CN112604624A - External circulation ammonification reaction experimental equipment and method for analyzing factors influencing external circulation ammonification reaction by using same - Google Patents
External circulation ammonification reaction experimental equipment and method for analyzing factors influencing external circulation ammonification reaction by using same Download PDFInfo
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Abstract
The invention discloses an external circulation ammonification reaction experimental facility and a method for analyzing factors influencing the external circulation ammonification reaction by using the same. The settling separator of the device is provided with a circulation inlet and a circulation outlet which are communicated with the interior of the settling separator, one end of the upper horizontal section of the lifting pipe is communicated with the circulation inlet, one end of the upper horizontal section of the return pipe is communicated with the circulation outlet, the circulating pump is arranged at the lower horizontal section of the lifting pipe, and the lifting pipe is also provided with an adjusting valve for adjusting the flow rate of the lifting pipe; the flow meter is arranged at the steam outlet; the gas distributor is arranged on the lifting pipe, and a gas ammonia nozzle is detachably arranged on the gas distributor; the riser is made of transparent materials, tracer particles are added into slurry of the riser, and the Laser emitter emits sheet light to a flow field of the riser and the sheet light is shot by a high-speed camera at a certain frequency. The invention researches the influence rule of different structural parameters and the interaction thereof on the characteristics of bubble induced turbulence, mass transfer reaction and ammonia escape rate, and provides guidance for the optimization design of the reactor.
Description
Technical Field
The invention relates to the technical field of phosphorus ammonia production, in particular to an external circulation ammonification reaction experimental facility and a method for analyzing factors influencing the external circulation ammonification reaction by using the same.
Background
The external circulation reactor is widely applied to industrial applications such as biochemistry, pharmacy, sewage treatment, ammonium phosphate production and the like due to simple structure, no internal components and good mixing performance. In the production of ammonium phosphate, wet-process phosphoric acid is mainly adopted, the impurity content is high, the slurry viscosity is high, the reaction of ammonia gas and phosphoric acid is insufficient, and the ammonia escape rate is high. One of the key factors determining the productivity of the external loop reactor is gas-liquid mass transfer, which can be improved by increasing the specific gas-liquid interface area or mass transfer coefficient, thereby increasing the productivity. Smaller bubble diameters, higher and more uniform radial gas fraction distributions result in increased interfacial area; enhancing turbulence can increase the frequency of surface renewal of the bubbles, thereby promoting higher mass transfer rates. The diameter and turbulence intensity of the bubbles depend on the dynamic characteristics of the flow field, and the fluid dynamic characteristics are mainly influenced by the reactor structure, including the diameter ratio of a downcomer to a riser, the length of a horizontal pipe, the structure of a distributor and the like. Although many scholars at home and abroad research the influence of the reactor structure on the flow and mass transfer characteristics of the reactor, the influence of a certain structural parameter is often researched, and the influence of the interaction of all parameters on the flow characteristics is not comprehensively considered; the reactor often has three phases of gas, liquid and solid, and mass transfer and reaction, so that the system is very complex, and the interaction, flow, mass transfer and reaction coupling mechanism of the three phases of gas, liquid and solid is still lack of deep research. The interaction between the bubbles is a key factor influencing flow field distribution and mass transfer reaction, and the research on the interaction can deeply research the gas-liquid two-phase mass transfer reaction mechanism and is beneficial to regulating and controlling the mass transfer reaction.
Disclosure of Invention
The invention aims to provide an experimental facility for the external circulation ammonification reaction with adjustable structural parameters and a method for analyzing factors influencing the external circulation ammonification reaction by using the experimental facility for the external circulation ammonification reaction with adjustable structural parameters.
