CN113797856A - Supergravity rotating fluidized field enhanced liquid-solid adsorption equipment and method - Google Patents
Supergravity rotating fluidized field enhanced liquid-solid adsorption equipment and method Download PDFInfo
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- CN113797856A CN113797856A CN202111115121.7A CN202111115121A CN113797856A CN 113797856 A CN113797856 A CN 113797856A CN 202111115121 A CN202111115121 A CN 202111115121A CN 113797856 A CN113797856 A CN 113797856A
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- 239000003463 adsorbent Substances 0.000 claims abstract description 35
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- 239000003054 catalyst Substances 0.000 claims description 26
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 26
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- 239000002351 wastewater Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention provides a supergravity rotating fluidized field strengthening liquid-solid adsorption device and a method, the device comprises a rotating bed and a fluidized bed, wherein the rotating bed comprises a shell, a liquid inlet pipe, a liquid distributor, a liquid outlet pipe and a driving mechanism; a filling column is arranged in the shell, an adsorbent or a carrier is filled in the filling column, the bottom surface of the filling column is of a porous structure, and the pore diameter is smaller than the particle size of the adsorbent or the carrier; the liquid inlet pipe penetrates from the top of the shell; the liquid distributor is inserted in the adsorbent or the carrier and is communicated with the liquid inlet pipe; the liquid outlet pipe penetrates from the bottom of the shell; the driving mechanism is used for driving the filling column to rotate; the fluidized bed is connected to the bottom of the housing through a gas inlet. The invention can effectively solve the problems in the traditional process.
Description
Technical Field
The invention belongs to the technical field of liquid-solid adsorbents and catalysts prepared by an impregnation method, and particularly relates to a supergravity rotating fluidized field enhanced liquid-solid adsorption device and method.
Background
The supported catalyst is the most widely used catalyst at present, generally consists of a carrier and an active component, and the impregnation method is the most common preparation method of the catalyst. The impregnation method is to use a porous carrier as a substrate, realize the loading of active components on the surface of the porous carrier by means of chemical bond force and external force, and complete the preparation of the catalyst through the procedures of mixing, drying, molding, impregnation, roasting decomposition, sieving, packaging and the like. The performance of the shaped catalyst is not only closely connected with the carrier structure, but also has a certain relation with the treatment mode in the dipping process. In the whole dipping process, the selection of the dipping equipment becomes an important link of the whole process, the common dipping equipment comprises a stirring kettle and a fluidized bed, the stirring kettle is found to be uneven in self stirring, the dispersibility of active components is poor, the stirring is limited, the loading capacity of a carrier cannot reach the optimum in the actual operation process, the fluidized bed is applied to solve the problem, the dipping equipment is the most widely used dipping equipment in the industry, and dipping liquid is in contact with a fluidized carrier, so that the contact force and probability of the two phases are effectively increased. However, in the dipping process of the fluidized bed, the active components on the surface of the carrier are easy to fall off due to the fact that the collision degree between the carriers is increased, and the optimal dispersion of the active components is not achieved. The equipment updating and the process improvement are both used for improving the loading capacity and the dispersity of the active components. In the actual production process, the production of the supported catalyst not only needs to keep higher loading amount, but also has simple whole process requirement and high production capacity. Therefore, it is urgently needed to develop a catalyst production device which is suitable for mass production and has excellent loading performance.
Disclosure of Invention
The traditional impregnation method for preparing the catalyst has the following problems: the catalyst prepared by the stirring kettle has low load and uneven distribution of active components; the problems that the carrier collision is serious, the active components are easy to fall off and the like in the fluidized bed process are solved; the catalyst prepared by the rotary bed impregnation method has a weak expanded state of the carrier and insufficient local loading. Aiming at the problems, the invention provides a supergravity rotating fluidized field enhanced liquid-solid adsorption device and a supergravity rotating fluidized field enhanced liquid-solid adsorption method, which are used for preparing a supported catalyst by an impregnation method and effectively solve the problems in the traditional process.
