CN114522632A - Preparation device and preparation method of pseudo-boehmite - Google Patents

Preparation device and preparation method of pseudo-boehmite Download PDF

Info

Publication number
CN114522632A
CN114522632A CN202011230431.9A CN202011230431A CN114522632A CN 114522632 A CN114522632 A CN 114522632A CN 202011230431 A CN202011230431 A CN 202011230431A CN 114522632 A CN114522632 A CN 114522632A
Authority
CN
China
Prior art keywords
carbon dioxide
pseudoboehmite
inlet
aging
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202011230431.9A
Other languages
Chinese (zh)
Other versions
CN114522632B (en
Inventor
苏海霞
史建公
杨柳
任靖
王博
殷喜平
谭伟
王赫鹏
张南
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Sinopec Catalyst Co
Original Assignee
China Petroleum and Chemical Corp
Sinopec Catalyst Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp, Sinopec Catalyst Co filed Critical China Petroleum and Chemical Corp
Priority to CN202011230431.9A priority Critical patent/CN114522632B/en
Publication of CN114522632A publication Critical patent/CN114522632A/en
Application granted granted Critical
Publication of CN114522632B publication Critical patent/CN114522632B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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

Landscapes

  • 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 of pseudo-boehmite and a preparation method of pseudo-boehmite, wherein the preparation device comprises a pseudo-boehmite reactor which is provided with a meta-aluminate inlet for entering a meta-aluminate solution and a carbon dioxide inlet for entering carbon dioxide, a reaction chamber for reacting meta-aluminate and 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 discharge port for discharging the solution containing the pseudo-boehmite obtained by the reaction; the reaction chamber is internally provided with a distributor which uniformly distributes the carbon dioxide entering from the carbon dioxide inlet into the reaction chamber. The preparation device realizes the generation of the 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 metaaluminate solution; the carbon dioxide reacts with the metaaluminate solution to obtain a solution containing the pseudoboehmite.

