CN 108014732 A CN108014732 A CN 108014732A CN 201610973912 A CN201610973912 A CN 201610973912A CN 108014732 A CN108014732 A CN 108014732A
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- reactor
- aging
- reactor body
- reaction
- agitating shaft
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- 230000032683 aging Effects 0.000 title claims abstract description 113
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 title claims abstract description 37
- 229910021502 aluminium hydroxide Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims description 73
- 239000000463 material Substances 0.000 claims description 38
- 230000005540 biological transmission Effects 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 8
- 239000010865 sewage Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 abstract description 8
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 abstract description 2
- 229910001593 boehmite Inorganic materials 0.000 description 18
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 18
- 239000007788 liquid Substances 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- 239000004411 aluminium Substances 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 238000002156 mixing Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000011261 inert gas Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- -1 aluminum alkoxide Chemical class 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- IOGARICUVYSYGI-UHFFFAOYSA-K azanium (4-oxo-1,3,2-dioxalumetan-2-yl) carbonate Chemical compound [NH4+].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O IOGARICUVYSYGI-UHFFFAOYSA-K 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004643 material aging Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
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- 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
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
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- 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
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- 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
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- 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
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- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J35/615—100-500 m2/g
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/638—Pore volume more than 1.0 ml/g
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- 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
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- B01F2035/99—Heating
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- 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
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- B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to catalyst field, discloses a kind of aging method of continuous ageing reactor and aluminium hydroxide.Continuous ageing reactor provided by the invention includes reactor body, the feed inlet (3) for being arranged at the reactor body top and the discharge port (10) for being arranged at the reactor body lower part, demarcation strip (14) is provided with the reactor body inner wall, the reactor body is divided into more than 2 aging chambers by the demarcation strip (14);Agitating shaft (12) is provided with the middle part of the reactor body, corresponding to each aging chamber on the agitating shaft (12) is respectively arranged with blade (13).Pass through continuous ageing reactor provided by the invention and the aging method of aluminium hydroxide, it is possible to achieve the continuous ageing of aluminium hydroxide slurry, prepares high purity pseudoboehmite.
Description
Technical field
The present invention relates to catalyst field, and in particular, to a kind of aging side of continuous ageing reactor and aluminium hydroxide
Method.
Background technology
Boehmite is that a kind of particle is tiny, crystallization is imperfect, has the aluminium hydroxide of thin fold lamella, its is aqueous
State is thixotropy gel, has the characteristics that specific surface area height, large pore volume, the high boehmite of crystalline phase purity is that a kind of performance is excellent
Good catalyst carrier.Boehmite can not only improve the activity of catalyst, but also can carry as catalyst carrier for hydrgenating
The intensity of high catalyst.The direct phases of physico-chemical property such as the performance of boehmite and its specific surface area, pore structure, crystallite dimension
Close, therefore, it is necessary to its physico-chemical property be adjusted, to reach application demand in the preparation process of boehmite.Wherein
A kind of most often applied means for adjusting physico-chemical property are to carry out burin-in process to aluminium hydroxide slurry, so that changing it compares surface
The physico-chemical properties such as product, pore structure and crystallite dimension.
At present, the main method of boehmite is prepared by choline aluminium Hydrolyze method, alum pyrolysismethod, aluminium carbonate ammonium
Pyrolysismethod and aluminium alcoholates method.And in addition to aluminium alcoholates method, the boehmite of other methods preparation, purity is difficult to be guaranteed, Wu Faman
Requirement of the sufficient catalyst carrier to boehmite purity.The step of aluminium alcoholates method prepares boehmite be:First by alcohol and metal
Aluminium reacts generation aluminum alkoxide at a certain temperature, and aluminum alkoxide hydrolyzes generation alcohol and aluminium hydroxide slurry, passes through again afterwards again
Different physico-chemical property boehmites are made in aging process.
