CN114522632B - Pseudo-boehmite preparation device and pseudo-boehmite preparation method - Google Patents
Pseudo-boehmite preparation device and pseudo-boehmite preparation method Download PDFInfo
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- CN114522632B CN114522632B CN202011230431.9A CN202011230431A CN114522632B CN 114522632 B CN114522632 B CN 114522632B CN 202011230431 A CN202011230431 A CN 202011230431A CN 114522632 B CN114522632 B CN 114522632B
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- boehmite
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- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 title claims abstract description 148
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 214
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 108
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 108
- 238000006243 chemical reaction Methods 0.000 claims abstract description 66
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 94
- 238000009826 distribution Methods 0.000 claims description 73
- 230000032683 aging Effects 0.000 claims description 54
- 238000003860 storage Methods 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 32
- 238000010790 dilution Methods 0.000 claims description 19
- 239000012895 dilution Substances 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 18
- 239000012265 solid product Substances 0.000 description 16
- 238000001035 drying Methods 0.000 description 15
- 238000001228 spectrum Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000003679 aging effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- VCNTUJWBXWAWEJ-UHFFFAOYSA-J aluminum;sodium;dicarbonate Chemical compound [Na+].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O VCNTUJWBXWAWEJ-UHFFFAOYSA-J 0.000 description 3
- 229910001647 dawsonite Inorganic materials 0.000 description 3
- 150000004684 trihydrates Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- -1 aluminum alkoxide Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- UOCIZHQMWNPGEN-UHFFFAOYSA-N dialuminum;oxygen(2-);trihydrate Chemical compound O.O.O.[O-2].[O-2].[O-2].[Al+3].[Al+3] UOCIZHQMWNPGEN-UHFFFAOYSA-N 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- 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
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to the technical field of compound preparation, and discloses a preparation device and a preparation method of pseudo-boehmite, wherein the preparation device comprises a pseudo-boehmite reactor provided with a meta-aluminate inlet for entering meta-aluminate solution and a carbon dioxide inlet for entering carbon dioxide, a reaction chamber for reacting the meta-aluminate with the carbon dioxide to obtain a solution containing the pseudo-boehmite is arranged in the pseudo-boehmite reactor, and the pseudo-boehmite reactor is provided with a product outlet for discharging the solution containing the pseudo-boehmite obtained by the reaction; a distributor which uniformly distributes the carbon dioxide entering from the carbon dioxide inlet into the reaction chamber is arranged in the reaction chamber. The preparation device realizes the generation of pseudo-boehmite, so that the reaction for synthesizing the pseudo-boehmite is stably and uniformly carried out. The preparation method comprises the following steps: so that the carbon dioxide is uniformly distributed in the meta-aluminate solution; the carbon dioxide reacts with the meta-aluminate solution to obtain a solution containing pseudo-boehmite.
Description
Technical Field
The invention relates to the technical field of compound preparation, in particular to a device and a method for preparing pseudo-boehmite.
Background
The pseudo-boehmite has the characteristics of high specific surface area, large pore volume, good molding property, good peptization and thixotropic properties and the like, and is widely used as a drying agent, an adsorbent, a molding binder, a catalyst carrier, raw materials for preparing active alumina and the like in the petrochemical industry.
The method for producing pseudo-boehmite mainly comprises an aluminum alkoxide hydrolysis method and a neutralization method. The carbonization method for preparing the pseudo-boehmite relies on the sintering method to produce the alumina, utilizes the intermediate product NaAlO 2 solution and CO 2 waste gas as reaction raw materials, is the process route with the lowest cost, and the waste liquid in production can be returned to the alumina production process for reuse, so that the method has the advantages of basically no waste discharge, little environmental pollution and simple process, and is a method with competitive advantage and prospect.
Disclosure of Invention
The invention aims to provide a preparation device of pseudo-boehmite, which realizes the generation of the pseudo-boehmite and can lead the reaction for synthesizing the pseudo-boehmite to be carried out smoothly and evenly.
In order to achieve the above object, according to one aspect of the present invention, there is provided a pseudo-boehmite preparation apparatus comprising a pseudo-boehmite reactor provided with a meta-aluminate inlet for a meta-aluminate solution to enter and a carbon dioxide inlet for carbon dioxide to enter, a reaction chamber for reacting meta-aluminate with carbon dioxide to obtain a solution containing pseudo-boehmite being provided in the pseudo-boehmite reactor, the pseudo-boehmite reactor being provided with a product discharge port for discharging the solution containing pseudo-boehmite obtained by the reaction; the preparation device of pseudo-boehmite still includes set up in the distributor in the reaction chamber, the distributor sets up to with carbon dioxide that gets into by the carbon dioxide import evenly distributed in the reaction chamber.