The invention relates to an external circulation ammoniation reaction experimental facility, which comprises a sedimentation separator, a stirring device, a lifting pipe, a return pipe, a circulating pump, a gas distributor, a flowmeter, a Laser emitter and a high-speed camera;
the settling separator is provided with a circulation inlet and a circulation outlet which are communicated with the inside of the settling separator, the riser is of a [ type ], one end of the upper horizontal section of the riser is communicated with the circulation inlet, the other end of the upper horizontal section of the riser is detachably connected with the vertical section of the riser through a flange, the return pipe is of a ] type, one end of the upper horizontal section of the return pipe is communicated with the circulation outlet, the lower horizontal section of the return pipe is detachably connected with the lower horizontal section of the riser through a flange, the circulating pump is arranged on the lower horizontal section of the riser, and a regulating valve for regulating the flow of the riser is further arranged on a pipeline section of the riser between the gas distributor and the circulating pump;
the top of the settling separator is provided with a steam outlet, and the bottom of the settling separator is provided with a slurry outlet and a slag discharge port;
the flow meter is arranged at the steam outlet and used for detecting the flow of the escaped ammonia gas;
the gas distributor is arranged on the lifting pipe, and a gas ammonia nozzle is detachably arranged on the gas distributor;
the vertical section of the lifting pipe is also provided with a phosphoric acid inlet;
the riser is made of transparent materials, tracer particles are added into slurry of the riser, a Laser emitter emits sheet light to a flow field of the riser, and the tracer particles in the flow field reflect light rays which are shot at a certain frequency by a high-speed camera arranged on one side of a vertical section of the riser;
the stirring device is used for mixing and stirring the slurry in the sedimentation separator.
Further, the phosphoric acid inlet is positioned below the gas distributor.
Further, agitating unit includes driving piece, rotation axis and a plurality of blade, the vertical setting of rotation axis is in among the sedimentation separator, it is a plurality of the blade is installed around the rotation axis bottom, the top of rotation axis stretches out sedimentation separator with the driving piece transmission is connected, the driving piece drive the rotation axis drives the blade is rotatory.
Further, the circulation outlet is positioned above the circulation inlet.
Furthermore, the gas distributor comprises a gas inlet pipe, the gas outlet end of the gas inlet pipe penetrates through the vertical section of the lifting pipe and extends into the lifting pipe, the gas ammonia nozzle is arranged at the gas outlet end of the gas inlet pipe, and the gas ammonia nozzle is horizontally arranged and horizontally sprays gas.
Further, the gas ammonia nozzle includes the ring pipe, be equipped with the screw hole on the lateral wall on the ring pipe, be equipped with the external screw thread on the outer wall of the end of giving vent to anger of intake pipe, the end spiral of giving vent to anger of intake pipe is in the screw hole, and with the ring pipe is inside to be linked together, a plurality of first round holes have been seted up along its inner circumference to the ring pipe inboard, and is a plurality of the axis of first round hole all is located same horizontal plane and all passes the centre of a circle of ring pipe, a plurality of second round holes have been seted up along its outer circumference interval in the ring pipe outside, and is a plurality of the axis of second round hole all is located same horizontal plane.
Furthermore, the aperture of the first round holes and the second round holes is 0.2-1 mm.
Further, the gas ammonia nozzle includes the outlet duct, the intake pipe is located one of riser is served and is equipped with first venthole, be equipped with the second venthole on the outlet duct, a pot head of outlet duct is established in the intake pipe, the other end seals, the outlet duct just can be relative the intake pipe removes to adjust the horizontal distance between first venthole and the second venthole, first venthole and the jet-propelled of second venthole level.
A method for analyzing factors influencing an external circulation ammonification reaction uses the external circulation ammonification reaction experimental equipment, and comprises the following specific analysis steps:
and (3) result analysis step: the reactor operates, tracer particles are added into a steam port, a Laser emitter emits a piece of light to a flow field of a vertical section of a lifting pipe, the tracer particles in the flow field reflect light rays and are shot by a high-speed camera at a certain frequency, the shot liquid phase can be analyzed to obtain instantaneous flow field distribution by using a high-speed particle shooting technology, instantaneous flow field data are analyzed, speed pulsation of space and time is extracted, and bubble induced turbulence characteristics are analyzed; the time-average field distribution can be obtained by carrying out averaging processing; the shot bubble image is subjected to enhancement processing and converted into a binary image, the edge of the bubble is extracted, the particle size and the long-short axis ratio distribution of the bubble are obtained, and the position distribution of the bubble is further obtained; extracting image analysis data of a series of continuous moments to obtain an evolution rule of a bubble motion path, a particle size and a major-minor axis ratio, reading the flow of a steam outlet flowmeter, measuring the mass fraction of ammonia gas by using a nano reagent spectrophotometry, and calculating the ammonia escape rate;