For hydroxide slurry ageing process, industrial generally use autoclave aging reaction device, by hydroxide material
It is added in autoclave aging device, maintains certain temperature, pressure to carry out burin-in process, the shortcomings that this processing mode is aging
Process is intermittent operation, and production efficiency is relatively low, simultaneously because batch is handled, the aging condition of every batch of is difficult to keep complete
It is homogeneous, cause the physical property of product fluctuation larger.There is presently no the relevant report of aluminium hydroxide slurry continuous ageing.
The content of the invention
The object of the present invention is to provide a kind of continuous ageing reactor, which can realize the continuous of aluminium hydroxide slurry
Aging, can be used for preparing high purity pseudoboehmite.
To achieve these goals, the first aspect of the invention is to provide a kind of continuous ageing reactor, the reactor
Including reactor body, it is arranged at the feed inlet on the reactor body top and is arranged at going out for the reactor body lower part
Material mouth, is provided with demarcation strip on the reactor body inner wall, the reactor body is divided into more than 2 by the demarcation strip
Aging chamber;Agitating shaft is provided with the middle part of the reactor body, each aging chamber is corresponded on the agitating shaft and is respectively arranged with paddle
Leaf.
The second aspect of the invention is to provide a kind of aging method of aluminium hydroxide, and this method is anti-in above-mentioned continuous ageing
Answer in device and carry out, wherein, aluminium hydroxide slurry enters the continuous ageing reactor from the feed inlet, in the stirring of agitating shaft
Under, aluminium hydroxide slurry passes sequentially through each aging chamber, and is discharged from the discharge port, wherein, the reaction temperature of the aging reaction
Spend for 25-360 DEG C, reaction pressure 0-20MPa, when the reaction time is 0.1-72 small.
Through the above technical solutions, continuous ageing reactor provided by the invention and aging method be based on plug flow model or
Plug flow model designs, and provides effective aging space for material aging reaction, is carried out continuously aging reaction, production
It is efficient, it is able to maintain that aging condition is homogeneous in ageing process, the stability of product characteristics is good, can substantially reduce hydroxide produce
The production cost of product.Also, continuous ageing structure of reactor provided by the invention is simple, compact, manufacture cost is low.
In addition, the upper and lower ends in the present invention in agitating shaft are equipped with guiding blowdown apparatus, prevent pollutant from entering aging
System, ensures the purity of ageing prod.
Further, the condition of the invention by regulating and controlling aging reaction, can accurately control the thin water aluminium of the plan finally obtained
The physico-chemical property such as the specific surface area of stone and pore volume.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Attached drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is a kind of structure chart of the continuous ageing reactor of preferred embodiment of the present invention.
Description of reference numerals
1st, transmission parts 2, relief valve connection
3rd, feed inlet 4, chuck heat-conducting medium import
5th, spare feed inlet 6, chuck temperature-measuring port
7th, chuck 8, the outlet of chuck heat-conducting medium
9th, agitating shaft blowdown valve 10, discharge port
11st, chuck alternate outlets 12, agitating shaft
13rd, blade 14, demarcation strip
15th, interface of the level gauge 16, blowdown drum
17th, drain
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The endpoint of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of a scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
In the present invention, in the case where not making conversely explanation, the noun of locality such as " upper and lower " used is typically referred in attached drawing
Above and below.
As shown in Figure 1, the continuous ageing reactor of the present invention includes reactor body, is arranged on the reactor body
The feed inlet 3 in portion and the discharge port 10 for being arranged at the reactor body lower part;It is provided with the reactor body inner wall point
The reactor body is divided into more than 2 aging chambers by partition plate 14, the demarcation strip 14;Set in the middle part of the reactor body
There is agitating shaft 12, corresponding to each aging chamber on the agitating shaft 12 is respectively arranged with blade 13.
According to the present invention, there is no particular limitation for the structure of the reactor body, can be appropriate according to the needs of reaction
Ground selects, the one kind being specifically as follows in reaction tower, reaction kettle or reaction tube.It is preferably reaction tower in them.