The device for preparing the pseudo-boehmite realizes the generation of the pseudo-boehmite, and can lead the reaction for synthesizing the pseudo-boehmite to be carried out stably and uniformly.
Preferably, the distributor comprises a distribution pipe arranged in the reaction chamber, the distribution pipe is provided with a distribution pipe inlet communicated with the carbon dioxide inlet, and a plurality of distribution holes are formed in the distribution pipe and uniformly distributed in the distribution pipe.
Preferably, the distributor comprises a distribution plate arranged in the reaction chamber, a plurality of distribution openings are formed in the distribution plate, the distribution openings are uniformly distributed in the distribution plate, and the distribution plate is arranged at a downstream position of the carbon dioxide inlet along the flow direction of the carbon dioxide.
Preferably, the preparation device of pseudo-boehmite comprises a liquid distribution plate arranged in the reaction chamber, wherein the liquid distribution plate is arranged between the distribution plate and the meta-aluminate inlet, a plurality of liquid inlets for passing the meta-aluminate solution are arranged on the liquid distribution plate, and a plurality of liquid inlets are uniformly arranged on the liquid distribution plate.
Preferably, the preparation device of pseudo-boehmite comprises a first storage tank, a first storage chamber capable of containing meta-aluminate solution is arranged in the first storage tank, a first discharge outlet for discharging the meta-aluminate solution from the first storage chamber is arranged in the first storage tank, and the first discharge outlet is communicated with the meta-aluminate inlet.
Preferably, the preparation device of pseudo-boehmite comprises a second storage tank, wherein a second storage chamber capable of containing carbon dioxide is arranged in the second storage tank, a second discharge outlet for discharging carbon dioxide out of the second storage chamber is arranged in the second storage tank, and the second discharge outlet is communicated with the carbon dioxide inlet; or alternatively
The preparation device of pseudo-boehmite include the second holding vessel, be provided with the second storage chamber that can hold carbon dioxide in the second holding vessel, the second holding vessel is equipped with and supplies carbon dioxide to discharge the second discharge port of second storage chamber, the second discharge port with the carbon dioxide import is linked together, and be provided with the dilution gas import that supplies the dilution gas of adjusting the concentration of carbon dioxide to get into on the second holding vessel.
Preferably, the preparation device of pseudo-boehmite includes ageing tank, be provided with ageing cavity in the ageing tank, ageing tank is provided with ageing import and supplies ageing liquid exhaust ageing export after ageing, wherein:
The aging inlet communicates with the product outlet.
Preferably, the apparatus for preparing pseudo-boehmite comprises a separation scrubber provided downstream of the aging tank, the separation scrubber being configured to be able to receive the aged pseudo-boehmite-containing solution discharged from the aging tank and to wash and separate the solution.
Preferably, the apparatus for preparing pseudo-boehmite comprises a dryer provided downstream of the separation scrubber, the dryer being configured to receive the pseudo-boehmite-containing mixture discharged from the separation scrubber and to dry the mixture.
The second aspect of the present invention provides a method for preparing pseudo-boehmite, which comprises:
Step S00: so that the carbon dioxide is uniformly distributed in the meta-aluminate solution;
step S20: the carbon dioxide reacts with the meta-aluminate solution to obtain a solution containing pseudo-boehmite.
Preferably, in said step S20, said carbon dioxide and said meta-aluminate solution are reacted at 15 ℃ to 30 ℃; and/or
In the step S20, the reaction time of the carbon dioxide and the meta-aluminate solution is 10S to 3000S.
Preferably, the preparation method of the pseudo-boehmite comprises the following steps:
step S40: aging the solution containing pseudo-boehmite obtained in the step S20 to obtain an aging solution, preferably at a temperature of 10 ℃ to 75 ℃ for more than 0 hours and less than or equal to 5 hours.
Preferably, in the step S00, the carbon dioxide is introduced in an amount of 0.5L/min-5L/min; and/or
In the step S00, the concentration of the meta-aluminate solution is 10g/L to 300g/L.
Drawings
Fig. 1 is a schematic view showing the overall structure of a pseudo-boehmite production apparatus according to a preferred embodiment of the invention;
Fig. 2 is a schematic cross-sectional structure of a pseudo-boehmite production apparatus according to another preferred embodiment of the invention;
fig. 3 is a schematic overall structure of a pseudo-boehmite production apparatus according to a preferred embodiment of the invention;
FIG. 4 is an XRD pattern of the corresponding product obtained in the examples, wherein curve 1 shows the XRD pattern of the product containing pseudo-boehmite and aluminum oxide trihydrate, curve 2 shows the XRD pattern of the product containing pseudo-boehmite and dawsonite (NaAlCO 3(OH)2), and curve 3 shows the XRD pattern of the product containing pseudo-boehmite alone; the three peak components of the chemical formula are marked below to represent the standard spectra of the corresponding compounds, respectively.