In order to achieve the purpose, the invention provides a supergravity rotating fluidized field strengthening liquid-solid adsorption device, which comprises a rotating bed and a fluidized bed, wherein the rotating bed comprises a shell, a liquid inlet pipe, a liquid distributor, a liquid outlet pipe and a driving mechanism; a filling column is arranged in the shell, an adsorbent or a carrier is filled in the filling column, the bottom surface of the filling column is of a porous structure, and the pore diameter is smaller than the particle size of the adsorbent or the carrier; the liquid inlet pipe penetrates from the top of the shell; the liquid distributor is inserted in the adsorbent or the carrier and is communicated with the liquid inlet pipe; the liquid outlet pipe penetrates from the bottom of the shell; the driving mechanism is used for driving the filling column to rotate; the fluidized bed is connected to the bottom of the housing through a gas inlet.
Further, the liquid distributor is in a 'king' shape, radial spraying is conducted, and the radial length of the liquid distributor is smaller than the radius of the filling column.
Further, the bottom surface of the filling column is an upward convex conical surface.
Further, the gas inlet is arranged symmetrically along the radial direction of the shell, and the gas inlet is provided with a regulating valve.
Further, the driving mechanism comprises a motor and a rotating shaft; the rotating shaft is rotatably connected with the shell through a bearing and is fixedly connected with the filling column.
Further, solid particles are filled in the filling column, the solid particles are active carbon, active alumina, molecular sieves or silica gel, and the solid particles are columnar or spherical; the rotating speed of the driving mechanism is 0-1500 r/min; the gas in the fluidized bed is inert gas nitrogen.
The invention also provides a method for strengthening liquid-solid adsorption by the supergravity rotating fluidized field, which is implemented by adopting the supergravity rotating fluidized field strengthening liquid-solid adsorption equipment, wherein the equipment is used by coupling a rotating bed and a fluidized bed, the impregnation process is completed by two strengthening means, and the impregnation mode comprises a rotating mode, a fluidizing mode and a coupling mode:
1) in the rotating mode, the rotating bed works, the fluidized bed does not work, the filling column is filled with the adsorbent or the carrier, the impregnation liquid enters the filling column from the liquid distributor, the driving mechanism drives the filling column to rotate, and the adsorbent or the carrier is in a high-speed rotating state in the impregnation process to finish the impregnation process;
2) in the fluidization mode, the fluidized bed works, the rotating bed does not work, gas enters the rotating bed from the fluidized bed through the gas inlet, and contacts with the adsorbent or the carrier through the porous structure on the bottom surface of the filling column, so that the adsorbent or the carrier is in an expansion state, and the fluidization process is completed;
3) and in the coupling mode, the rotating bed and the fluidized bed work, and in the dipping process, the two modes are coupled to realize a super-gravity rotating fluidized state.
Further, the apparatus is used for preparing a supported catalyst or adsorbing resorcinol wastewater.
Further, the supported catalyst is prepared by using the equipment, active carbon with the particle size of 2mm is used as a carrier, 0.5% copper and manganese salt solution is used as an impregnation liquid, the loading amount of the active carbon is 80g, the flow rate of the impregnation liquid is 150-240L/h, the rotating speed of a rotating bed is 1000r/min, the impregnation time is 15min, the temperature is controlled to be 30 ℃, and the impregnation liquid is circular impregnation.
Further, the equipment is used for adsorbing resorcinol wastewater, active carbon with the particle size of 2mm is used as an adsorbent, the loading amount is 100g, the flow rate of resorcinol liquid is 160L/h, the rotating speed of a rotating bed is 900r/min, the initial concentration of resorcinol is 1300mg/L, the temperature is 20 ℃, and the time is 30 min.