the experimental steps are as follows:
when the gas ammonia nozzle comprises a circular ring pipe, replacing the circular ring pipe, wherein the first circular hole and the second circular hole of each circular ring pipe have different apertures and the other process conditions are the same, operating the reactor again, and repeating the analysis steps; researching the influence rule of the aperture during air injection on the characteristics of bubble induced turbulence, bubble rising path, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate;
when the gas ammonia nozzle comprises the gas outlet pipe, the distance between the first gas outlet hole and the second gas outlet hole is adjusted, other process conditions are the same, the reactor is operated again, the analysis steps are repeated, and the influence rule of the interaction relation of the parallel bubbles with different initial distances on the ammonia escape rate can be researched;
connecting pipelines with different lengths at the flange connection position of the other end of the upper horizontal section of the riser and the vertical section of the riser and the flange connection position of the lower horizontal section of the backflow pipe and the lower horizontal section of the riser, changing the lengths of the upper horizontal section of the riser and the lower horizontal section of the backflow pipe, operating the reactor again under the same other process conditions, repeating the analysis steps, and researching the influence rule of water with the lengths of the horizontal section of the riser and the horizontal section of the backflow pipe on bubble induced turbulence characteristics, bubble rising paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate;
changing the rotating speed of the stirring device, operating the reactor again under the same other process conditions, measuring the impurity quality and the ammonia escape rate of the material slag discharge port, and analyzing the influence rules of different rotating speeds on the settling separation efficiency and the ammonia escape rate;
changing the rotating speed of the circulating pump, operating the reactor again under the same other process conditions, repeating the analysis steps, and analyzing the influence rule of the rotating speed of the circulating pump on the bubble induced turbulence characteristic, the bubble ascending path, the particle size distribution, the long-short axial ratio distribution evolution, the mass transfer reaction and the ammonia escape rate;
changing the opening of the regulating valve, operating the reactor again under the same other process conditions, repeating the analysis steps, and researching the influence rules of different equivalent diameter ratios on bubble induced turbulence characteristics, bubble rising paths, particle size distribution, long-short axis ratio distribution evolution, mass transfer reaction and ammonia slip rate.
And further, changing the position of a circulating outlet, respectively arranging the position of the circulating outlet on a slag discharge port or the side wall of the sedimentation separator, when the circulating outlet is arranged on the side wall of the sedimentation separator, locating the circulating outlet above the circulating inlet, operating the reactor again under the same other process conditions, repeating the analysis steps, and analyzing the influence rule of the position of the circulating outlet on the bubble induced turbulence characteristic, the bubble rising path, the particle size distribution, the long-short axial ratio distribution evolution, the mass transfer reaction and the ammonia escape rate.
The external circulation ammoniation reaction experimental equipment can adjust the aperture of a gas ammonia spray head, adjust the distance between two holes of a distributor, adjust the lengths of an upper horizontal section of a lifting pipe and a lower horizontal section of a return pipe, change the opening of an adjusting valve to change the equivalent diameter ratio of the lifting pipe and a downcomer, adjust the rotating speed of a motor and change the position of a circulating outlet so as to research the influence rules of different structural parameters and the interaction thereof on bubble induced turbulence characteristics, bubble rising paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate, and provide guidance for the optimization design of a reactor.
Drawings
FIG. 1 is a schematic structural diagram of an experimental apparatus for an external loop ammonification reaction of the present invention;
FIG. 2 is a schematic structural diagram of a gas distributor and a gas ammonia nozzle of the experimental apparatus for external circulation ammonification reaction of the present invention;
FIG. 3 is an enlarged schematic view of the experimental apparatus for an external loop ammonification reaction of the present invention at A in FIG. 2;
fig. 4 is a schematic structural diagram of a gas distributor and a gas ammonia nozzle of another embodiment of the external loop ammoniation reaction experimental facility of the present invention.