Description

Preparation device and preparation method of pseudo-boehmite
Technical Field
The invention relates to the technical field of compound preparation, in particular to a preparation device and a preparation method of pseudo-boehmite.
Background
The pseudo-boehmite has the characteristics of high specific surface area, large pore volume, good molding property, good peptization thixotropic property and the like, and can be widely used as a drying agent, an adsorbent, a molding binder, a catalyst carrier, a raw material for preparing active alumina and the like in the petrochemical industry.
The method for producing pseudoboehmite mainly comprises an aluminum alkoxide hydrolysis method and a neutralization method. The preparation of pseudo-boehmite by carbonization method relies on the technological process of producing alumina by sintering method, and the intermediate product NaAlO is utilized2Solution and CO2The waste gas is used as a reaction raw material, the process route with the lowest cost is provided, the waste liquid in the production can be returned to the alumina production flow for reuse, no waste material is discharged basically, the environmental pollution is small, the process is simple, and the method has competitive advantages and promising 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 ensure that the reaction for synthesizing the pseudo-boehmite is carried out stably and uniformly.
In order to achieve the above object, the present invention provides an apparatus for preparing pseudoboehmite, comprising a pseudoboehmite reactor, wherein the pseudoboehmite reactor is provided with a meta-aluminate inlet for allowing a meta-aluminate solution to enter and a carbon dioxide inlet for allowing carbon dioxide to enter, a reaction chamber for allowing meta-aluminate to react with carbon dioxide to obtain a solution containing the pseudoboehmite is arranged in the pseudoboehmite reactor, and the pseudoboehmite reactor is provided with a product discharge port for discharging the solution containing the pseudoboehmite obtained by the reaction; the preparation device of the pseudo-boehmite further comprises a distributor arranged in the reaction chamber, and the distributor is arranged to uniformly distribute the carbon dioxide entering from the carbon dioxide inlet into the reaction chamber.
The preparation device of the pseudo-boehmite realizes the generation of the pseudo-boehmite and can ensure that the reaction for synthesizing the pseudo-boehmite is carried out stably and uniformly.
Preferably, the distributor including set up in the distribution pipe in the reaction chamber, the distribution pipe be provided with the distribution pipe import that the carbon dioxide import is linked together, be provided with a plurality of distribution holes on the distribution pipe, it is a plurality of distribution hole evenly distributed in the distribution pipe.
Preferably, the distributor comprises a distribution plate arranged in the reaction chamber, the distribution plate is provided with a plurality of distribution openings, the distribution openings are uniformly distributed on the distribution plate, and the distribution plate is arranged at the downstream position of the carbon dioxide inlet along the flow direction of the carbon dioxide.
Preferably, the preparation device of the pseudo-boehmite comprises a liquid distribution plate arranged in the reaction chamber, the liquid distribution plate is arranged between the distribution plate and the metaaluminate inlet, a plurality of liquid inlets for the metaaluminate solution to pass through are arranged on the liquid distribution plate, and the plurality of liquid inlets are uniformly arranged on the liquid distribution plate.
Preferably, the preparation device of the pseudoboehmite comprises a first storage tank, a first storage chamber capable of containing metaaluminate solution is arranged in the first storage tank, the first storage tank is provided with a first discharge port for discharging the metaaluminate solution out of the first storage chamber, and the first discharge port is communicated with the metaaluminate inlet.
Preferably, the preparation device of the pseudo-boehmite comprises a second storage tank, a second storage chamber capable of containing carbon dioxide is arranged in the second storage tank, the second storage tank is provided with a second discharge port for discharging the carbon dioxide out of the second storage chamber, and the second discharge port is communicated with the carbon dioxide inlet; or
The preparation device of the pseudo-boehmite comprises a second storage tank, wherein a second storage chamber capable of containing carbon dioxide is arranged in the second storage tank, the second storage tank is provided with a second discharge port for discharging the carbon dioxide out of the second storage chamber, the second discharge port is communicated with the carbon dioxide inlet, and the second storage tank is provided with a diluent gas inlet for allowing diluent gas for adjusting the concentration of the carbon dioxide to enter.
Preferably, the preparation device of the pseudo-boehmite comprises an aging tank, an aging chamber is arranged in the aging tank, the aging tank is provided with an aging inlet and an aging outlet for discharging aged aging liquid, wherein:
the aging inlet is communicated with the product discharge port.
Preferably, the apparatus for preparing pseudoboehmite comprises a separation scrubber arranged at the downstream of the aging tank, and the separation scrubber is arranged to receive the aged pseudoboehmite-containing solution discharged from the aging tank and wash and separate the solution.
Preferably, the apparatus for preparing pseudoboehmite comprises a dryer disposed downstream of the separator-scrubber, the dryer being disposed to be able to receive the pseudoboehmite-containing mixture discharged from the separator-scrubber and dry the mixture.
The second aspect of the present invention provides a method for preparing pseudoboehmite, comprising:
step S00: so that the carbon dioxide is uniformly distributed in the metaaluminate solution;
step S20: the carbon dioxide reacts with the metaaluminate solution to obtain a solution containing the pseudoboehmite.
Preferably, in the step S20, the carbon dioxide and the metaaluminate solution are reacted at 15 ℃ to 30 ℃; and/or
In the step S20, the reaction time of the carbon dioxide and the metaaluminate solution is 10S to 3000S.
Preferably, the preparation method of the pseudoboehmite comprises the following steps:
step S40: and aging the solution containing the pseudoboehmite obtained in the step S20 to obtain an aging solution, wherein the aging temperature is preferably 10-75 ℃, and the aging time is preferably more than 0 hour and less than or equal to 5 hours.