In the present invention, the feed inlet 3 is arranged at the top of the reactor body, and the discharge port 10 is arranged at institute
State the lower part of reactor body.In continuous ageing reaction process, material enters the reactor body by the feed inlet 3,
In the case where agitating shaft 12 drives blade to rotate, the material is constantly mixed, and passes sequentially through each aging chamber from top to bottom, finally
Material after aging is obtained by the discharge port 10.
In the present invention, there is no particular limitation for the material, in order to adjust aging reaction condition, ensures sufficient aging
Time, the material are preferably the poor material of mobility, such as slurry material, gel state material etc.., can as the material
To enumerate the slurry of the hydroxide such as aluminium hydroxide, magnesium hydroxide, magnalium hydrotalcite.
According to the present invention, there is no particular limitation for the structure of the demarcation strip 14, as long as can reach reduces reduction of speed under material
The effect of degree.The demarcation strip 14 can be the loop configuration being fixed on the reactor body inner wall, or
The annular or near loop configuration that polylith demarcation strip 14 is spliced to form.In the case that demarcation strip 14 described in polylith splices, every piece of separation
There is no particular limitation for the shape of plate, can also have gap between demarcation strip 14.
The centre of the loop configuration has axis hole, and the agitating shaft is arranged in the axis hole.The size of the axis hole
There is no particular limitation, and material decrease speed that can be as needed is specifically chosen, such as the diameter of the axis hole can be institute
The 20-50% of reactor body internal diameter is stated, is preferably 20-40%, more preferably 30-40%.
In order to adjust material decrease speed, there can also be the perforate that can decline material on the demarcation strip 14.Institute
The gap stated between perforate and above-mentioned polylith demarcation strip 14 can accelerate material decrease speed.The size of the gap and perforate and
Size can be specifically chosen according to the conditions of the aging reactions such as material solid content.Preferably, the gross area of the gap and perforate
The 1-30% of the separation plate suqare is accounted for, is preferably 2-15%, more preferably 4-7%.Phase is preferably distinguished in the gap and perforate
It is distributed for agitating shaft central symmetry, can be uniformly distributed axially, center or periphery can also be closer to.Preferred feelings
Under condition, the immediate vicinity of the demarcation strip 14 can have more gaps and perforate.
In the case of further preferably, in order to make material be uniformly mixed during decline, the demarcation strip 14 can be with
The tapered structure tilted down from inner wall is arranged to, by making material decline close to the position of blade 13, material can be filled
Divide and mixed by blade 13.There is no particular limitation at 14 inclination angle relative to horizontal direction of demarcation strip, such as can be 0-
30 °, be preferably 0.5-15 °, more preferably 1-10 °
In the present invention, the aging chamber being separated to form the reactor body by demarcation strip 14, its size is without spy
Other restriction, can be identical or different, preferably makes the aging space of each aging chamber identical.In the present invention, the aging is empty
Between refer in the aging chamber carry out material mixing complete aging reaction space.
According to the present invention, transmission parts 1 are provided with the top of the reactor body, the transmission parts 1 are used to drive
The agitating shaft 12 rotates.There is no particular limitation for the transmission parts 1, can rotate the agitating shaft 12.Specifically
Ground, the transmission parts can be magnetic stirring apparatus.In the case of preferable, in order to ensure the reaction inside the reactor body
Pressure, the transmission parts 1 are sealings.There is no particular limitation for the mode of the sealing, in order to ensure good sealing effect
Fruit, is preferably transmission seal or mechanical seal.The sealing can be specifically chosen as needed, can also be by above-mentioned sealing means
It is used in combination.For example, the mode of the sealing can be mechanical seal.
According to the present invention, the agitating shaft 12 runs through the reactor body.When the agitating shaft 12 rotates, drive each
Blade 13 in aging chamber rotates at the same time, material is uniformly mixed, and progressively move down.By the agitating shaft for setting one
12, the operation and maintenance process of reactor can be made easy.