1. A settling separator; 11. a circulation inlet; 12. a recycle outlet; 13. a steam outlet; 14. a slurry outlet; 15. a slag discharge port; 2. a stirring device; 21. a drive member; 22. a rotating shaft; 23. a blade; 3. a riser tube; 31. an upper horizontal section of the riser; 32. a vertical section of riser; 33. a lower horizontal section of the riser; 34. a flange; 35. adjusting a valve; 36. a phosphoric acid inlet; 4. a return pipe; 41. an upper horizontal section of the return pipe; 42. a lower horizontal section of the return pipe; 5. a circulation pump; 6. a gas distributor; 61. A gas ammonia nozzle; 611. a circular ring tube; 6111. a threaded hole; 6112. a first circular hole; 6113. a second circular hole; 612. an air outlet pipe; 6121. a second air outlet; 62. an air inlet pipe; 621. a first air outlet hole; 7. a flow meter; 8. a Laser emitter; 9. high-speed cameras.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
As shown in fig. 1, the experimental apparatus for the external circulation ammonification reaction of the present invention comprises a sedimentation separator 1, a stirring device 2, a riser 3, a return pipe 4, a circulation pump 5, a gas distributor 6, a flow meter 7, a Laser emitter 8 and a high-speed camera 9;
the settling separator 1 is provided with a circulation inlet 11 and a circulation outlet 12 which are communicated with the inside of the settling separator, the lifting pipe 3 is in a [ shape ], one end of an upper horizontal section 31 of the lifting pipe is communicated with the circulation inlet 11, the other end of the upper horizontal section 31 of the lifting pipe is detachably connected with a vertical section 32 of the lifting pipe through a flange 34, the return pipe 4 is in a ] shape, one end of an upper horizontal section 41 of the return pipe is communicated with the circulation outlet 12, a lower horizontal section 42 of the return pipe is detachably connected with a lower horizontal section 33 of the lifting pipe through the flange 34, the circulating pump 5 is arranged at the lower horizontal section 33 of the lifting pipe, and a regulating valve 35 for regulating the flow of the lifting pipe 3 is further arranged on a pipe section;
the top of the sedimentation separator 1 is provided with a steam outlet 13, and the bottom of the sedimentation separator 1 is provided with a slurry outlet 14 and a slag discharge port 15;
the flow meter 7 is arranged at the steam outlet 13 and is used for detecting the flow of the escaped ammonia gas;
the gas distributor 6 is arranged on the lifting pipe 3, and a gas ammonia nozzle 61 is detachably arranged on the gas distributor 6;
the vertical section 32 of the riser is also provided with a phosphoric acid inlet 36;
the lifting pipe 3 is made of transparent materials, tracer particles are added in slurry of the lifting pipe 3, the Laser emitter 8 emits light sheets to a flow field of the lifting pipe 3, the tracer particles in the flow field reflect light rays, and the light rays are shot at a certain frequency by a high-speed camera 9 arranged on one side of a vertical section 32 of the lifting pipe;
the stirring device 2 is used for mixing and stirring the slurry in the sedimentation separator 1.
The phosphoric acid inlet 36 is located below the gas distributor 6.
The experimental equipment for the external circulation ammoniation reaction can adjust the aperture of a gas ammonia spray head, adjust the distance between two holes of a distributor, adjust the lengths of an upper horizontal section 31 of a lifting pipe and a lower horizontal section 42 of a return pipe, change the opening degree of an adjusting valve 35 to change the equivalent diameter ratio of the lifting pipe 3 and a downcomer, adjust the rotating speed of a motor and change the position of a circulating outlet 12, so as to research the influence rules of different structural parameters and the interaction thereof on bubble induced turbulence characteristics, bubble rising paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate, and provide guidance for the optimization design of the reactor.
The structure of the stirring device 2 is various, and is not limited herein, in this embodiment, the stirring device 2 may include a driving member 21, a rotating shaft 22, and a plurality of blades 23, the rotating shaft 22 is vertically disposed in the sedimentation separator 1, the plurality of blades 23 are installed around the bottom end of the rotating shaft 22, the top end of the rotating shaft 22 extends out of the sedimentation separator 1 and is in transmission connection with the driving member 21, the driving member 21 drives the rotating shaft 22 to drive the blades 23 to rotate, the driving member 21 may be a motor, and the rotating speed of the motor may be adjusted, so as to adjust the rotating speed of the rotating shaft 22 and the rotating speed of the blades 23, so that the fluid in the sedimentation separator 1 generates forced cyclone, enhance the turbulent motion of gas and liquid, and may disperse the flocculent solid particles in the sedimentation separator 1, further reduce the viscosity, and improve the turbulent diffusion; the insufficiently reacted ammonia gas escaping from the recycling outlet 12 is broken into small bubbles under the action of strong swirling shear, and continues to react with the phosphoric acid in the sedimentation separator 1. Fe, Ca, Mg, Al, SiO in wet-process phosphoric acid2、SO4 2-Impurities such as F and the like generate insoluble solid impurity particles in the ammonia neutralization process, the solid impurity particles are settled along the settling separator 1 under the centrifugal force of the forced cyclone, and can be discharged from the slag discharge port 15, and the cleaner slurry is output to the next process from the slurry outlet 14. The supernatant liquid is output from the circulating outlet 12 and flows through the bottom return pipe 4 to enter the riser pipe 3 for re-reaction.