Preferably, in the step S00, the introduction amount of the carbon dioxide is 0.5L/min-5L/min; and/or
In the step S00, the concentration of the metaaluminate solution is 10g/L-300 g/L.
Drawings
FIG. 1 is a schematic view showing the overall construction of an apparatus for preparing pseudoboehmite according to a preferred embodiment of the present invention;
FIG. 2 is a schematic sectional view showing the structure of an apparatus for preparing pseudoboehmite according to another preferred embodiment of the present invention;
FIG. 3 is a schematic view showing the overall construction of an apparatus for preparing pseudoboehmite according to a preferred embodiment of the present invention;
FIG. 4 is an XRD spectrum of the corresponding product obtained in example, wherein curve 1 shows an XRD spectrum of a product containing pseudoboehmite and alumina trihydrate, and curve 2 shows an XRD spectrum of a product containing pseudoboehmite and dawsonite (NaAlCO)3(OH)2) The XRD spectrum of the product of (1), curve 3 represents the XRD spectrum of the product containing only pseudoboehmite; bottom labeling of chemistryThe three peak groups of formula (I) represent the standard spectra of the corresponding compounds.
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 delivery pump; 14-a second storage tank; 140-a second storage chamber; 14 a-a flow controller; 16-pseudo-boehmite reactor; 160-a reaction chamber; 162-reaction stirring slurry; 164-metaaluminate inlet; 166-a carbon dioxide inlet; 168-product discharge; 169-vent; 180-distribution pipes; 182-a distribution plate; 19-liquid distribution plate; 20 a-an aging tank; 200 a-an aging chamber; 202-aging and stirring; 20 b-a separator scrubber; 20 c-a dryer; 22 a-a first delivery duct; 22 b-a first buffer tank; 22 c-a first pressure gauge; 22 d-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-a second flow controller; 26-a thermostat; 26 a-a third delivery pipe; 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, the use of directional terms such as "upper, lower, left and right" in the absence of a contrary explanation generally means that the directions shown in the drawings and the practical application are considered to be the same, and "inner and outer" mean the inner and outer of the outline of the component.
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 therein with a reaction chamber 160 for reacting a meta-aluminate with carbon dioxide to obtain a solution containing pseudo-boehmite, it being understood that a meta-aluminate inlet 164 and a carbon dioxide inlet 166 are both in communication with the pseudo-boehmite reactor 16; the pseudo-boehmite reactor 16 is provided with a product discharge port 168 for discharging the solution containing the pseudo-boehmite obtained by the reaction, the product discharge port 168 is communicated with the reaction chamber 160, the product discharge port 168 can be arranged at the bottom of the pseudo-boehmite reactor 16, and the product discharge port 168 can also be arranged at the top of the pseudo-boehmite reactor 16; the distributor is arranged in the reaction chamber 160, the distributor is arranged to uniformly distribute the 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 also 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, so that the reaction can be uniformly and stably carried out. Wherein the meta-aluminate solution comprises a sodium meta-aluminate solution. It will be appreciated that the metaaluminate solution may be heated to a predetermined temperature whereby the reaction between the carbon dioxide and the metaaluminate may be carried out at a suitable temperature and, in addition, the pseudoboehmite reactor 16 may be subjected to a heated atmosphere such that the reaction between the carbon dioxide and the metaaluminate may be carried out at a moderate temperature. In addition, the reaction gives a solution containing pseudoboehmite 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 communicated 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, for example, the 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 the periphery of the carbon dioxide inlet 166, a plurality of distribution holes may be disposed on the distribution pipe 180, the plurality of distribution holes may be uniformly distributed in the distribution pipe 180, and thus, the carbon dioxide entering the distribution pipe 180 may be uniformly distributed within the reaction chamber 160 through the uniformly arranged 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 a meta-aluminate solution may enter the reaction chamber 160 through the meta-aluminate inlet 164.
As shown in fig. 2, the distributor includes a distribution plate 182 disposed in the reaction chamber 160, the distribution plate 182 has a plurality of distribution ports, the plurality of distribution ports may be uniformly distributed on the distribution plate 182, and the distribution plate 182 may be disposed at a position downstream of the carbon dioxide inlet 166 in the flow direction of 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 metaaluminate solution, thereby ensuring that the reaction is uniformly and stably performed.
The carbon dioxide inlet 166 may be disposed at the bottom wall of the pseudo-boehmite reactor 16, the meta-aluminate inlet 164 may be disposed at the top of the pseudo-boehmite reactor 16, the 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 parts distributed along the height direction of the pseudo-boehmite reactor 16. Alternatively, the carbon dioxide inlet 166 may be provided in the top wall of the pseudo-boehmite reactor 16 and the meta-aluminate solution may be provided in the 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, the 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 the product obtained by the reaction and the quality of the product can be improved. The product outlet 168 may be located in the sidewall 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 metaaluminate inlet 164, and a plurality of liquid inlets through which a metaaluminate solution passes may be disposed on the liquid distribution plate 19, and the liquid distribution plate 19 may be uniformly disposed on the liquid distribution plate 19, it being 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 metaaluminate solution can be uniformly distributed in the reaction chamber 160, and meanwhile, the speed of the metaaluminate solution entering the reaction chamber 160 can be properly controlled, so that the stability and uniformity of the reaction are further improved.