According to the present invention, there is no particular limitation for the structure of the blade 13 and quantity, it is possible to achieve the mixing of material is
Can.The blade 13 can be inclined blade turbine formula blade, hinged joint paddle blade, anchor impeller and one kind or more in frame blade
Kind.It is highly preferred that the blade 13 is inclined blade turbine formula blade.In the case of preferable, in order to ensure the uniform mixing of material, make
Material carries out aging at uniform temperature, and the quantity for the blade 13 that corresponding each aging chamber is set is 2-8 leaves, is preferably
4-6 leaves.In the present invention, the quantity of blade 13 described in each aging chamber can be it is one or more groups of, specifically can be according to old
The volume size for changing space carries out reasonable Arrangement, generally 1-6 groups, is preferably 1-2 groups.
According to the present invention, the rotating speed of the blade 13 can be selected according to the situation of specific aging reaction and material.In order to
Ensure the uniform mixing of material, the rotating speed of the blade 13 is preferably more than 50 revs/min, is preferably more than 60 revs/min, more
Preferably more than 80 revs/min, more preferably more than 100 revs/min.In the aging reaction for needing to crystallize, in order not to
Destroy the forming process of material crystal grain, it is preferable that the rotating speed of the blade 13 is preferably less than 350 revs/min, more preferably
Less than 300 revs/min, more preferably less than 200 revs/min, more preferably less than 150 revs/min
According to the present invention, position of the blade 13 on the agitating shaft 12 can specifically be set as needed, can
Ensure the uniform mixing of material.In the case of preferable, position of the blade 13 on the agitating shaft 12 can be adjusted,
And then the mixed effect of blade 13 can be more easily controlled as needed, further improve blending efficiency.
According to the present invention, the impurity in agitating shaft 12 enters the reactor body in order to prevent, the agitating shaft 12
Top and bottom are respectively arranged with guiding sewage draining exit, the guiding sewage draining exit respectively with the blowdown drum 16, agitating shaft blowdown valve 9
It is connected.By setting the guiding sewage draining exit, the abrasion iron filings in agitating shaft 12 can be discharged to outside the aging reaction device,
Ensure the purity of the material of aging reaction.
According to the present invention, the reactor body side wall is coated with chuck 7, and heat-conducting medium is filled with the chuck 7.Root
According to the present invention, the top of the chuck 7 is provided with chuck heat-conducting medium import 4, and the lower part of the chuck 7 is provided with chuck heat conduction
Media outlet 8.The chuck heat-conducting medium import 4 is used to add the heat-conducting medium, and the chuck catheter outlet 8 is used to discharge
The heat-conducting medium.In addition, as needed, the lower part of the chuck 7 is also provided with chuck alternate outlets 11.The chuck
7 are used for the heating and insulation of the reactor body.Heat-conducting medium inside the chuck 7 can specifically be selected according to heating-up temperature
Select, the heat-conducting medium in the chuck 7 can be the heat-conducting medium with certain temperature, such as steam etc., or can be
Heated heat-conducting medium inside the chuck, such as conduction oil.Specifically, may be provided for adding inside the chuck 7
The electrically heated rod of the heat heat-conducting medium.By the setting of the chuck 7, can make to keep necessarily old inside reactor body
Change temperature, ensure the progress of aging reaction.
According to the present invention, chuck temperature-measuring port 6 is provided with the chuck 7, the chuck temperature-measuring port 6 is used to survey by temperature
Device is measured, so as to measure the temperature of the heat-conducting medium inside chuck 7.
According to the present invention, in order to ensure the aging reaction lasting reaction time, the quantity of the aging chamber is 2-10, excellent
Elect 2-8, more preferably 3-6 as.
According to the present invention, the reactor body is preferably voltage-resistant reactor, to meet the aging reaction under certain pressure
Demand.Pressure can be evaporated by the liquid phase in material and produced in the reactor body, can also carry out pressurising as needed.
The pressurising can be carried out by the way of gas is filled with, and there is no particular limitation for the gas, be preferably inert gas.As
The inert gas can be the common inert gases such as helium, argon gas, nitrogen.