Description of the reference numerals
10-A preparation device of pseudo-boehmite; 12-a first storage tank; 120-a first storage chamber; 12 a-a transfer pump; 14-a second storage tank; 140-a second storage chamber; 14 a-a flow controller; a 16-pseudo-boehmite reactor; 160-a reaction chamber; 162-reaction stirring slurry; 164-meta-aluminate inlet; 166-carbon dioxide inlet; 168-product discharge port; 169-vent; 180-distributing pipes; 182-distribution plate; 19-a liquid distribution plate; 20 a-an aging tank; 200 a-an aging chamber; 202-aging stirring slurry; 20 b-separation scrubber; 20 c-a dryer; 22 a-a first delivery tube; 22 b-a first buffer tank; 22 c-a first pressure gauge; 22 d-a first filter; 22 e-a first control valve; 22 f-a first one-way valve; 22 g-first flow controller; 24 a-a second delivery tube; 24 b-a second buffer tank; 24 c-a second pressure gauge; 24 d-a second filter; 24 e-a second control valve; 24 f-a second one-way valve; 24 g-second flow controller; 26-a thermostat; 26 a-a third delivery tube; 26 c-a third pressure gauge; 26 d-a third filter; 26 e-a third control valve; 26 f-a third one-way valve; 26 g-third flow controller.
Detailed Description
In the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, left, right" and the like are used generally to refer to the orientation understanding shown in the drawings and in practice, and "inner, outer" refer to the inner, outer of the outline of the components.
The invention provides a preparation device of pseudo-boehmite, the preparation device 10 of pseudo-boehmite comprises a pseudo-boehmite reactor 16, the pseudo-boehmite reactor 16 is provided with a meta-aluminate inlet 164 for a meta-aluminate solution to enter, the meta-aluminate solution can enter the pseudo-boehmite reactor 16 through the meta-aluminate inlet 164, the meta-aluminate inlet 164 can be arranged at the bottom of the pseudo-boehmite reactor 16, and the meta-aluminate inlet 164 can also be arranged at the top of the pseudo-boehmite reactor 16; the pseudo-boehmite reactor 16 is provided with a carbon dioxide inlet 166 for carbon dioxide to enter, carbon dioxide can enter the pseudo-boehmite reactor 16 through the carbon dioxide inlet 166, and the carbon dioxide inlet 166 can be arranged at the bottom of the pseudo-boehmite reactor 16; the pseudo-boehmite reactor 16 is provided with a reaction chamber 160 for reacting meta-aluminate with carbon dioxide to obtain a solution containing pseudo-boehmite, and it is understood that the meta-aluminate inlet 164 and the carbon dioxide inlet 166 are both communicated with the pseudo-boehmite reactor 16; the pseudo-boehmite reactor 16 is provided with a product outlet 168 for discharging a solution containing pseudo-boehmite obtained by the reaction, the product outlet 168 is communicated with the reaction chamber 160, the product outlet 168 can be arranged at the bottom of the pseudo-boehmite reactor 16, and the product outlet 168 can also be arranged at the top of the pseudo-boehmite reactor 16; the reaction chamber 160 is internally provided with a distributor, the distributor is arranged to uniformly distribute carbon dioxide entering from the carbon dioxide inlet 166 into the reaction chamber 160, and the carbon dioxide can be uniformly distributed in the reaction chamber 160 through the distributor, so that the carbon dioxide can be uniformly distributed in the meta-aluminate solution, and the uniformly distributed carbon dioxide can be fully contacted with the meta-aluminate in the meta-aluminate solution, thereby enabling the reaction to be uniformly and stably carried out. Wherein the meta-aluminate solution comprises a sodium meta-aluminate solution. It will be appreciated that the meta-aluminate solution may be heated to a preset temperature whereby the reaction between carbon dioxide and meta-aluminate may be carried out at a suitable temperature, and alternatively, the pseudo-boehmite reactor 16 may be subjected to a heated atmosphere such that the reaction between carbon dioxide and meta-aluminate is carried out at a moderate temperature. In addition, the reaction gives a solution containing pseudo-boehmite in the form of a gel or slurry.
As shown in fig. 1, the distributor may include a distribution pipe 180 disposed within the reaction chamber 160, the distribution pipe 180 may be provided with a distribution pipe inlet communicating with the carbon dioxide inlet 166, for example, the carbon dioxide inlet 166 may be disposed at a bottom wall of the pseudo-boehmite reactor 16, the distribution pipe inlet of the distribution pipe 180 may be communicated with the carbon dioxide inlet 166, such as a first end of the distribution pipe 180 may be formed as an open end, which may be formed as a distribution pipe inlet, wherein the open end may be covered at a periphery of the carbon dioxide inlet 166, a plurality of distribution holes may be disposed on the distribution pipe 180, and the plurality of distribution holes may be uniformly distributed at the distribution pipe 180, such that carbon dioxide entering the distribution pipe 180 is uniformly distributed within the reaction chamber 160 through the uniformly disposed plurality of distribution holes. It is understood that the distribution pipe 180 may extend in the flow direction of the carbon dioxide.