A plurality of liquid distribution plates 19 can be arranged between the distribution plate 182 and the metaaluminate inlet 164, and the plurality of liquid distribution plates 19 can be distributed at intervals along the height direction of the pseudo-boehmite reactor 16, so that the speed of the metaaluminate solution entering the reaction chamber 160 and the distribution uniformity of the metaaluminate solution can be better controlled.
As shown in fig. 1, a first storage tank 12 may be provided, a first storage chamber 120 capable of containing a metaaluminate solution may be provided in the first storage tank 12, the first storage tank 12 may be provided with a first discharge port for the metaaluminate solution to be discharged out of the first storage chamber 120, and the first discharge port may be communicated with the metaaluminate inlet 164. In order to enable better transfer of the metaaluminate solution into the pseudoboehmite reactor 16, a metaaluminate transfer pipe may be provided between the first discharge port and the metaaluminate inlet 164 and a transfer pump 12a may be provided on the metaaluminate transfer pipe, the transfer pump 12a may transfer the metaaluminate solution into the pseudoboehmite 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, and a second discharge port through which carbon dioxide is discharged out of the second storage chamber 140 may be provided in the second storage tank 14, and the second discharge port may be communicated with the carbon dioxide inlet 166.
A carbon dioxide transfer line 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 transfer line, the flow controller 14a controlling the amount of carbon dioxide entering the pseudoboehmite reactor 16.
A dilution gas inlet through which the dilution gas is introduced into the second storage chamber 140 may be provided on 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, and the inert gas may comprise nitrogen.
As shown in fig. 3, a first delivery pipe 22a capable of delivering the dilution gas may be provided on the dilution gas inlet; a first pressure gauge 22c capable of detecting the pressure of the diluent gas in the first delivery pipe 22a may be provided on the first delivery pipe 22 a; a first buffer tank 22b may be provided on the first delivery pipe 22a, the first buffer tank 22b being capable of containing 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, the dilution gas in the first delivery pipe 22a may be smoothly delivered by providing the first buffer tank 22b, 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 also 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 into which carbon dioxide enters may be provided in the second storage tank 14, and a second transport pipe 24a capable of transporting carbon dioxide may be provided in the air inlet; a second pressure gauge 24c capable of detecting the pressure of carbon dioxide in the second delivery pipe 24a may be provided on the second delivery pipe 24 a; a second buffer tank 24b may be provided on the second transport 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 the carbon dioxide to enter and exit, the carbon dioxide in the second transport pipe 24a may be smoothly transported by providing the second buffer tank 24b, and the second buffer tank 24b may be 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 transport 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 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 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 also be provided downstream of the second flow controller 24g in the flow direction of 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 carbon dioxide.
A third transport pipe 26a capable of transporting a metaaluminate solution may be provided between the first discharge port of the first storage tank 12 and the metaaluminate inlet 164; a thermostat 26 may be provided on the third delivery pipe 26a to maintain the metaaluminate solution at a preset temperature, it being understood that the thermostat 26 has a thermostatic inlet and a thermostatic outlet; a third filter 26d for filtering particles in the metaaluminate solution may be provided on the third transport pipe 26a, and the third filter 26d may be provided downstream of the thermostat 26 in the flow direction of the metaaluminate solution; a third flow controller 26g capable of controlling the flow rate of the metaaluminate solution in the third transport pipe 26a may be provided on the third transport pipe 26a, and the third flow controller 26g may be provided downstream of the third filter 26d in the flow direction of 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 rate 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 26 a; 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 metaaluminate solution.
Further, an aging tank 20a may be provided, an aging chamber 200a may be provided in the aging tank 20a, the aging tank 20a may be provided with an aging inlet and an aging outlet through which an aged aging liquid is discharged, wherein: the aging inlet may be in communication with the product discharge 168. After the solution containing pseudoboehmite obtained by the reaction enters the aging chamber 200a, the crystal of the pseudoboehmite continues to grow, thereby completing the growth of the crystal structure 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 chamber 200a may be provided with an aging paddle 202 for stirring, thereby further improving the aging effect.
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 to receive the aged pseudoboehmite-containing solution discharged from the aging tank 20a and wash and separate the solution, for example, the pseudoboehmite-containing solution may be filtered to obtain a solid product, while the separated solid product may be optionally washed with water. It is noted that the solid product is a mixture containing pseudoboehmite, in which alumina trihydrate (Al (OH)) may be mixed in addition to the pseudoboehmite3*3H2O) and/or dawsonite (NaAl (OH)2CO3)。
In addition, a dryer 20c may be provided downstream of the separation scrubber 20b, and the dryer 20c may be provided to be able to receive the pseudo-boehmite-containing mixture discharged from the separation scrubber 20b and dry the mixture. Wherein, the temperature during drying can be 10-100 ℃, more preferably, the temperature during drying can be 20-80 ℃, and more preferably, the temperature during drying can be 30-60 ℃; preferably, the drying time may be 10s to 4h, further preferably, the drying time may be 5min to 2.5h, still further preferably, the drying time may be 20min to 1 h.