According to the present invention, relief valve connection 2 is provided with the top of the reactor body, the relief valve connection 2 is used for
Connect pressure safety valve.By being provided with the pressure safety valve, aging reaction safety at a higher pressure can be made
Carry out.
According to the present invention, drain 17 is provided with the top of the reactor body.The drain 17 is used to adjust institute
State the pressure inside reactor body.
According to the present invention, interface of the level gauge 15 is provided with the side wall of the reactor body.The liquid level gauge is used for
The material liquid level inside the reactor body is detected in continuous ageing reaction.Specifically, the liquid level gauge can shake for tuning fork
Dynamic formula liquid level gauge, magnetic floating liquid level gauge, pressure difference liquid level gauge, ultrasonic level gage etc..The set-up mode of the interface of the level gauge 15
It can be made choice according to specifically used liquid level gauge.
In the present invention, spare feed inlet 5 is provided with the middle part of the reactor body.5 conduct of spare feed inlet
Material enters passage, can select as needed, such as is used when needing shorter ageing time.
The aging method of aluminium hydroxide provided by the invention, this method carry out in above-mentioned continuous ageing reactor, its
In, aluminium hydroxide slurry enters the continuous ageing reactor, under the stirring of agitating shaft, aluminium hydroxide from the feed inlet 3
Slurry passes sequentially through each aging chamber, and is discharged from the discharge port 10, wherein, the reaction temperature of the aging reaction is 25-360
DEG C, reaction pressure 0-20MPa, when the reaction time is 0.1-72 small.
Preferably, the reaction temperature of the aging reaction is 60-280 DEG C, reaction pressure 0.5-10MPa, the reaction time
For 0.5-24 it is small when.Refer to that material enters the time discharged from discharge port 10 from feed inlet 3 in this reaction time.
In the present invention, the control that the reaction temperature of the aging reaction passes through chuck 7.The reaction pressure can be by hydrogen
Liquid phase evaporation in alumina slurry produces, and can also carry out pressurising as needed.The pressurising can use and be filled with gas
Mode carries out, and there is no particular limitation for the gas, is preferably inert gas.Can be helium, argon as the inert gas
The common inert gas such as gas, nitrogen.
In the present invention, the reaction pressure is the pressure in terms of gauge pressure.
In the present invention, the aging reaction is carried out continuously, and the charging rate of the aluminium hydroxide slurry is not special
Limit, in order to ensure that the aging of aluminium hydroxide fully carries out, the charging rate is preferably 50-2000g/ minutes, more preferably
50-1000g/ minutes.During the reaction, the liquid level in the continuous ageing reactor is monitored by liquid level gauge, and can
Suitably to adjust charging rate as needed.
There is no particular limitation for the aluminium hydroxide slurry, such as can be that aluminium alcoholates method prepares alkane during boehmite
The aluminium hydroxide slurry that epoxide aluminium hydrolyzes.There is no particular limitation for the solid content of the aluminium hydroxide slurry, in order to ensure
The aging reaction fully carries out, and the solid content of the aluminium hydroxide slurry is preferably 5-30 weight %.The hydroxide aluminium paste
Water, alcohol, acid etc. can be contained in material.
According to the present invention, there is no particular limitation for the rotating speed of the agitating shaft 12, can be specifically chosen as needed.Specifically
Ground, the rotating speed of the agitating shaft 12 can be used for the size for adjusting obtained boehmite crystal grain.In order to ensure material
Uniformly mixing, the rotating speed of the blade 13 is preferably more than 50 revs/min, is preferably more than 60 revs/min, and more preferably 80
More than rev/min, more preferably more than 100 revs/min.Crystallized in the aging reaction of aluminium hydroxide, in order not to destroy
The forming process of crystal grain, it is preferable that the rotating speed of the blade 13 is preferably less than 350 revs/min, more preferably 300 revs/min
Hereinafter, it is more preferably less than 200 revs/min, more preferably less than 150 revs/min.