The circulation outlet 12 can be positioned above the circulation inlet 11, the circulation slurry circulation inlet 11 is arranged at the lower end of the sedimentation separator 1, escaped ammonia gas can further react with residual phosphoric acid in the sedimentation separator 1, and the circulation outlet 12 is arranged at the upper end of the sedimentation separator 1, so that separated clear liquid can be effectively conveyed to the lifting pipe 3 through a bottom reflux area for further reaction. In a word, the yield of the ammonium phosphate can be effectively improved and the escape of ammonia can be reduced by adjusting the positions of the inlet and the outlet.
The structure of the gas distributor 6 is various, and is not limited herein, for example: the gas distributor 6 can comprise a gas inlet pipe 62, the gas outlet end of the gas inlet pipe 62 penetrates through the vertical section 32 of the riser and extends into the riser 3, a gas ammonia nozzle 61 is arranged at the gas outlet end of the gas inlet pipe 62, the gas ammonia nozzle 61 is horizontally arranged and used for injecting gas, and the gas ammonia nozzle 61 is horizontally sprayed, so that the problem that slurry blocks a gas injection hole can be avoided, impinging stream is formed, rotational flow can be enhanced, and mixing of gas and liquid is enhanced; the ammonia gas is horizontally sprayed into the lifting pipe 3, so that the movement path of the lifting pipe is more complex and the ammonia gas stays for a longer time, and mass transfer and reaction are enhanced.
As shown in fig. 2 and 3, in an implementable manner, the gas ammonia nozzle 61 may include a circular ring tube 611, a threaded hole 6111 is formed in an outer side wall of the circular ring tube 611, an external thread is formed on an outer wall of an air outlet end of the air inlet tube 62, the air outlet end of the air inlet tube 62 is screwed in the threaded hole 6111 and is communicated with the inside of the circular ring tube 611, a plurality of first round holes 6112 are formed in the inner side of the circular ring tube 611 along the inner circumference thereof, axes of the plurality of first round holes 6112 are all located on the same horizontal plane and all pass through the center of the circular ring tube 611, a plurality of second round holes 6113 are formed in the outer side of the circular ring tube 611 along the outer circumference thereof at intervals, and axes of the plurality of second round. The ammonia gas can be sprayed to the central area of the riser tube 3 through the first round hole 6112 to form an impact effect, so that the turbulence degree is enhanced, the retention time of bubbles is prolonged, and the mixing of gas and liquid is enhanced, thereby being beneficial to the full reaction. The ammonia gas can be sprayed to other areas of the riser 3 through the second round hole 6113, so that the moving path is more complicated, the ammonia gas stays for a longer time, and the mass transfer and reaction enhancement are facilitated. The nozzles with different apertures of the first circular hole 6112 and the second circular hole 6113 can be replaced to meet the requirements of different gas treatment amounts, and the larger the gas treatment amount is, the larger the aperture can be correspondingly increased, for example: the aperture of the first circular holes 6112 and the second circular holes 6113 can be 0.2-1 mm.
As shown in fig. 4, in another implementation manner, the gas ammonia nozzle 61 may include an air outlet pipe 612, one end of the air inlet pipe 62 located in the riser 3 is provided with a first air outlet 621, the air outlet pipe 612 is provided with a second air outlet 6121, one end of the air outlet pipe 612 is sleeved on the air inlet pipe 62, the other end is closed, the air outlet pipe 612 is movable relative to the air inlet pipe 62 to adjust a horizontal distance between the first air outlet 621 and the second air outlet 6121, the first air outlet 621 and the second air outlet 6121 horizontally inject air, the air outlet pipe 612 and the air inlet pipe 62 may be connected by a thread, so that the horizontal distance between the first air outlet 621 and the second air outlet 6121 can be adjusted by rotating the air outlet pipe 612.