The present invention also provides a method for preparing pseudoboehmite, preferably, a method for preparing diaspore using the apparatus 10 for preparing pseudoboehmite according to the present invention, the method for preparing pseudoboehmite comprising: step S00: so that the carbon dioxide is uniformly distributed in the metaaluminate solution; step S20: the carbon dioxide reacts with the metaaluminate solution to obtain a solution containing the pseudoboehmite.
In step S00, the amount of carbon dioxide introduced may be 0.5L/min-5L/min, and the reaction proceeds uniformly and smoothly by setting the amount of carbon dioxide introduced within the above range. Preferably, the introduction amount of the carbon dioxide can be 1L/min-3.5L/min; more preferably, the amount of carbon dioxide introduced may be 1L/min to 2.5L/min.
In step S00, the concentration of the metaaluminate solution may be 10g/L-300g/L, and the concentration of the metaaluminate solution is set within the above range, so that the reaction proceeds uniformly and smoothly. Preferably, the concentration of the metaaluminate solution can be 15-180 g/L; further preferably, the concentration of the metaaluminate solution can be 20-100 g/L; even more preferably, the concentration of the metaaluminate solution may be 20-80g/L, most preferably, the concentration of the metaaluminate solution may be 20-40 g/L. Wherein the meta-aluminate solution comprises sodium meta-aluminate. In step S20, the carbon dioxide and the metaaluminate solution may be reacted at 15 to 30 ℃, and the reaction may be performed in the above temperature range, so that the reaction therebetween 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 a sufficient reaction between the two to be carried out and ensures the reaction efficiency. Further preferably, the reaction time may be 50s to 1800s, and still further preferably, the reaction time may be 200s to 1500 s.
In step S20, the solution containing pseudoboehmite obtained by the reaction is in the form of a gel or slurry, the pH of the solution containing pseudoboehmite is preferably 7.5 to 10.5, and the pH of the solution containing pseudoboehmite is controlled within the above range, which is advantageous for improving the quality of the obtained product.
In addition, the inventor researches and discovers that when the concentration of the metaaluminate solution is more than or equal to 20g/L and less than 40g/L, the reaction can obtain a product basically containing the pseudoboehmite; when the concentration of the metaaluminate 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 reaction can obtain a product basically containing pseudoboehmite; when the concentration of the metaaluminate solution is not less than 40g/L and the pH 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 may include the step of aging the pseudo-boehmite-containing solution obtained in the step of S20 to obtain an aged solution, in step S40. Preferably, the solution containing pseudoboehmite is aged at a predetermined temperature to allow crystals of the product to grow, thereby obtaining a complete crystal structure.
Wherein, the aging temperature can be 10-75 ℃, thus improving the aging effect and the aging efficiency, and preferably, the aging temperature can be 15-60 ℃; in addition, the aging time can be more than 0 hour and less than or equal to 5 hours, so that the aging efficiency is improved, the energy consumption is reduced, and the aging effect is ensured.
The preparation method of the pseudoboehmite may include step S60, in which the obtained aging solution is separated and washed to obtain a solid product, which is described in the foregoing, and is not described herein again. Wherein, solid-liquid separation can be carried out by selecting a filtering mode, and in the separation process, the solid product can be washed by water.
The preparation method of the pseudoboehmite may include the step of drying the obtained solid product S80. Wherein, the temperature during drying can be 10-100 ℃, thereby not only ensuring the drying effect, but also basically not influencing the obtained solid product, further preferably, the temperature during drying can be 20-80 ℃, further preferably, the temperature during drying can be 30-60 ℃; in addition, the drying time may be 10s to 4h, further preferably, the drying time may be 5min to 2.5h, and still further preferably, the drying time may be 20min to 1 h.
In addition, the specific surface area of the prepared pseudo-boehmite can be 90-400m2·g-1The pore volume can be 0.2-2.0m3·g-1The pore diameter can be 3.0-20.0 nm. Therefore, the prepared pseudoboehmite has wider application range.
The effects of the present invention will be further described with reference to examples.
Examples
Examples 1 to 28
The preparation of the pseudo-boehmite is carried out by using the preparation device of the pseudo-boehmite shown in FIG. 1 and the preparation method of the pseudo-boehmite provided by the invention.
In each example, the amount of carbon dioxide introduced, the solution concentration of the metaaluminate solution, the reaction temperature of carbon dioxide and the metaaluminate solution, the aging temperature for aging the pseudoboehmite-containing solution obtained by the reaction, the aging time, the washing agent selected for separating and washing the obtained aged solution, the separation and washing temperature, and the drying temperature for drying the solid product obtained after separation and washing are shown in table 1 below.
TABLE 1
Figure BDA0002765013190000131
Figure BDA0002765013190000141
Test example
Test example 1
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 measured, and the results are shown in table 2 below.
TABLE 2
Figure BDA0002765013190000142
Figure BDA0002765013190000151
In table 2 above, "/" indicates that no correlation test was performed.
Test example two
XRD test is carried out on the solid product obtained in the example 4 to obtain a spectrogram shown as a curve 1 in a figure 4, and according to comparison with a standard spectrogram below, the solid product mainly contains pseudo-boehmite and alumina trihydrate; XRD test is carried out on the solid product obtained in the example 9, so as to obtain a spectrogram shown as a curve 2 in a figure 4, and according to comparison with a standard spectrogram below, the solid product mainly contains pseudo-boehmite and simultaneously contains dawsonite; XRD testing of the solid product obtained in example 1 gave the spectrum shown by curve 3 in figure 4, which was substantially pseudoboehmite, according to comparison 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, numerous simple modifications can be made to the technical solution of the invention, including combinations of the individual specific technical features in any suitable way. The invention is not described in detail in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.