By the aging method of aluminium hydroxide provided by the invention, the ageing process of aluminium hydroxide is carried out continuously.By
The blowdown apparatus setting up and down of agitating shaft, it is ensured that the purity of obtained boehmite.By the bar for controlling aging reaction
Part, it is 50-400cm that can obtain specific surface area2/ g, the boehmite that pore volume is 0.3-2.0mL/g, the boehmite
Crystallite dimension is 1-50nm.
The present invention will be described in detail by way of examples below.
Embodiment 1
The present embodiment is carried out using the continuous ageing reactor shown in Fig. 1.
As shown in Figure 1, the continuous ageing reactor includes reaction tower, is arranged at 3 and of feed inlet on the reaction tower top
It is arranged at the discharge port 10 of the reaction tower lower part;Demarcation strip 14 is provided with the reaction inner wall of tower, the demarcation strip 14 will
The reaction tower is divided into 6 aging chambers;Agitating shaft 12 is provided with the middle part of the reaction tower, is corresponded on the agitating shaft 12 each
Aging chamber is respectively arranged with blade 13.
The demarcation strip 14 is the middle tapered structure for having axis hole, being tilted down from inner wall, and the demarcation strip 14 is opposite
In the angle that horizontal direction tilts down be 3 °, the 50% of a diameter of reaction tower internal diameter of the axis hole, the demarcation strip
Do not have perforate on 14.
Transmission parts 1 are provided with the top of the reaction tower, the transmission parts 1 are the magnetic stirring apparatus of mechanical seal,
For driving the agitating shaft 12 to rotate.
The agitating shaft 12 runs through the reaction tower, corresponds to each aging chamber thereon and sets one group of 6 leaf inclined blade turbine formula paddle
Leaf 13.The top and bottom of the agitating shaft 12 are respectively arranged with guiding sewage draining exit, the guiding sewage draining exit respectively with the row
Dirty tank 16, agitating shaft blowdown valve 9 are connected.
According to the present invention, the reaction tower side wall is coated with chuck 7, is filled with conduction oil in the chuck 7, and be used for
Heat the electrically heated rod of the conduction oil.Chuck temperature-measuring port 6 is provided with the chuck 7, is provided with the chuck temperature-measuring port 6
Thermometer, so as to measure the temperature of the heat-conducting medium inside chuck 7.The top of the chuck 7 be provided with chuck heat-conducting medium into
Mouth 4, the lower part of the chuck 7 are provided with chuck heat-conducting medium outlet 8.The chuck heat-conducting medium import 4 is used to add described
Heat-conducting medium, the chuck catheter outlet 8 are used to discharge the heat-conducting medium.The lower part of the chuck 7 is also provided with pressing from both sides
Cover alternate outlets 11.
Relief valve connection 2 is provided with the top of the reaction tower, the relief valve connection 2 is connected with pressure safety valve.Institute
State and drain 17 is additionally provided with the top of reaction tower.Two interface of the level gauge 15, liquid level are provided with the side wall of the reaction tower
Count interface 15 and connect pressure difference liquid level gauge, the amount of slurry in successive reaction reaction tower is monitored by liquid level gauge.In the present embodiment, institute
State and spare feed inlet 5 is additionally provided with the middle part of reaction tower.
In the ageing process of aluminium hydroxide, solid content be 10 weight % aluminium hydroxide slurry from the feed inlet 3 into
Entering the continuous ageing reactor, charging rate is 500g/ minutes, is discharged after reaction from the discharge port 10, in the process,
Aluminium hydroxide slurry is constantly mixed, and passes sequentially through each aging chamber from top to bottom, is obtained always eventually through the discharge port
Material after change.In addition, the condition of reaction is:Reaction temperature is 90 DEG C, reaction pressure 1MPa, when the reaction time is 2 small, institute
The rotating speed for stating agitating shaft 12 is 100 revs/min.