A method for analyzing factors influencing an external circulation ammonification reaction uses the external circulation ammonification reaction experimental equipment, and comprises the following specific analysis steps:
and (3) result analysis step: the reactor operates, tracer particles are added into a steam port, a Laser emitter 8 emits a piece of light to a flow field of a vertical section 32 of a lifting pipe, the tracer particles in the flow field reflect light rays and are shot by a high-speed camera 9 at a certain frequency, the shot liquid phase can be analyzed to obtain instantaneous flow field distribution by using a high-speed particle shooting technology, instantaneous flow field data are analyzed, space and time velocity pulsation is extracted, and bubble induced turbulence characteristics are analyzed; the time-average field distribution can be obtained by carrying out averaging processing; the shot bubble image is subjected to enhancement processing and converted into a binary image, the edge of the bubble is extracted, the particle size and the long-short axis ratio distribution of the bubble are obtained, and the position distribution of the bubble is further obtained; extracting image analysis data of a series of continuous moments to obtain an evolution rule of a bubble motion path, a particle size and a major-minor axis ratio, reading the flow of the flow meter 7 at the steam outlet 13, measuring the mass fraction of ammonia gas by using a nano reagent spectrophotometry, and calculating the ammonia escape rate;
the experimental steps are as follows:
when the gas ammonia nozzle 61 comprises the circular ring pipes 611, the circular ring pipes 611 are replaced, the first circular hole 6112 and the second circular hole 6113 of each circular ring pipe 611 have different apertures and the other process conditions are the same, the reactor is operated again, and the analysis steps are repeated; and researching the influence rule of the aperture on the characteristics of bubble induced turbulence, bubble rising path, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate during air injection so as to select the optimal aperture.
When the gas ammonia nozzle 61 comprises the gas outlet pipe 612, the distance between the first gas outlet hole 621 and the second gas outlet hole 6121 is adjusted, other process conditions are the same, the reactor is operated again, the analysis steps are repeated, and the influence rule of the interaction relation of the parallel bubbles with different initial distances on the ammonia escape rate can be researched to select the optimal distance between the first gas outlet hole 621 and the second gas outlet hole 6121.
Pipelines with different lengths are connected to the joint of the other end of the upper horizontal section 31 of the riser and the flange 34 of the vertical section 32 of the riser and the joint of the lower horizontal section 42 of the return pipe and the flange 34 of the lower horizontal section 33 of the riser, the lengths of the upper horizontal section 31 of the riser and the lower horizontal section 42 of the return pipe are changed, other process conditions are the same, the reactor is operated again, the analysis steps are repeated, and the influence rule of the length water of the horizontal section of the riser 3 and the horizontal section of the return pipe 4 on bubble induced turbulence characteristics, bubble rising paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate is researched, so that the optimized length range of the upper horizontal section 31 of the riser and the lower horizontal section 42 of the return pipe is selected.
Changing the rotating speed of the stirring device 2, operating the reactor again under the same other process conditions, measuring the impurity quality and the ammonia escape rate of the material slag discharge port 15, analyzing the influence rule of different rotating speeds on the settling separation efficiency and the ammonia escape rate, and obtaining the optimized rotating speed range of the stirring device 2.
Changing the rotating speed of the circulating pump 5, operating the reactor again under the same other process conditions, repeating the analysis steps, and analyzing the influence rule of the rotating speed of the circulating pump 5 on the bubble induced turbulence characteristic, the bubble rising path, the particle size distribution, the long-short axial ratio distribution evolution, the mass transfer reaction and the ammonia slip rate to obtain the optimized rotating speed range of the circulating pump 5.
Changing the opening of the regulating valve 35, operating the reactor again under the same other process conditions, repeating the analysis steps, and researching the influence rules of different equivalent diameter ratios of the lifting pipe 3 and the settling separator 1 on the bubble induced turbulence characteristic, the bubble ascending path, the particle size distribution, the long-short axis ratio distribution evolution, the mass transfer reaction and the ammonia slip rate to obtain the optimized optimal equivalent diameter ratio range of the lifting pipe 3 and the settling separator 1.
Changing the position of the circulating outlet 12, respectively arranging the position of the circulating outlet 12 on the slag discharge port 15 or the side wall of the sedimentation separator 1, when the circulating outlet 12 is arranged on the side wall of the sedimentation separator 1, the circulating outlet 12 is positioned above the circulating inlet 11, the other process conditions are the same, operating the reactor again, repeating the analysis steps, and analyzing the influence rule of the position of the circulating outlet 12 on the bubble induced turbulence characteristic, the bubble rising path, the particle size distribution, the long-short axial ratio distribution evolution, the mass transfer reaction and the ammonia escape rate.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. The utility model provides an outer circulation ammoniation reaction experimental facilities which characterized in that: comprises a sedimentation separator (1), a stirring device (2), a lifting pipe (3), a return pipe (4), a circulating pump (5), a gas distributor (6), a flowmeter (7), a Laser emitter (8) and a high-speed camera (9);
the sedimentation separator (1) is provided with a circulating inlet (11) and a circulating outlet (12) which are communicated with the interior of the sedimentation separator, the lifting pipe (3) is of a [ shape ], one end of the upper horizontal section (31) of the lifting pipe is communicated with the circulating inlet (11), the other end of the upper horizontal section (31) of the riser is detachably connected with the vertical section (32) thereof through a flange (34), the return pipe (4) is of a type, one end of the upper horizontal section (41) of the return pipe is communicated with the circulating outlet (12), the lower horizontal section (42) of the return pipe is detachably connected with the lower horizontal section (33) of the riser through a flange (34), the circulating pump (5) is arranged at the lower horizontal section (33) of the lifting pipe, the section of the lifting pipe (3) between the gas distributor (6) and the circulating pump (5) is also provided with an adjusting valve (35) for adjusting the flow rate of the lifting pipe;
a steam outlet (13) is arranged at the top of the settling separator (1), and a slurry outlet (14) and a slag discharge port (15) are arranged at the bottom of the settling separator (1);
the flow meter (7) is arranged at the steam outlet (13) and used for detecting the flow of the escaped ammonia gas;
the gas distributor (6) is arranged on the lifting pipe (3), and a gas ammonia nozzle (61) is detachably arranged on the gas distributor (6);
a phosphoric acid inlet (36) is also arranged on the vertical section (32) of the lifting pipe (3);
the lifting pipe (3) is made of transparent materials, tracer particles are added into slurry of the lifting pipe (3), a Laser emitter (8) emits sheet light to a flow field of the lifting pipe (3), the tracer particles in the flow field reflect light rays, and the light rays are shot by a high-speed camera (9) arranged on one side of a vertical section (32) of the lifting pipe (3) at a certain frequency;
the stirring device (2) is used for mixing and stirring the slurry in the sedimentation separator (1).
2. The external loop ammoniation reaction experimental facility as claimed in claim 1, wherein: the phosphoric acid inlet (36) is located below the gas distributor (6).
3. The external loop ammoniation reaction experimental facility as claimed in claim 1, wherein: agitating unit (2) are including driving piece (21), rotation axis (22) and a plurality of blade (23), rotation axis (22) vertical setting is in sedimentation separator (1), it is a plurality of blade (23) are installed around rotation axis (22) bottom, the top of rotation axis (22) is stretched out sedimentation separator (1) with driving piece (21) transmission is connected, driving piece (21) drive rotation axis (22) drive blade (23) are rotatory.
4. The external loop ammoniation reaction experimental facility as claimed in claim 1, wherein: the circulation outlet (12) is located above the circulation inlet (11).
5. An external loop ammoniation reaction laboratory apparatus as claimed in any one of claims 1 to 3, wherein: the gas distributor (6) comprises a gas inlet pipe (62), the gas outlet end of the gas inlet pipe (62) penetrates through the vertical section (32) of the lifting pipe (3) and extends into the lifting pipe (3), the gas ammonia nozzle (61) is arranged at the gas outlet end of the gas inlet pipe (62), and the gas ammonia nozzle (61) is horizontally arranged and horizontally sprays gas.
6. The experimental apparatus for an external loop ammonification reaction of claim 5, wherein: the gas ammonia nozzle (61) comprises an annular pipe (611), a threaded hole (6111) is formed in the outer side wall of the annular pipe (611), an external thread is formed in the outer wall of the air outlet end of the air inlet pipe (62), the air outlet end of the air inlet pipe (62) is screwed in the threaded hole (6111) and is communicated with the inside of the annular pipe (611), a plurality of first round holes (6112) are formed in the inner side of the annular pipe (611) along the inner circumference of the annular pipe, the axes of the first round holes (6112) are located on the same horizontal plane and penetrate through the circle center of the annular pipe (611), a plurality of second round holes (6113) are formed in the outer side of the annular pipe (611) along the outer circumference of the annular pipe at intervals, and the axes of the second round holes (6113) are located on the same horizontal plane.
7. The experimental apparatus for an external loop ammonification reaction of claim 6, wherein: the aperture of the first round holes (6112) and the second round holes (6113) is 0.2-1 mm.
8. The experimental apparatus for an external loop ammonification reaction of claim 5, wherein: the gas ammonia nozzle (61) comprises an air outlet pipe (612), one end of the air inlet pipe (62) in the lifting pipe (3) is provided with a first air outlet hole (621), the air outlet pipe (612) is provided with a second air outlet hole (6121), one end of the air outlet pipe (612) is sleeved on the air inlet pipe (62), the other end of the air outlet pipe is sealed, the air outlet pipe (612) can move relative to the air inlet pipe (62) to adjust the horizontal distance between the first air outlet hole (621) and the second air outlet hole (6121), and the first air outlet hole (621) and the second air outlet hole (6121) horizontally jet air.
9. A method for analyzing factors affecting an ammoniation reaction of an external loop stream, comprising: the use of an external loop ammoniation reaction experimental set-up as defined in any one of claims 6 to 8, the specific analytical procedures were as follows:
and (3) result analysis step: the reactor is operated, tracer particles are added into a steam port, a Laser emitter (8) emits a piece of light to a flow field of a vertical section (32) of a lifting pipe (3), the tracer particles in the flow field reflect light rays, the light rays are shot by a high-speed camera (9) at a certain frequency, the shot liquid phase can analyze instantaneous flow field distribution by using a high-speed particle shooting technology, instantaneous flow field data are analyzed, space and time velocity pulsation is extracted, and bubble induced turbulence characteristics are analyzed; the time-average field distribution can be obtained by carrying out averaging processing; the shot bubble image is subjected to enhancement processing and converted into a binary image, the edge of the bubble is extracted, the particle size and the long-short axis ratio distribution of the bubble are obtained, and the position distribution of the bubble is further obtained; extracting image analysis data of a series of continuous moments to obtain an evolution rule of a bubble motion path, a particle size and a major-minor axis ratio, reading the flow of a flow meter (7) at a steam outlet (13), measuring the mass fraction of ammonia gas by using a nano reagent spectrophotometry, and calculating the ammonia escape rate;
the experimental steps are as follows:
when the gas ammonia nozzle (61) comprises the circular ring pipes (611), replacing the circular ring pipes (611), wherein the first circular hole (6112) and the second circular hole (6113) of each circular ring pipe (611) have different apertures and the other process conditions are the same, operating the reactor again, and repeating the analysis steps; researching the influence rule of the aperture during air injection on the characteristics of bubble induced turbulence, bubble rising path, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate;
when the gas ammonia nozzle (61) comprises the gas outlet pipe (612), adjusting the distance between the first gas outlet hole (621) and the second gas outlet hole (6121), operating the reactor again under the same other process conditions, repeating the analysis steps, and researching the influence rule of the interaction relation of the parallel bubbles with different initial distances on the ammonia escape rate;
connecting pipelines with different lengths at the joint of the other end of the upper horizontal section (31) of the riser and the flange (34) of the vertical section (32) of the riser and the joint of the lower horizontal section (42) of the backflow pipe and the flange (34) of the lower horizontal section (33) of the riser, changing the lengths of the upper horizontal section (31) of the riser and the lower horizontal section (42) of the backflow pipe, keeping the other process conditions the same, operating the reactor again, repeating the analysis steps, and researching the influence rule of the length water of the horizontal section of the riser (3) and the horizontal section of the backflow pipe (4) on bubble induced turbulence characteristics, bubble ascending paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate;
changing the rotating speed of the stirring device (2), operating the reactor again under the same other process conditions, measuring the impurity quality and the ammonia escape rate of the material slag discharge port (15), and analyzing the influence rules of different rotating speeds on the settling separation efficiency and the ammonia escape rate;
changing the rotating speed of the circulating pump (5), operating the reactor again under the same other process conditions, repeating the analysis steps, and analyzing the influence rule of the rotating speed of the circulating pump (5) on the characteristics of bubble-induced turbulence, bubble ascending paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate;
changing the opening of the regulating valve (35), operating the reactor again under the same other process conditions, repeating the analysis steps, and researching the influence rules of the bubble induced turbulence characteristics, the bubble rising path, the particle size distribution, the long-short axis ratio distribution evolution, the mass transfer reaction and the ammonia escape rate of different equivalent diameter ratios.
10. A method of analysing factors affecting an ammoniation reaction of an external loop stream as claimed in claim 9, characterized in that: changing the position of a circulating outlet (12), respectively arranging the position of the circulating outlet (12) on a slag discharge port (15) or the side wall of a sedimentation separator (1), when the circulating outlet (12) is arranged on the side wall of the sedimentation separator (1), the circulating outlet (12) is positioned above the circulating inlet (11), other process conditions are the same, operating the reactor again, repeating the analysis steps, and analyzing the influence rule of the position of the circulating outlet (12) on bubble induced turbulence characteristics, bubble rising paths, particle size distribution, long-short axial ratio distribution evolution, mass transfer reaction and ammonia escape rate.
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