Claims (13)

1. The preparation device of the pseudoboehmite is characterized in that the preparation device (10) of the pseudoboehmite comprises a pseudoboehmite reactor (16), the pseudoboehmite reactor (16) is provided with a meta-aluminate inlet (164) for a meta-aluminate solution to enter and a carbon dioxide inlet (166) for a carbon dioxide to enter, a reaction chamber (160) for a meta-aluminate to react with the carbon dioxide to obtain a solution containing the pseudoboehmite is arranged in the pseudoboehmite reactor (16), and the pseudoboehmite reactor (16) is provided with a product discharge port (168) for discharging the solution containing the pseudoboehmite obtained by the reaction; the preparation device (10) of the pseudoboehmite further comprises a distributor arranged in the reaction chamber (160), and the distributor is arranged to uniformly distribute the carbon dioxide entering from the carbon dioxide inlet (166) to the reaction chamber (160).
2. The preparation device of pseudo-boehmite according to claim 1, characterized in that the distributor comprises a distribution pipe (180) disposed 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 pseudoboehmite according to claim 1, characterized in that the distributor comprises a distribution plate (182) disposed in the reaction chamber (160), the distribution plate (182) is provided with a plurality of distribution ports, the plurality of distribution ports are uniformly distributed on the distribution plate (182), and the distribution plate (182) is disposed at a downstream position of the carbon dioxide inlet (166) in a flow direction of the carbon dioxide.
4. The preparation device of the pseudo-boehmite according to claim 3, characterized in that the preparation device (10) comprises a liquid distribution plate (19) arranged in the reaction chamber (160), the liquid distribution plate (19) is arranged between the distribution plate (182) and the metaaluminate inlet (164), and the liquid distribution plate (19) is provided with a plurality of liquid inlets for the passage of the metaaluminate solution, and the liquid inlets are uniformly arranged on the liquid distribution plate (19).
5. The apparatus for preparing pseudoboehmite according to claim 1, characterized in that the apparatus (10) comprises a first storage tank (12), a first storage chamber (120) capable of containing a metaaluminate solution is arranged in the first storage tank (12), the first storage tank (12) is provided with a first discharge port for discharging the metaaluminate solution from the first storage chamber (120), and the first discharge port is communicated with the metaaluminate inlet (164).
6. The apparatus for preparing pseudoboehmite according to claim 1, characterized in that the apparatus (10) for preparing pseudoboehmite comprises a second storage tank (14), a second storage chamber (140) capable of containing carbon dioxide is provided in the second storage tank (14), the second storage tank (14) is provided with a second discharge port through which carbon dioxide is discharged out of the second storage chamber (140), and the second discharge port is communicated with the carbon dioxide inlet (166); or
The preparation device (10) of the 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), the second storage tank (14) is provided with a second discharge port for discharging the carbon dioxide out of the second storage chamber (140), the second discharge port is communicated with a carbon dioxide inlet (166), and the second storage tank (14) is provided with a diluent gas inlet for entering a diluent gas for adjusting the concentration of the carbon dioxide.
7. The apparatus for preparing pseudoboehmite according to any one of claims 1-6, characterized in that the apparatus (10) for preparing pseudoboehmite comprises an aging tank (20a), an aging chamber (200a) is provided in the aging tank (20a), and the aging tank (20a) is provided with an aging inlet and an aging outlet through which an aged aging liquid is discharged, wherein:
the aging inlet is in communication with the product discharge outlet (168).
8. The apparatus for preparing pseudoboehmite according to claim 7, characterized in that the apparatus (10) for preparing pseudoboehmite comprises a separation scrubber (20b), the separation scrubber (20b) being disposed downstream of the aging tank (20a), and the separation scrubber (20b) being disposed so as to be able to receive the aged solution containing pseudoboehmite discharged from the aging tank (20a) and wash and separate the solution.
9. The apparatus for preparing pseudoboehmite according to claim 8, characterized in that the apparatus (10) for preparing pseudoboehmite comprises a dryer (20c) disposed downstream of the separation scrubber (20b), the dryer (20c) being disposed so as to be able to receive the mixture containing pseudoboehmite discharged from the separation scrubber (20b) and dry the mixture.
10. A preparation method of pseudoboehmite is characterized by comprising the following steps:
step S00: so that the carbon dioxide is uniformly distributed in the metaaluminate solution;
step S20: the carbon dioxide reacts with the metaaluminate solution to obtain a solution containing the pseudoboehmite.
11. The method of preparing pseudoboehmite according to claim 10, characterized in that in the step S20, the carbon dioxide and the metaaluminate solution are reacted at 15 ℃ -30 ℃; and/or
In the step S20, the reaction time of the carbon dioxide and the metaaluminate solution is 10S to 3000S.
12. The method of preparing pseudoboehmite according to claim 10, characterized in that it comprises:
step S40: and (3) aging the solution containing the pseudoboehmite obtained in the step (S20) to obtain an aging solution, wherein the aging temperature is preferably 10-75 ℃, and the aging time is preferably more than 0 hour and less than or equal to 5 hours.
13. The method for producing pseudoboehmite according to any one of claims 10-12, characterized in that in said step S00, the amount of carbon dioxide introduced is 0.5L/min-5L/min; and/or
In the step S00, the concentration of the metaaluminate solution is 10g/L-300 g/L.
CN202011230431.9A 2020-11-06 2020-11-06 Pseudo-boehmite preparation device and pseudo-boehmite preparation method Active CN114522632B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011230431.9A CN114522632B (en) 2020-11-06 2020-11-06 Pseudo-boehmite preparation device and pseudo-boehmite preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011230431.9A CN114522632B (en) 2020-11-06 2020-11-06 Pseudo-boehmite preparation device and pseudo-boehmite preparation method