After the completion of aging reaction, it is 203cm to obtain specific surface area2/ g, pore volume 0.7mL/g, crystallite dimension are 5nm's
Boehmite.
Embodiment 2
The aging reaction of aluminium hydroxide is carried out according to the method for embodiment 1, unlike, reaction temperature is 120 DEG C, reaction
Pressure is 2MPa, and when the reaction time is 4 small, the rotating speed of the agitating shaft 12 is 120 revs/min.
After the completion of aging reaction, it is 164cm to obtain specific surface area2/ g, pore volume 1.1mL/g, crystallite dimension are 8nm's
Boehmite.
By above-described embodiment, the aging method of continuous ageing reactor and aluminium hydroxide provided by the invention can
For the aging reaction of aluminum hydroxide slurry, final obtained boehmite is suitable as catalyst carrier.Also, stir
Abrasion iron filings in axis improve the purity of boehmite by guiding sewage draining exit to discharge.
The preferred embodiment of the present invention described in detail above, still, during present invention is not limited to the embodiments described above
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, it can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (13)
1. a kind of continuous ageing reactor, the reactor include reactor body, be arranged at the reactor body top into
Material mouth (3) and the discharge port (10) for being arranged at the reactor body lower part, it is characterised in that
Demarcation strip (14) is provided with the reactor body inner wall, the reactor body is divided into by the demarcation strip (14)
More than 2 aging chambers;
Agitating shaft (12) is provided with the middle part of the reactor body, correspond to each aging chamber on the agitating shaft (12) is set respectively
There is blade (13).
2. reactor according to claim 1, wherein, the demarcation strip (14) is loop configuration, or polylith demarcation strip
(14) loop configuration is spliced to form, there is axis hole among the loop configuration;
Preferably, the 20-50% of a diameter of reactor body internal diameter of the axis hole;
Preferably, the demarcation strip (14) is the tapered structure tilted down from inner wall;
Preferably, the demarcation strip (14) inclination angle relative to horizontal direction is 0-30 °;
Preferably, there is perforate on the demarcation strip (14).
3. reactor according to claim 1, wherein, the agitating shaft (12) runs through the reactor body.
4. reactor according to claim 3, wherein, transmission parts (1), institute are provided with the top of the reactor body
Transmission parts (1) are stated to be used to drive the agitating shaft (12) to rotate.
5. according to the reactor described in any one in claim 1-4, wherein, the top and bottom point of the agitating shaft (12)
Guiding sewage draining exit is not provided with.
6. according to the reactor described in any one in claim 1-4, wherein, the blade that corresponding each aging chamber is set
(13) quantity is 2-8 leaves;
Preferably, the blade (13) is inclined blade turbine formula blade.
7. reactor according to claim 6, wherein, position of the blade (13) on the agitating shaft (12) can be with
Adjust.
8. according to the reactor described in any one in claim 1-4, wherein, the reactor body side wall is coated with chuck
(7);
Preferably, it is filled with heat-conducting medium in the chuck (7).
9. according to the reactor described in any one in claim 1-4, wherein, the quantity of the aging chamber is 2-10.
10. according to the reactor described in any one in claim 1-4, wherein, the reactor body is reaction tower, reaction
One kind in kettle or reaction tube.
11. a kind of aging method of aluminium hydroxide, it is characterised in that this method is in claim 1-10 described in any one
Carried out in continuous ageing reactor, aluminium hydroxide slurry enters the continuous ageing reactor from the feed inlet (3), is stirring
Under the stirring of axis, aluminium hydroxide slurry passes sequentially through each aging chamber, and is discharged from the discharge port (10), wherein, the aging
The reaction temperature of reaction is 25-360 DEG C, reaction pressure 0-20MPa, when the reaction time is 0.1-72 small.
12. aging method according to claim 11, wherein, the rotating speed of the agitating shaft (12) is 50-350 revs/min.
13. the aging method according to claim 11 or 12, wherein, the solid content of the aluminium hydroxide slurry is 5-30 weights
Measure %.
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