The invention has the following advantages:
the invention is the coupling of the rotating bed and the fluidized bed, the rotating bed is used as the dipping equipment in the whole dipping process, and the fluidized bed is additionally arranged, so that the efficient reinforced dipping of the adsorbent or the carrier in a high-speed rotating environment is realized. The invention relates to an impregnation process in the preparation of a catalyst by an impregnation method, and the subsequent processes such as drying, calcining and the like are required to be configured to complete the preparation of the catalyst. Compared with the traditional impregnation work, the supergravity rotating fluidized field reinforced liquid-solid adsorption equipment reinforced liquid-solid impregnation method is a semi-continuous process, active components in the impregnation liquid exist in a dispersed form in a rotating bed, the liquid-solid two-phase adsorption mass transfer is enhanced by realizing good atomization, so that the loading capacity is increased, the good distribution of the active components on a carrier is kept, and the fluidized bed device is arranged at the bottom of the rotating bed and is used for realizing the puffing state of the carrier in the rotating bed and further increasing the liquid-solid adsorption mass transfer. The invention is suitable for preparing the load type catalyst and is used for the working conditions of adsorbing waste water by the adsorbent and the like. The load type catalyst prepared by the method can effectively improve the load of the carrier on the active component, shortens the load time, has better dispersibility of the active component on the surface of the carrier, realizes good activity of the catalyst, improves the adsorption capacity of the adsorbent, and has certain engineering practical application significance.
Drawings
FIG. 1 is a schematic structural diagram of a supergravity rotating fluidized field enhanced liquid-solid adsorption apparatus;
FIG. 2 is a schematic structural view of a rotating bed;
FIG. 3 is a schematic diagram of a liquid distributor;
FIG. 4 is a schematic view of the structure of a fluidized bed.
In the figure: 1-a fluidized bed; 2-a housing; 3-a liquid inlet pipe; 4-a liquid distributor; 5-a liquid outlet pipe; 6-filling the column; 7-gas inlet; 8-motor.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a supergravity rotating fluidized field enhanced liquid-solid adsorption device which comprises a rotating bed and a fluidized bed 1, wherein the rotating bed comprises a shell 2, a liquid inlet pipe 3, a liquid distributor 4, a liquid outlet pipe 5 and a driving mechanism; a filling column 6 is arranged in the shell 2, an adsorbent or a carrier is filled in the filling column 6, the bottom surface of the filling column 6 is of a porous structure, the pore diameter is smaller than the particle diameter of the adsorbent or the carrier, liquid is ensured to flow out in time, and gas is effectively contacted with the adsorbent or the carrier; the liquid inlet pipe 3 penetrates from the top of the shell 2; the liquid distributor 4 is inserted in the adsorbent or the carrier and is communicated with the liquid inlet pipe 3; the liquid outlet pipe 5 penetrates from the bottom of the shell 2; the driving mechanism is used for driving the filling column 6 to rotate; the fluidized bed 1 is connected to the bottom of the housing 2 via a gas inlet 7.
Further, liquid distributor 4 is "king" font design, radially sprays, and liquid distributor 4 radial length is less than the radius of filling post 6.
Further, the bottom surface of the filling column 6 is an upwardly convex conical surface. The adsorbent or the carrier is stacked in a conical shape, so that the disturbance of solid particles is enhanced, and the discharge of absorption liquid or modified liquid is facilitated.
Further, the gas inlets 7 are symmetrically arranged along the radial direction of the housing 2, and the gas inlets 7 are provided with regulating valves for regulating the fluidization intensity of the fluidized bed 1.
Further, the driving mechanism includes a motor 8 and a rotating shaft; the rotating shaft is rotatably connected with the shell 2 through a bearing and is fixedly connected with the filling column 6, so that the filling column 6 is driven to rotate.
Further, solid particles are filled in the filling column 6, the solid particles are active carbon, active alumina, molecular sieves or silica gel, and the solid particles are columnar or spherical; the rotating speed of the driving mechanism is 0-1500 r/min; the gas in the fluidized bed 1 is inert gas nitrogen.