Publications (2)

Publication Number Publication Date
CN114522632A true CN114522632A (en) 2022-05-24
CN114522632B CN114522632B (en) 2024-04-19

Family

ID=81618588

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011230431.9A Active CN114522632B (en) 2020-11-06 2020-11-06 Pseudo-boehmite preparation device and pseudo-boehmite preparation method

Country Status (1)

Country Link
CN (1) CN114522632B (en)

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0147167A2 (en) * 1983-12-22 1985-07-03 Aluminum Company Of America Continuous process for neutralization of aluminate solution to form gels and appartatus therefor
CN1356266A (en) * 2000-12-05 2002-07-03 中国石油化工股份有限公司 Process for preparing hydrated aluminium oxide
CN1398787A (en) * 2002-05-31 2003-02-26 中国石油化工集团公司 Prepn of gamma-alumina
CN2616525Y (en) * 2003-03-10 2004-05-19 中国石油化工股份有限公司 Reactor for preparing aluminium hydroxide
RU2355637C1 (en) * 2007-10-11 2009-05-20 Открытое акционерное общество "РУСАЛ Всероссийский Алюминиево-магниевый Институт" Carboniser of aluminate solutions
CN202621146U (en) * 2012-04-24 2012-12-26 常州华狮化工有限公司 Novel tower
CN203540517U (en) * 2013-10-29 2014-04-16 中国石油化工股份有限公司 Liquid distributor and reaction kettle
CN105347375A (en) * 2015-11-20 2016-02-24 中石化催化剂（北京）有限公司 Production device of pseudo-boehmite and method thereof
CN205182696U (en) * 2015-11-17 2016-04-27 麦森能源科技有限公司 Bubbling reactor
CN106268539A (en) * 2015-05-21 2017-01-04 中国石化工程建设有限公司 Gas-liquid distributor for fluidized bed reactor
CN207287376U (en) * 2017-09-08 2018-05-01 江苏嘉隆化工有限公司 Gas distributor
CN208839568U (en) * 2018-08-31 2019-05-10 山东裕源集团有限公司 Mixing reactor is used in a kind of production of bromine
CN111468047A (en) * 2020-04-23 2020-07-31 河南兴浩新材料科技股份有限公司 Continuous preparation method of aluminum sol
CN211159747U (en) * 2019-10-23 2020-08-04 新疆甘泉堡企业服务有限公司 Process synthesis system of high-purity pseudo-boehmite