As shown in fig. 1, a meta-aluminate inlet 164 may be provided at the bottom of the pseudo-boehmite reactor 16, and meta-aluminate solution may enter the reaction chamber 160 from the meta-aluminate inlet 164.
As shown in fig. 2, the distributor includes a distribution plate 182 disposed within the reaction chamber 160, the distribution plate 182 having a plurality of distribution ports disposed thereon, the plurality of distribution ports being uniformly distributed on the distribution plate 182, the distribution plate 182 being disposed at a position downstream of the carbon dioxide inlet 166 in the flow direction of the carbon dioxide. Under the action of the distribution plate 182, the carbon dioxide can be uniformly distributed in the reaction chamber 160, so that the carbon dioxide can be uniformly distributed in the meta-aluminate solution, and uniform and stable reaction is ensured.
The carbon dioxide inlet 166 may be disposed at a bottom wall of the pseudo-boehmite reactor 16, the meta-aluminate inlet 164 may be disposed at a top of the pseudo-boehmite reactor 16, a distribution plate 182 may be disposed between the carbon dioxide inlet 166 and the meta-aluminate inlet 164, and the distribution plate 182 may divide the reaction chamber 160 into two portions distributed along a height direction of the pseudo-boehmite reactor 16. In addition, the carbon dioxide inlet 166 may be disposed at a top wall of the pseudo-boehmite reactor 16 and the meta-aluminate solution may be disposed at a side wall of the pseudo-boehmite reactor 16.
To vent unreacted carbon dioxide, a vent 169 may be provided at the top of the pseudo-boehmite reactor 16. In addition, a reaction stirring paddle 162 can be arranged in the reaction chamber 160, and the reaction can be more stably and uniformly carried out under the stirring action of the reaction stirring paddle 162, so that the yield of a product obtained by the reaction and the quality of the product are improved. The product discharge outlet 168 may be provided in a side wall of the pseudo-boehmite reactor 16.
As shown in fig. 2, a liquid distribution plate 19 may be disposed in the reaction chamber 160, the liquid distribution plate 19 may be disposed between the distribution plate 182 and the meta-aluminate inlet 164, and a plurality of liquid inlets through which the meta-aluminate solution passes may be disposed on the liquid distribution plate 19, and the plurality of liquid inlets may be uniformly disposed on the liquid distribution plate 19, it may be understood that the liquid distribution plate 19 may divide the reaction chamber 160 into two portions distributed along the height direction of the pseudo-boehmite reactor 16, and the liquid distribution plate 19 may be disposed above the distribution plate 182 as viewed from the orientation shown in fig. 2. By arranging the liquid distribution plate 19, the meta-aluminate solution can be uniformly distributed in the reaction chamber 160, and meanwhile, the rate of entering the reaction chamber 160 by the meta-aluminate solution can be moderately controlled, so that the stability and uniformity of the reaction are further improved.
A plurality of liquid distribution plates 19 may be disposed between the distribution plate 182 and the meta-aluminate inlet 164, and the plurality of liquid distribution plates 19 may be spaced apart along the height direction of the pseudo-boehmite reactor 16, thereby better controlling the rate at which the meta-aluminate solution enters the reaction chamber 160 and the uniformity of the distribution of the meta-aluminate solution.
As shown in fig. 1, a first storage tank 12 may be provided, a first storage chamber 120 capable of containing a meta-aluminate solution may be provided within the first storage tank 12, the first storage tank 12 may be provided with a first discharge outlet for the meta-aluminate solution to exit the first storage chamber 120, and the first discharge outlet may be in communication with the meta-aluminate inlet 164. In order to be able to better deliver the meta-aluminate solution into the pseudo-boehmite reactor 16, a meta-aluminate delivery pipe may be provided between the first discharge outlet and the meta-aluminate inlet 164 and a delivery pump 12a may be provided on the meta-aluminate delivery pipe, the delivery pump 12a being able to deliver the meta-aluminate solution into the pseudo-boehmite reactor 16.
In addition, a second storage tank 14 may be provided, a second storage chamber 140 capable of containing carbon dioxide may be provided in the second storage tank 14, the second storage tank 14 may be provided with a second discharge port through which carbon dioxide is discharged from the second storage chamber 140, and the second discharge port may be in communication with the carbon dioxide inlet 166.
A carbon dioxide delivery tube may be provided between the second exhaust port and the carbon dioxide inlet 166 and a flow controller 14a may be provided on the carbon dioxide delivery tube, the flow controller 14a controlling the amount of carbon dioxide entering the pseudo-boehmite reactor 16.
A dilution gas inlet through which the dilution gas enters may be provided in the second storage tank 14, and the concentration of carbon dioxide may be adjusted. Wherein the diluent gas may comprise air and/or an inert gas, which may comprise nitrogen.
As shown in fig. 3, a first delivery pipe 22a capable of delivering a dilution gas may be provided on the dilution gas inlet; a first pressure gauge 22c capable of detecting the pressure of the dilution gas in the first delivery pipe 22a may be provided on the first delivery pipe 22a; a first buffer tank 22b may be provided on the first transfer pipe 22a, the first buffer tank 22b being capable of accommodating the dilution gas, and the first buffer tank 22b being provided with a first buffer inlet and a first buffer outlet for the dilution gas to enter and exit, by providing the first buffer tank 22b, the dilution gas in the first transfer pipe 22a may be smoothly transferred, and the first buffer tank 22b may be provided downstream of the first pressure gauge 22c in the flow direction of the dilution gas; a first filter 22d that filters particulate matter in the dilution gas may be provided on the first delivery pipe 22a, and the first filter 22d may be provided downstream of the first buffer tank 22b in the flow direction of the dilution gas; a first flow controller 22g capable of controlling the flow rate of the dilution gas in the first delivery pipe 22a may be provided on the first delivery pipe 22a, and the first flow controller 22g may be provided downstream of the first filter 22d in the flow direction of the dilution gas; a first control valve 22e may be provided on the first delivery pipe 22a, the first control valve 22e may be provided between the first flow controller 22g and the first filter 22d, and the first control valve 22e may be provided downstream of the first flow controller 22g in the flow direction of the dilution gas; a first check valve 22f may be provided on the first delivery pipe 22a, and the first check valve 22f may be provided downstream of the first flow controller 22g in the flow direction of the dilution gas.
In addition, an air inlet through which carbon dioxide enters may be provided in the second storage tank 14, and a second delivery pipe 24a capable of delivering carbon dioxide may be provided in the air inlet; a second pressure gauge 24c capable of detecting the pressure of the carbon dioxide in the second delivery pipe 24a may be provided on the second delivery pipe 24a; a second buffer tank 24b may be provided on the second transfer pipe 24a, the second buffer tank 24b being capable of containing carbon dioxide, and the second buffer tank 24b being provided with a second buffer inlet and a second buffer outlet for carbon dioxide to enter and exit, the carbon dioxide in the second transfer pipe 24a being smoothly transferred by providing the second buffer tank 24b, the second buffer tank 24b being provided downstream of the second pressure gauge 24c in the flow direction of the carbon dioxide; a second filter 24d that filters particulate matter in the carbon dioxide may be provided on the second delivery pipe 24a, and the second filter 24d may be provided downstream of the second buffer tank 24b in the flow direction of the carbon dioxide; a second flow controller 24g capable of controlling the flow rate of the carbon dioxide in the second delivery pipe 24a may be provided on the second delivery pipe 24a, and the second flow controller 24g may be provided downstream of the second filter 24d in the flow direction of the carbon dioxide; a second control valve 24e may be provided on the second delivery pipe 24a, the second control valve 24e may be provided between the second flow controller 24g and the second filter 24d, and the second control valve 24e may be provided downstream of the second flow controller 24g in the flow direction of the carbon dioxide; a second check valve 24f may be provided on the second delivery pipe 24a, and the second check valve 24f may be provided downstream of the second flow controller 24g in the flow direction of the carbon dioxide.
A third delivery tube 26a capable of delivering a meta-aluminate solution may be provided between the first discharge outlet of the first storage tank 12 and the meta-aluminate inlet 164; a thermostat 26 may be provided on the third delivery pipe 26a to maintain the meta-aluminate solution at a preset temperature, it being understood that the thermostat 26 has a constant temperature inlet and a constant temperature outlet; a third filter 26d for filtering particulate matters in the meta-aluminate solution may be provided on the third delivery pipe 26a, and the third filter 26d may be provided downstream of the thermostat 26 in the flow direction of the meta-aluminate solution; a third flow controller 26g capable of controlling the flow rate of the meta-aluminate solution in the third delivery pipe 26a may be provided on the third delivery pipe 26a, and the third flow controller 26g may be provided downstream of the third filter 26d in the flow direction of the carbon dioxide; a third control valve 26e may be provided on the third delivery pipe 26a, and the third control valve 26e may be provided between the third flow controller 26g and the third filter 26 d; a third pressure gauge 26c capable of detecting the pressure in the third delivery pipe 26a may be provided on the third delivery pipe 26a; a third check valve 26f may be provided on the third delivery pipe 26a, and the third check valve 26f may be provided downstream of the third flow controller 26g in the flow direction of the meta-aluminate solution.
In addition, an aging tank 20a may be provided, and an aging chamber 200a may be provided in the aging tank 20a, the aging tank 20a being provided with an aging inlet and an aging outlet for discharging aged aging liquid, wherein: the aging inlet may be in communication with the product outlet 168. After the solution containing pseudo-boehmite obtained by the reaction enters the aging chamber 200a, the crystal of pseudo-boehmite continues to grow, thereby completing the crystal structure growth of the desired product. It is understood that a heating part may be provided on the aging tank 20a, and the heating part may heat the aging liquid in the aging chamber 200a to improve the aging effect; in addition, the aging stirring paddle 202 having a stirring function may be provided in the aging chamber 200a, whereby the aging effect can be further improved.
As shown in fig. 1, a separation scrubber 20b may be disposed downstream of the aging tank 20a, and the separation scrubber 20b may be disposed so as to be capable of receiving the aged pseudo-boehmite-containing solution discharged from the aging tank 20a and washing and separating the solution, for example, the pseudo-boehmite-containing solution may be filtered to obtain a solid product while the separated solid product may be optionally washed with water. The solid product is a mixture containing pseudo-boehmite, in which alumina trihydrate (Al (OH) 3*3H2 O) and/or dawsonite (NaAl (OH) 2CO3) may be mixed in addition to the pseudo-boehmite.
In addition, a dryer 20c may be provided downstream of the separation scrubber 20b, and the dryer 20c may be provided to be capable of receiving the pseudo-boehmite-containing mixture discharged from the separation scrubber 20b and drying the mixture. Wherein the temperature at the time of drying may be 10-100 ℃, further preferably, the temperature at the time of drying may be 20-80 ℃, still further preferably, the temperature at the time of drying may be 30-60 ℃; preferably, the drying time may be 10s to 4 hours, further preferably, the drying time may be 5min to 2.5 hours, still further preferably, the drying time may be 20min to 1 hour.
The invention also provides a preparation method of pseudo-boehmite, preferably, the preparation device 10 of pseudo-boehmite provided by the invention can be utilized to prepare the pseudo-boehmite, and the preparation method of the pseudo-boehmite comprises the following steps: step S00: so that the carbon dioxide is uniformly distributed in the meta-aluminate solution; step S20: the carbon dioxide reacts with the meta-aluminate solution to obtain a solution containing pseudo-boehmite.
In the step S00, the carbon dioxide inflow amount may be 0.5L/min to 5L/min, and setting the carbon dioxide inflow amount within the above range can make the reaction proceed uniformly and smoothly. Preferably, the carbon dioxide is introduced in an amount of 1L/min-3.5L/min; still more preferably, the carbon dioxide may be introduced in an amount of 1L/min to 2.5L/min.
In step S00, the concentration of the meta-aluminate solution may be 10g/L to 300g/L, and setting the concentration of the meta-aluminate solution within the above-mentioned range may allow the reaction to proceed uniformly and smoothly. Preferably, the concentration of the meta-aluminate solution may be 15-180g/L; further preferably, the concentration of the meta-aluminate solution may be in the range of 20 to 100g/L; still more preferably, the concentration of the meta-aluminate solution may be in the range of 20-80g/L, most preferably, the concentration of the meta-aluminate solution may be in the range of 20-40g/L. Wherein the meta-aluminate solution comprises sodium meta-aluminate. In step S20, the carbon dioxide and the meta-aluminate solution may react at 15 ℃ to 30 ℃, and the reaction may be performed within the above temperature range, so that the reaction between the two may be performed more smoothly and uniformly.
In step S20, the reaction time of the carbon dioxide and the meta-aluminate solution may be 10S to 3000S. Setting the reaction time within the above range allows sufficient reaction between the two and ensures the reaction efficiency. Further preferably, the reaction time may be 50s to 1800s, still further preferably, the reaction time may be 200s to 1500s.
In step S20, the solution containing pseudo-boehmite is obtained in a colloidal or slurry form, and the pH of the solution containing pseudo-boehmite is preferably 7.5-10.5, and the pH of the solution containing pseudo-boehmite is controlled within the above-mentioned range, which is advantageous for improving the quality of the obtained product.
In addition, the inventor researches that when the concentration of the meta-aluminate solution is more than or equal to 20g/L and less than 40g/L, the reaction can obtain a product basically containing pseudo-boehmite; when the concentration of the meta-aluminate solution is not less than 40g/L, and the pH value of the solution obtained by the reaction is controlled to be less than 10.5, the product basically containing pseudo-boehmite can be obtained by the reaction; when the concentration of the meta-aluminate solution is not less than 40g/L and the pH value of the solution obtained by the reaction is controlled to be not less than 10.5, the reaction can obtain a product substantially containing alumina trihydrate.
The preparation method of the pseudo-boehmite can comprise the step S40 of aging the solution containing the pseudo-boehmite obtained in the step S20 to obtain an aging solution. Preferably, the solution containing pseudo-boehmite may be aged at a predetermined temperature to allow the crystals of the product to grow, thereby obtaining a complete crystal structure.
Wherein the aging temperature can be 10-75 ℃, so that the aging effect and the aging efficiency can be improved, and the aging temperature can be 15-60 ℃ preferably; in addition, the aging time may be more than 0 hours and less than or equal to 5 hours, thereby not only improving the aging efficiency, reducing the energy consumption, but also ensuring the aging effect.
The preparation method of pseudo-boehmite may include step S60, in which the obtained aging liquid is separated and washed to obtain a solid product, and the solid product is described in the foregoing and is not described herein. Wherein, the solid-liquid separation can be carried out by filtering, and the solid product can be washed by water in the separation process.
The preparation method of pseudo-boehmite may include step S80, and the obtained solid product is dried. Wherein the temperature at the time of drying may be 10-100 ℃, thereby not only ensuring the drying effect, but also having no substantial influence on the obtained solid product, further preferably, the temperature at the time of drying may be 20-80 ℃, still further preferably, the temperature at the time of drying may be 30-60 ℃; in addition, the drying time may be 10s to 4 hours, more preferably, the drying time may be 5min to 2.5 hours, still more preferably, the drying time may be 20min to 1 hour.
In addition, the specific surface area of the pseudo-boehmite prepared can be 90-400m 2·g-1, the pore volume can be 0.2-2.0m 3·g-1, and the pore diameter can be 3.0-20.0nm. Therefore, the pseudo-boehmite prepared by the method has a wider application range.
The effects of the present invention will be further described with reference to examples.
Examples
Examples 1 to 28
The pseudo-boehmite preparation device shown in figure 1 and the pseudo-boehmite preparation method provided by the invention are utilized for preparing the pseudo-boehmite.
In various examples, the carbon dioxide introduction amount, the solution concentration of the meta-aluminate solution, the reaction temperature of the carbon dioxide and the meta-aluminate solution, the aging temperature at which the pseudo-boehmite-containing solution obtained by the reaction was aged, the aging time, the washing agent and the separation washing temperature selected when the obtained aging liquid was subjected to the separation washing, and the drying temperature at which the solid product obtained after the separation washing was dried are shown in table 1 below.
TABLE 1
Test case
Test case one
The PH of the pseudo-boehmite-containing solution obtained in each example and the specific surface area, pore volume and pore diameter of the obtained solid product were examined, and the results are shown in table 2 below.
TABLE 2
In table 2, the "/" indicates that no correlation detection was performed.
Test case two
XRD testing was performed on the solid product obtained in example 4, to obtain a spectrum shown in curve 1 in FIG. 4, wherein the solid product mainly contains pseudo-boehmite and alumina trihydrate according to comparison with the standard spectrum below; XRD testing was performed on the solid product obtained in example 9, to obtain a spectrum shown in curve 2 in FIG. 4, wherein the solid product mainly contains pseudo-boehmite and dawsonite as well, according to comparison with the standard spectrum below; XRD testing was performed on the solid product obtained in example 1, resulting in a spectrum shown in curve 3 of fig. 4, based on the fact that the solid product was substantially pseudo-boehmite compared with the standard spectrum below.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of individual specific technical features in any suitable way. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition. Such simple variations and combinations are likewise to be regarded as being within the scope of the present disclosure.
Claims (11)
1. A pseudo-boehmite preparation device (10) comprising a pseudo-boehmite reactor (16), wherein the pseudo-boehmite reactor (16) is provided with a meta-aluminate inlet (164) for entering meta-aluminate solution and a carbon dioxide inlet (166) for entering carbon dioxide, a reaction chamber (160) for reacting the meta-aluminate with the carbon dioxide to obtain a solution containing the pseudo-boehmite is arranged in the pseudo-boehmite reactor (16), and the pseudo-boehmite reactor (16) is provided with a product outlet (168) for discharging the solution containing the pseudo-boehmite obtained by the reaction; the pseudo-boehmite preparation device (10) further comprises a distributor arranged in the reaction chamber (160), wherein the distributor is used for uniformly distributing carbon dioxide entering from the carbon dioxide inlet (166) into the reaction chamber (160);
The distributor comprises a distribution plate (182) arranged in the reaction chamber (160), a plurality of distribution openings are formed in the distribution plate (182), the distribution openings are uniformly distributed in the distribution plate (182), and the distribution plate (182) is arranged at a downstream position of the carbon dioxide inlet (166) along the flow direction of the carbon dioxide;
The preparation device (10) of pseudo-boehmite comprises a liquid distribution plate (19) arranged in the reaction chamber (160), wherein the liquid distribution plate (19) is arranged between the distribution plate (182) and the meta-aluminate inlet (164), a plurality of liquid inlets for passing meta-aluminate solution are formed in the liquid distribution plate (19), and the liquid inlets are uniformly formed in the liquid distribution plate (19).
2. The apparatus for preparing pseudo-boehmite according to claim 1, characterized in that the distributor comprises a distribution pipe (180) arranged in the reaction chamber (160), the distribution pipe (180) is provided with a distribution pipe inlet communicated with the carbon dioxide inlet (166), the distribution pipe (180) is provided with a plurality of distribution holes, and the plurality of distribution holes are uniformly distributed in the distribution pipe (180).
3. The apparatus for preparing pseudo-boehmite according to claim 1, characterized in that the apparatus (10) for preparing pseudo-boehmite comprises a first storage tank (12), a first storage chamber (120) capable of containing meta-aluminate solution is provided in the first storage tank (12), the first storage tank (12) is provided with a first discharge outlet for discharging meta-aluminate solution from the first storage chamber (120), and the first discharge outlet is communicated with the meta-aluminate inlet (164).
4. The apparatus for preparing pseudo-boehmite according to claim 1, characterized in that said apparatus for preparing pseudo-boehmite (10) comprises a second storage tank (14), a second storage chamber (140) capable of containing carbon dioxide being provided in said second storage tank (14), said second storage tank (14) being provided with a second outlet for carbon dioxide to exit said second storage chamber (140), said second outlet being in communication with said carbon dioxide inlet (166); or alternatively
The preparation device (10) of pseudo-boehmite comprises a second storage tank (14), a second storage chamber (140) capable of containing carbon dioxide is arranged in the second storage tank (14), a second discharge outlet for discharging carbon dioxide out of the second storage chamber (140) is formed in the second storage tank (14), the second discharge outlet is communicated with the carbon dioxide inlet (166), and a dilution gas inlet for entering dilution gas for adjusting the concentration of carbon dioxide is formed in the second storage tank (14).
5. The apparatus for producing pseudo-boehmite according to any one of claims 1-4, characterized in that the apparatus (10) for producing pseudo-boehmite comprises an aging tank (20 a), an aging chamber (200 a) is provided in the aging tank (20 a), the aging tank (20 a) is provided with an aging inlet and an aging outlet for discharging aged aging liquid, wherein:
The aging inlet communicates with the product outlet (168).
6. The apparatus for preparing pseudo-boehmite according to claim 5, characterized in that the apparatus (10) for preparing pseudo-boehmite comprises a separation scrubber (20 b), said separation scrubber (20 b) being arranged downstream of the aging tank (20 a), said separation scrubber (20 b) being arranged so as to be able to receive the aged pseudo-boehmite-containing solution discharged from the aging tank (20 a) and to wash and separate the solution.
7. The apparatus for preparing pseudo-boehmite according to claim 6, characterized in that the apparatus (10) for preparing pseudo-boehmite comprises a dryer (20 c) arranged downstream of the separation scrubber (20 b), the dryer (20 c) being arranged so as to be able to receive the pseudo-boehmite-containing mixture exiting from the separation scrubber (20 b) and to dry it.
8. A method for preparing pseudo-boehmite, characterized in that the method for preparing pseudo-boehmite is performed in the apparatus for preparing pseudo-boehmite according to any one of claims 1-7, and the method for preparing pseudo-boehmite comprises:
Step S00: so that the carbon dioxide is uniformly distributed in the meta-aluminate solution;
step S20: the carbon dioxide reacts with the meta-aluminate solution to obtain a solution containing pseudo-boehmite.
9. The method for preparing pseudo-boehmite according to claim 8 wherein in step S20, the carbon dioxide and the meta-aluminate solution are reacted at 15-30 ℃; and/or
In the step S20, the reaction time of the carbon dioxide and the meta-aluminate solution is 10S to 3000S.
10. The method for preparing pseudo-boehmite according to claim 8, comprising:
step S40: aging the solution containing pseudo-boehmite obtained in the step S20 to obtain an aging solution, preferably at a temperature of 10 ℃ to 75 ℃ for more than 0 hours and less than or equal to 5 hours.
11. The method for preparing pseudo-boehmite according to any one of claims 8-10, characterized in that in said step S00 the carbon dioxide is introduced in an amount of 0.5L/min-5L/min; and/or
In the step S00, the concentration of the meta-aluminate solution is 10g/L to 300g/L.
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