Example 2
The embodiment provides a method for strengthening liquid-solid adsorption by a hypergravity rotating fluidized field, which is implemented by adopting the hypergravity rotating fluidized field strengthening liquid-solid adsorption equipment, wherein the equipment is used by coupling a rotating bed and a fluidized bed 1, the impregnation process is completed by two strengthening means, and the impregnation mode comprises a rotation mode, a fluidization mode and a coupling mode:
1) in the rotating mode, the rotating bed works, the fluidized bed 1 does not work, the filling column 6 is filled with the adsorbent or the carrier, the impregnation liquid enters the filling column 6 from the liquid distributor 4, the driving mechanism drives the filling column 6 to rotate, and the adsorbent or the carrier is in a high-speed rotating state in the impregnation process to finish the impregnation process;
2) in the fluidization mode, the fluidized bed 1 works, the rotating bed does not work, gas enters the rotating bed from the fluidized bed 1 through the gas inlet 7, and contacts with the adsorbent or the carrier through the porous structure on the bottom surface of the filling column 6, so that the adsorbent or the carrier is in an expansion state, the fluidization state is realized, and the fluidization process is completed;
3) and in the coupling mode, the rotating bed and the fluidized bed 1 work, in the dipping process, the two modes are coupled, and the adsorbent or the carrier rotates at a high speed and is simultaneously swept by bottom gas, so that the super-gravity rotating fluidized state is realized.
Furthermore, the impregnation liquid is recycled, and the whole process is semi-batch operation.
Further, after the adsorption process is completed, the liquid is discharged from the liquid outlet pipe 5. The rotation intensity of the filling column 6 can be regulated and controlled by the motor 8, and the fluidized intensity of the adsorbent can be controlled by the gas velocity of the high-pressure gas.
Example 3
The above-described apparatus was used to prepare supported catalysts on a pilot scale. Active carbon with the particle size of 2mm is used as a carrier, and 0.5% of copper and manganese salt solution is used as impregnation liquid to prepare the transition metal catalyst. The filling amount of the activated carbon is 80g, the flow rate of the impregnation liquid is 150-240L/h, the rotating speed of the rotating bed is 1000r/min, the impregnation time is 15min, the temperature is controlled to be 30 ℃, and the impregnation liquid is circular impregnation. After the impregnated activated carbon is activated at high temperature, the preparation process is completed, and in the experimental process, the impregnation effect of the liquid-solid adsorption equipment enhanced by the rotating bed and the super-gravity rotating fluidized field is compared. The experimental result shows that the load capacity of the copper and the manganese of the load catalyst prepared by the rotating bed is 5.3 percent and 3.9 percent respectively; the supported catalyst prepared by the supergravity rotating fluidized field enhanced liquid-solid adsorption equipment has the copper loading of 7.2% and the manganese loading of 5.6%, which shows that the supergravity rotating fluidized field enhanced liquid-solid adsorption equipment can effectively improve the metal loading of the catalyst.
Example 4
The resorcinol wastewater is adsorbed by the equipment, activated carbon (the loading is 100 g) with the particle size of 2mm is used as an adsorbent, the flow rate of resorcinol liquid is 160L/h, the rotating speed of a rotating bed is 900r/min, the initial concentration of resorcinol is 1300mg/L, the temperature is 20 ℃, and the time is 30 min. The influence of the removal effect and the rotating speed of the enhanced liquid-solid adsorption equipment of the rotating bed and the hypergravity rotating fluidized field on the removal rate is investigated in the experimental process. The experimental result shows that under the same working condition, the removal rate of resorcinol by the supergravity rotating fluidized field reinforced liquid-solid adsorption equipment is 99%, and the removal rate of resorcinol by the rotating bed is 95.4%; in the supergravity rotating fluidized field strengthening liquid-solid adsorption equipment, the removal rate is increased along with the increase of the rotating speed.
The invention is not the best known technology.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A supergravity rotating fluidized field strengthening liquid-solid adsorption device comprises a rotating bed and a fluidized bed, and is characterized in that the rotating bed comprises a shell, a liquid inlet pipe, a liquid distributor, a liquid outlet pipe and a driving mechanism;
the shell is internally provided with a filling column, an adsorbent or a carrier is filled in the filling column, the bottom surface of the filling column is of a porous structure, and the pore diameter is smaller than the particle size of the adsorbent or the carrier;
the liquid inlet pipe penetrates from the top of the shell;
the liquid distributor is inserted in the adsorbent or the carrier and is communicated with the liquid inlet pipe;
the liquid outlet pipe penetrates from the bottom of the shell;
the driving mechanism is used for driving the filling column to rotate;
the fluidized bed is connected with the bottom of the housing through a gas inlet.
2. The apparatus of claim 1, wherein the liquid distributor is in a "king" shape design and is radially spraying, and the radial length of the liquid distributor is smaller than the radius of the packing column.
3. The apparatus of claim 2, wherein the bottom surface of the filling column is an upwardly convex conical surface.
4. The apparatus of claim 3, wherein the gas inlets are symmetrically arranged along the radial direction of the housing, and the gas inlets are provided with regulating valves.
5. The apparatus of claim 4, wherein the driving mechanism comprises a motor and a rotating shaft;
the rotating shaft is rotatably connected with the shell through a bearing and is fixedly connected with the filling column.
6. The supergravity rotating fluidized field reinforced liquid-solid adsorption equipment as claimed in claim 1, wherein solid particles are filled in the filling column, the solid particles are activated carbon, activated alumina, molecular sieves or silica gel, and the solid particles are in the form of columns or spheres;
the rotating speed of the driving mechanism is 0-1500 r/min;
the gas in the fluidized bed is inert gas nitrogen.
7. A method for strengthening liquid-solid adsorption by using a hypergravity rotating fluidized field is characterized in that the method is carried out by using the hypergravity rotating fluidized field strengthening liquid-solid adsorption equipment of any one of claims 1 to 6, the equipment is used by coupling a rotating bed and a fluidized bed, the impregnation process is completed by two strengthening means, and the impregnation mode comprises a rotating mode, a fluidizing mode and a coupling mode:
1) in the rotating mode, the rotating bed works, the fluidized bed does not work, the filling column is filled with the adsorbent or the carrier, the impregnation liquid enters the filling column from the liquid distributor, the driving mechanism drives the filling column to rotate, and the adsorbent or the carrier is in a high-speed rotating state in the impregnation process to finish the impregnation process;
2) in the fluidization mode, the fluidized bed works, the rotating bed does not work, gas enters the rotating bed from the fluidized bed through the gas inlet, and contacts with the adsorbent or the carrier through the porous structure on the bottom surface of the filling column, so that the adsorbent or the carrier is in an expansion state, and the fluidization process is completed;
3) and in the coupling mode, the rotating bed and the fluidized bed work, and in the dipping process, the two modes are coupled to realize a super-gravity rotating fluidized state.
8. The method for strengthening liquid-solid adsorption of the hypergravity rotating fluidized field according to claim 7, characterized in that the equipment is used for preparing a supported catalyst or adsorbing resorcinol wastewater.
9. The method for strengthening liquid-solid adsorption of the supergravity rotating fluidized field according to claim 8, wherein the apparatus is used to prepare a supported catalyst, activated carbon with a particle size of 2mm is used as a carrier, a 0.5% solution of copper and manganese salts is used as an impregnation solution, the loading amount of the activated carbon is 80g, the flow rate of the impregnation solution is 150-240L/h, the rotation speed of the rotating bed is 1000r/min, the impregnation time is 15min, the temperature is controlled to be 30 ℃, and the impregnation solution is a circulating impregnation.
10. The method for strengthening liquid-solid adsorption of the supergravity rotating fluidized field according to claim 8, wherein the equipment is used for adsorbing resorcinol wastewater, activated carbon with the particle size of 2mm is used as an adsorbent, the loading capacity is 100g, the resorcinol liquid flow rate is 160L/h, the rotating bed rotating speed is 900r/min, the initial concentration of resorcinol is 1300mg/L, the temperature is 20 ℃, and the time is 30 min.
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