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0147167A2 (en) * 1983-12-22 1985-07-03 Aluminum Company Of America Continuous process for neutralization of aluminate solution to form gels and appartatus therefor
CN1356266A (en) * 2000-12-05 2002-07-03 中国石油化工股份有限公司 Process for preparing hydrated aluminium oxide
CN1398787A (en) * 2002-05-31 2003-02-26 中国石油化工集团公司 Prepn of gamma-alumina
CN2616525Y (en) * 2003-03-10 2004-05-19 中国石油化工股份有限公司 Reactor for preparing aluminium hydroxide
RU2355637C1 (en) * 2007-10-11 2009-05-20 Открытое акционерное общество "РУСАЛ Всероссийский Алюминиево-магниевый Институт" Carboniser of aluminate solutions
CN202621146U (en) * 2012-04-24 2012-12-26 常州华狮化工有限公司 Novel tower
CN203540517U (en) * 2013-10-29 2014-04-16 中国石油化工股份有限公司 Liquid distributor and reaction kettle
CN106268539A (en) * 2015-05-21 2017-01-04 中国石化工程建设有限公司 Gas-liquid distributor for fluidized bed reactor
CN205182696U (en) * 2015-11-17 2016-04-27 麦森能源科技有限公司 Bubbling reactor
CN105347375A (en) * 2015-11-20 2016-02-24 中石化催化剂（北京）有限公司 Production device of pseudo-boehmite and method thereof
CN207287376U (en) * 2017-09-08 2018-05-01 江苏嘉隆化工有限公司 Gas distributor
CN208839568U (en) * 2018-08-31 2019-05-10 山东裕源集团有限公司 Mixing reactor is used in a kind of production of bromine
CN211159747U (en) * 2019-10-23 2020-08-04 新疆甘泉堡企业服务有限公司 Process synthesis system of high-purity pseudo-boehmite
CN111468047A (en) * 2020-04-23 2020-07-31 河南兴浩新材料科技股份有限公司 Continuous preparation method of aluminum sol

Also Published As

Publication number Publication date
CN114522632B (en) 2024-04-19

Similar Documents

Publication Publication Date Title
CN101125665B (en) Method for preparing SAPO-34 molecular sieve by liquid phase crystallization method
US20070012183A1 (en) Method and apparatus for the continuous preparation of porous materials and mixed metal oxides using continuous stirred reactors
CN108793185A (en) A kind of preparation method of nano-ZSM-5 molecular sieve
CN113149026B (en) Preparation method of molecular sieve with stepped hole structure
JP6346188B2 (en) Method and apparatus for making zeolite
CN107827121B (en) Synthesis method of SAPO-34 molecular sieve with high specific surface area
CN107082436A (en) A kind of preparation method of mesoporous micro porous molecular sieve
CN110759356A (en) Preparation method of coal gangue-based oriented multi-stage pore ZSM-5 molecular sieve membrane material
CN114522632B (en) Pseudo-boehmite preparation device and pseudo-boehmite preparation method
CN101974031A (en) Glyphosate reaction filter method and special filter for glyphosate thereof
CN107285333A (en) A kind of method that Fast back-projection algorithm AEI molecular sieves are heated with microwave
CN110229074A (en) A kind of preparation method of N- benzyloxycarbonyl group -2- amino -1- propyl alcohol
CN107297220A (en) A kind of worm meso-porous Al2O3/ molecular sieves compound material and preparation method thereof
CN110642278B (en) Method for preparing aluminum hydroxide
CN110734511B (en) Polyolefin catalyst with spherical double-mesoporous composite material as carrier, polyolefin and preparation methods of polyolefin catalyst and polyolefin
CN114247411B (en) Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation
CN112551565A (en) Carbonizing device and method for producing macroporous pseudo-boehmite by carbonization method
CN114314607A (en) MCM-22 molecular sieve, preparation method thereof and benzene alkylation reaction method adopting molecular sieve catalysis
CN111115669A (en) Method for generating solid product by gas-liquid reaction and method for continuously preparing pseudo-boehmite
CN110357124A (en) Multi-stage porous SAPO-34/SAPO-18 hands over interpromoting relation in five elements phase molecule sieve and preparation method and application
CN105753052A (en) Synthesis method of supported MoS2 catalyst
CN112723374A (en) NaY molecular sieve and synthesis method thereof
CN116037085B (en) Macroporous alumina carrier and preparation method thereof
CN106045809B (en) It is a kind of using prepared in slurry bed reactor for the reaction system and method for ethylene
CN110787765A (en) Reactor and method for preparing pseudo-boehmite

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant