CN111569790B - Gas distributor for organosilicon fluidized bed and organosilicon fluidized bed reactor - Google Patents
Gas distributor for organosilicon fluidized bed and organosilicon fluidized bed reactor Download PDFInfo
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- CN111569790B CN111569790B CN202010438987.0A CN202010438987A CN111569790B CN 111569790 B CN111569790 B CN 111569790B CN 202010438987 A CN202010438987 A CN 202010438987A CN 111569790 B CN111569790 B CN 111569790B
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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Abstract
The gas distributor provided by the invention is adopted in the organic silicon fluidized bed, so that the accumulation dead zone of a side wall area is favorably eliminated, meanwhile, the shearing and collision of particles can be promoted, the surface of the particles is updated, and the reaction activity in the fluidized bed is improved. The invention provides a gas distributor for an organic silicon fluidized bed, which comprises a gas distribution plate and a particle flow guide device, wherein the gas distribution plate is divided into a central area and a side wall area positioned at the periphery of the central area, and a plurality of vertical air holes are distributed in the central area; the particle diversion device is arranged on the side wall area and is used for sucking particles deposited on the side wall area and spraying the particles above the gas distribution plate in a horizontal direction or a roughly horizontal direction and at least above the central area.
Description
Technical Field
The invention relates to a gas distributor, in particular to a gas distributor suitable for an organic silicon monomer synthesis fluidized bed.
Background
In a fluidized bed of silicone, a gas distributor plays a crucial role in the performance of the fluidized bed. At present, the gas distribution plates widely used in the industry can be classified into two types: one is a simple straight hole distribution plate; the second type is a distributor plate with a hood. Because the organosilicon monomer synthesis system has the characteristics of strong heat release, strong system adhesion, easy agglomeration of particles, high-boiling-point substances and carbon deposition generated by side reaction and the design defect of the distributor, the following technical problems exist in the use process:
1. when the straight hole distribution plate is applied to a fluidized bed with a larger diameter, because the air flow distribution is uneven, the air speed of an air inlet hole close to the wall of the fluidized bed is low due to the side wall effect, material leakage is easy to occur, and a material accumulation dead zone is formed.
2. The blast cap distribution plate is provided with the blast cap on the vent hole, which can play a role of preventing material leakage, but the use of the blast cap also can not flow out towards the vertical upward direction when the gas passes through, and the gas-solid mixing and dispersing effect of the system is poor.
3. The gas-solid mixing and dispersing effect of the fluidized bed is uneven, the local gas-solid mixing and dispersing effect is poor, heat in particle agglomeration cannot be removed in time, side reactions are increased, and the reaction selectivity is reduced.
4. The silicon powder surface accumulates copper and carbon deposition, the reaction activity is low, the conversion rate is reduced, and the unit consumption of the silicon powder and the catalyst is increased.
In order to avoid the problems, the long-period stable operation of the device is realized, effective measures are needed to ensure that the airflow in the organosilicon fluidized bed is uniformly distributed, the gas and the solid are fully and uniformly contacted, local fluidization dead zones and hot spots are avoided, and the problem of low reaction activity of silicon powder in the fluidized bed is solved. The gas distributor is the most key part for realizing uniform distribution of gas flow in the dense-phase zone of the fluidized bed and uniform fluidization of gas and solid.
To above-mentioned problem, CN 110559955A discloses an organosilicon fluidized bed distributing plate, and the breather pipe is located the pipe wall of mounting groove side and the circumference equipartition has radial through-hole, and the through-hole is terminal surface under the hood, can play the effect that prevents to leak the material and can also make gas flow along vertical ascending direction simultaneously. CN207012953U discloses an organosilicon fluidized bed with a crushing device, which forms high-speed airflow through a crushing nozzle to update and crush the surface of materials in the bed, and can partially solve the problems that the fluidized bed in the prior art is low in reaction activity and a gas distributor is easy to block. CN 107126912 discloses a gas distribution plate of an organosilicon fluidized bed reactor, which is provided with a step-shaped vent with a narrow top and a wide bottom, so that silicon powder is prevented from leaking along the vent from the upper part of the distribution plate, and the vent is prevented from being blocked.
The above documents only partially solve the problem of material leakage of the distribution plate by improving the form of the nozzles of the distribution plate, or perform surface renewal on local materials in a fluidized bed fluid adding and crushing device to increase the reactivity. However, the problems of a fluidization dead zone, poor local heat dissipation effect, copper-rich and carbon deposition accumulated on the surface of silicon powder, low reaction activity and reduced chloromethane conversion rate caused by uneven airflow distribution cannot be essentially solved because the flow field in the reactor cannot be fundamentally optimized.
Therefore, developing a gas distributor suitable for a strongly exothermic and strongly adhesive agglomeration fluidized bed system of an organosilicon monomer synthesis system is very important for overcoming the nonuniform gas distribution in the fluidized bed, eliminating local fluidization dead zones, cleaning copper and carbon rich on the surface of silicon powder particles and improving the reaction activity and selectivity.
Disclosure of Invention
In view of the above, the present invention provides a gas distributor for a fluidized bed of organosilicon and a fluidized bed reactor of organosilicon using the gas distributor. The gas distributor provided by the invention is adopted in the organic silicon fluidized bed, so that the accumulation dead zone of a side wall area is favorably eliminated, and the shearing and collision of particles are promoted, thereby being favorable for realizing the surface updating of the particles and improving the reaction activity in the fluidized bed.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a gas distributor for an organic silicon fluidized bed, which comprises a gas distribution plate and a particle flow guide device, wherein the gas distribution plate is divided into a central area and a side wall area positioned at the periphery of the central area, and a plurality of vertical air holes are distributed in the central area; the particle diversion device is arranged on the side wall area and is used for sucking particles deposited on the side wall area and spraying the particles above the gas distribution plate in a horizontal direction or a roughly horizontal direction and at least above the central area.
In some embodiments, the central region comprises 70-80% (e.g., 70%, 75%, 80%) of the total area of the gas distribution plate, e.g., circular, and the sidewall region comprises 20-30% of the total area of the gas distribution plate, e.g., 0.8-3.5m in diameter.
In some embodiments, the particle diversion device comprises an air inlet pipe, a frustum-shaped reducer pipe and a diversion cylinder; the side wall area is provided with jet flow air holes;
the air inlet pipe is communicated with the jet flow air hole through the cone frustum-shaped reducer pipe; the inner diameter of the frustum-shaped variable-diameter pipe is gradually reduced along the direction from the joint of the frustum-shaped variable-diameter pipe and the air inlet pipe to the joint of the frustum-shaped variable-diameter pipe and the jet air hole;
the guide cylinder is arranged right above the jet flow air hole, the air inlet of the guide cylinder is positioned at the lower end of the guide cylinder and is opposite to the air outlet of the jet flow air hole, and a gap is formed between the air inlet of the guide cylinder and the air outlet of the jet flow air hole; the air outlet of the guide cylinder is arranged to enable the air flow to be ejected in the horizontal direction or approximately in the horizontal direction;
preferably, the air inlet of the guide cylinder is coaxial with the air outlet of the jet flow air hole, and the vertical distance between the air inlet of the guide cylinder and the air outlet of the jet flow air hole is 5-20mm (for example, 5mm, 10mm, 15mm, 20 mm);
preferably, the cone angle α of the truncated cone-shaped reducer is 30-60 °, such as 30 °, 40 °, 50 °, 60 °, and the like.
In some embodiments, the air outlet of the guide cylinder is arranged to face the central area and eject the air flow in a horizontal direction or a substantially horizontal direction.
In some embodiments, the jet air hole is sequentially divided into a vertical section and a flaring section from bottom to top along the vertical direction;
preferably, the flaring angle β of the flaring section of the jet flow orifice is 20-26 °;
preferably, the diameter D2 of the vertical section (16) of the jet air hole is 5-9mm, the length L of the vertical section is 2-15mm, and the maximum diameter D3 of the flaring section of the jet air hole is 6-10 mm.
In some embodiments, the sidewall region is provided with a plurality of particle deflectors radially distributed around the center of the gas distribution plate;
preferably, each particle diversion device is arranged at equal intervals, and each particle diversion device is symmetrically distributed in the sidewall area, for example, symmetrically distributed relative to the center of the gas distribution plate; the side wall region is for example in the shape of a circular ring as a whole; the number of particle diversion means is for example 2-16;
preferably, the air outlet of the guide shell of the particle guide device is set as follows: the air flow spraying direction of the air outlets of the guide shell of at least part of the particle guide device and the air flow spraying direction of the vertical air holes in the central area are intersected above the air distribution plate, so that interweaving, collision and shearing between horizontal jet flows and axial jet flows can be ensured.
In some embodiments, the air inlet tube comprises a vertical tube section and a horizontal tube section connected to the vertical tube section; the vertical pipe section is connected with the circular truncated cone-shaped reducer pipe; the diameter D1 of the inlet pipe is preferably 30-50mm, and the gas inlet pressure of the inlet pipe is preferably 1.0-1.6 MPa.
In some embodiments, the air inlet of the guide cylinder is provided with a truncated cone-shaped reducing port, and the guide cylinder comprises a guide vertical pipe section connected with the truncated cone-shaped reducing port and a guide bent pipe section connected with the guide vertical pipe section;
the inner diameter of the truncated cone-shaped reducing port gradually decreases from bottom to top;
preferably, the cone angle γ of the truncated cone-shaped reduction is 90 to 120 ° (e.g. 90 °, 100 °, 110 °, 120 °), and the maximum diameter D4 of the truncated cone-shaped reduction is 40 to 170 mm;
preferably, the diameter D5 of the diversion vertical pipe section is 20-150mm, and the length L1 of the diversion vertical pipe section is 50-200 mm;
preferably, the angle δ between the flow guiding bent pipe section and the horizontal direction is 30-60 °, such as 30 °, 40 °, 50 °, 60 °.
In some embodiments, the central area is uniformly provided with the vertical air holes with the same diameter, and the opening rate is 1-5%; the diameter D0 of the vertical air hole is 2-4mm, and the air inlet pressure of the vertical air hole is 0.2-0.5 MPa.
In some embodiments, the reactor has installed therein a gas distributor as described above;
the gas distribution plate of the gas distributor is fixedly arranged in the inner cavity of the reactor; the particle diversion device is fixedly connected with the inner wall of the reactor;
specifically, the gas distribution plate is fixedly connected with the lower end socket of the reactor through a fastener.
The technical scheme provided by the invention has the following beneficial effects:
(1) the gas distribution plate is divided into a center area and a side wall area, and meanwhile, the particle flow guide device is arranged on the side wall area, so that the gas distribution in the fluidized bed can be optimized.
In some preferred modes, the particle diversion device is specifically provided with an air inlet pipe, a cone-shaped reducer pipe and a diversion cylinder, a corresponding jet air hole is arranged in the side wall area, and a gap is reserved between an air inlet of the diversion cylinder and an air outlet of the jet air hole; after high-speed gas is input through the gas inlet pipe, the high-speed gas enters the jet flow air hole through the circular truncated cone-shaped reducer pipe, and is jetted through the jet flow air hole to form jet gas flow, the jet gas flow forms rotational flow at a gap between the jet flow air hole and the guide cylinder, particles deposited on the side wall area are sucked into the rotational flow under the action of the rotational flow, and then are sucked into the guide cylinder along with the jet gas flow and are jetted to the central area along the horizontal direction or the approximately horizontal direction through the guide cylinder; through the design, not only is the dead zone of the side wall in the fluidized bed eliminated, but also the particles enter the guide shell along with the airflow and are horizontally or approximately horizontally ejected and at least ejected to the upper part of the central area, so that the particles can form interlacing collision and shearing with the axial ejection flow of the vertical air hole in the central area, the heat transfer effect is improved, and the contact body sintering caused by poor local heat dissipation can be avoided.
(2) The particle flow guide device is arranged in the side wall area, so that a sedimentation dead zone on the distribution plate is eliminated, and the particle flow guide device provides horizontal or approximately horizontal jet flow to be in shearing collision with the vertical jet flow in the central area, so that the surface renewal of particles is realized, and the reaction activity in the fluidized bed is improved.
(3) The gas distributor is not easy to block, and the operation flexibility and the production period of the fluidized bed are obviously improved.
Drawings
FIG. 1 is a schematic longitudinal sectional view of the gas distributor of the present invention.
Fig. 2 is a schematic structural view of the vertical air hole in fig. 1.
FIG. 3 is a schematic view of the structure of the particle deflector of FIG. 1;
FIG. 4 is a schematic structural view of the air inlet pipe and the cone-shaped reducer pipe in FIG. 1;
FIG. 5 is a schematic diagram of the jet orifice of FIG. 1;
fig. 6 is a schematic structural view of the guide shell in fig. 1.
In the figure, 1, a gas distribution plate; 2. a particle diversion device; 3. a lower end enclosure; 11. a sidewall region; 12. a central region; 13. a vertical air hole; 14. a connecting arm; 15. jet flow air holes; 16. a vertical section; 17. a flared section; 21. an air inlet pipe; 22. a draft tube; 23. a flow guiding vertical pipe section; 24. a flow guiding bent pipe section; 25. an air outlet of the guide cylinder; 26. a truncated cone-shaped reducing port; 27. a cone-shaped reducer pipe; 28. a vertical pipe section; 29. a horizontal pipe section.
Detailed Description
In order to better understand the technical solution of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The terms of orientation, up, down, left, right, front, rear, front, back, top, bottom, vertical, horizontal, etc., referred to or may be referred to in this specification are defined relative to the configuration shown in the drawings, and are relative terms, and thus may be changed correspondingly according to the position and the use state thereof. The terms "inner" and "outer" may be used to refer to directions toward and away from, respectively, the geometric center of a particular component.
Where not otherwise stated herein, may be known or understood by those skilled in the art based on their knowledge and common general knowledge.
The invention provides a gas distributor for a fluidized bed of organic silicon, which comprises a gas distribution plate 1 and a particle diversion device 2, and is shown in figure 1. The gas distribution plate 1 is divided into a central area 12 and a sidewall area 11 located at the periphery of the central area 12, that is, the whole gas distribution plate 1 is divided into a central area and a sidewall area at the periphery of the central area. In the central area 12, a plurality of vertical air holes 13, i.e. axial openings, are provided. In the sidewall area 11, a particle deflector 2 is arranged, which particle deflector 2 is arranged in the sidewall area 11, and mainly by means of which particles deposited in the sidewall area 11 are sucked in and ejected in a horizontal direction or substantially in a horizontal direction in the form of jets which are at least partly ejected above the central area 12 of the gas distribution plate 1.
In some embodiments, the central region 12 comprises 70-80% of the total area of the gas distribution plate 1, and the remaining sidewall regions 11, i.e., the sidewall regions 11, comprise 20-30% of the total area of the gas distribution plate 1. The inventor finds that the preferable area division of the gas distribution plate can obtain better uniform gas flow distribution effect and high space utilization efficiency; however, if the proportion of the side wall area is too small, the effect of uniform air flow distribution is reduced because the central area has substantially uneven air flow distribution; if the occupation ratio of the side wall area is too large, the devices such as the guide shell occupy too much space, and the space utilization efficiency of the reactor is reduced.
The overall shape of the gas distribution plate 1 is not particularly limited, and, for example, a circular shape can be conventionally employed. The diameter of the gas distribution plate 1 may be specifically determined according to practical needs, for example, the diameter is 0.8-3.5 m.
Referring to fig. 1, 3-6, the particle diversion device 2 specifically comprises an air inlet pipe 21, a truncated cone-shaped reducer pipe 27 and a diversion cylinder 22; and jet holes 15 are correspondingly arranged in the side wall area 11.
The air inlet pipe 21 is communicated with the jet air holes 15 through the cone-shaped reducing pipe 27, namely, the air inlet pipe 21 is connected with the jet air holes 15 through the cone-shaped reducing pipe 27. Along the direction from the joint of the truncated cone-shaped reducer 27 and the air inlet pipe 21 to the joint of the truncated cone-shaped reducer 27 and the jet air hole 15, the inner diameter of the truncated cone-shaped reducer 27 is gradually reduced, namely gradually narrowed along the air flow direction, so that high-speed flow of the air flow is ensured, and jet flow is provided.
The guide shell 22 is arranged right above the jet flow air hole 15, an air inlet of the guide shell 22 is positioned at the lower end of the guide shell and is opposite to an air outlet of the jet flow air hole 15, and a gap is formed between the air inlet of the guide shell 22 and the air outlet of the jet flow air hole 15; therefore, the airflow jetted by the jet flow air holes 15 can enter the guide shell 22 with minimum loss, and simultaneously high-speed rotational flow is formed, so that deposited particles in the side wall area 11 are sucked into the guide shell 22 along with the rotational flow. The air outlet 25 of the guide shell 22 is arranged to eject the air flow in a horizontal direction or approximately in a horizontal direction; while at least some and more preferably all of the gas outlets 25 of the guide shell 22 are arranged towards the top of the central area 12 of the gas distribution plate 1. Therefore, the horizontal particle jet flow and the axial jet flow of the vertical air holes 13 in the central area 12 can be interlaced, collided and sheared, so that on one hand, material mixing is promoted, the heat transfer effect is improved, and the side reaction is reduced; on the other hand, the dead zone of the side wall is eliminated, and the gas-solid mixing of the fluidized bed is more uniform and sufficient, so that the reaction is more fully carried out; on the other hand, due to the collision and shearing of the particles (silicon powder), the copper and/or carbon rich accumulated on the surfaces of the particles are removed, the reaction activity of the particles is maintained, and the reaction conversion rate is improved. In a further embodiment, the gas jet direction of the gas outlets of the guide shell of at least some, preferably all, of the particle guide devices intersects the gas jet direction of the vertical gas holes in the central region above the gas distribution plate, so as to ensure sufficient interlacing, collision and shearing between the horizontal jet flow and the axial jet flow.
In some embodiments, the air inlet of the guide cylinder 22 and the air outlet of the jet air hole 15 are coaxial, and the vertical distance between the air inlet of the guide cylinder 22 and the air outlet of the jet air hole 15 is 5-20mm, such as 5mm, 10mm, 15mm, 20 mm.
In some embodiments, referring to fig. 4, the cone angle α of the frustum-shaped reducer 27 is designed to be 30-60 ° to facilitate the gradual change of the velocity and pressure of the gas; if the angle is too large, the gas cannot be sufficiently accelerated, and the pressure loss rapidly increases; if too small, the length of the truncated cone-shaped reducer 27 is too long, which wastes equipment space.
In some embodiments, the jet vents 15 are designed to: the vertical section 16 and the flaring section 17 are sequentially arranged along the direction from the gas inlet to the gas outlet of the jet flow gas hole 15, and as shown in fig. 5, the jet flow gas hole 15 is sequentially divided into the vertical section 16 and the flaring section 17 from bottom to top along the vertical direction; that is, form vertical air current earlier in the efflux gas pocket 15, this vertical air current is erupted through the gas outlet of flaring form afterwards, and gas process expansion is accelerated like this, and the speed can break through the sound velocity to higher speed and lower pressure blowout, entrainment that can be better and carry the granule. Specifically, the contour of the flared section 17 may be a circular truncated cone shape, and the inner diameter of the flared section 17 gradually increases from the inlet to the outlet of the flared section. Preferably, referring to FIG. 5, the flared section 17 of the jet orifice 15 has a flare angle β of 20-26. In some embodiments, the diameter D2 of the vertical section 16 of the jet orifice 15 is 5-9mm, the length L of the vertical section 16 is 2-15mm, and the maximum diameter D3 (i.e., the outlet diameter) of the flared section 17 of the jet orifice 15 is 6-10 mm.
Specifically, a plurality of particle deflectors 2 may be disposed on the sidewall area 11, and the particle deflectors (2) are radially distributed around the center of the gas distribution plate 1. Preferably, the particle guiding devices 2 are arranged at equal intervals, and the particle guiding devices 2 are symmetrically distributed in the sidewall area 11, for example, symmetrically distributed relative to the center of the gas distribution plate 1, so that when the air outlets 25 of the guiding cylinders 22 of the particle guiding devices 2 are all arranged to face to the right above the central area 12, the axial jet flow of the central area 12 and the horizontal jet flow of the guiding cylinders 22 which are horizontally or approximately horizontally jetted can be more sufficiently collided and sheared.
The side wall region 11 is, for example, annular in shape as a whole; the number of particle deflection means 2 is for example 2-16.
In some embodiments, the air inlet pipe 21 is designed to include a vertical pipe section 28 and a horizontal pipe section 29 connected to the vertical pipe section 28; the upright tube section 28 is connected with the truncated cone-shaped reducer 27. The design can lead the gas to be gradually compressed and accelerated in the contraction section, the pressure energy is better converted into the kinetic energy, and the energy loss is low. The diameter D1 of the inlet pipe 21 is preferably 30-50mm, and the gas inlet pressure of the inlet pipe 21 is preferably 1.0-1.6 MPa.
In some embodiments, referring to fig. 6, the air inlet of the guide shell 22 is provided with a truncated cone-shaped reducing opening 26, and the guide shell 22 comprises a guide vertical pipe section 23 connected with the truncated cone-shaped reducing opening 26 and a guide bent pipe section 24 connected with the guide vertical pipe section 23. Wherein, along the direction from the air inlet end to the air outlet end of the truncated cone-shaped reducing port 26, the inner diameter of the truncated cone-shaped reducing port 26 gradually decreases, namely gradually narrows along the direction of the air flow; as shown in fig. 6, the inner diameter of the truncated cone-shaped reduced diameter opening 26 gradually decreases from bottom to top. So design draft tube, can be more abundant inhale the granule that piles up on every side, the straight section of water conservancy diversion makes granule and gaseous intensive mixing, and the granule is given to the gas and accelerates, and the velocity direction of granule is then changed to radial by the axial to the turn of water conservancy diversion bend section.
Wherein, the cone angle gamma of the truncated cone-shaped reducing port 26 is preferably designed to be 90-120 degrees, and the angle is preferably selected to improve the effect of sucking the particles accumulated around; if the angle is too large, the suction force is reduced, and the effect is not good; if it is too small, the absorption range is too small, and the effect is also deteriorated. The maximum diameter D4 of the truncated cone-shaped reducing port 26 is designed to be 40-170 mm;
in some embodiments, the diameter D5 of the flow guide vertical pipe section 23 is 20-150mm, and the length L1 of the flow guide vertical pipe section 23 is 50-200 mm; the diameter of the diversion elbow section 24 is the same as that of the diversion vertical pipe section 23, and the included angle between the outlet direction of the diversion elbow and the horizontal direction is 0 degree.
In some embodiments, as shown in fig. 6, the angle δ between the flow directing elbow 24 and the horizontal is preferably 30-60 °. Preferably, the angle can change the particle moving direction under the condition of ensuring that the particle speed loss is not large, and the particle speed loss is too large when the angle is too small.
In some embodiments, the central area 12 of the gas distribution plate 1 is uniformly provided with vertical air holes 13 having equal diameters, that is, the vertical air holes 13 have equal diameters and are uniformly distributed in the central area 12, so that the gas flow is uniformly injected in the axial direction, thereby ensuring uniform fluidization of the central area 12 of the fluidized bed, and simultaneously, due to the uniform distribution of the vertical air holes, the particle jet flow ejected by the particle diversion device, which is preferably symmetrically and equidistantly distributed, can be more sufficiently and uniformly interlaced, collided and sheared. The open porosity of the central region 12 is 1-5%. The diameter D0 of the vertical air hole 13 can be 2-4mm, and the air inlet pressure of the vertical air hole 13 can be 0.2-0.5 MPa. The high air speed of the air inlet hole also avoids the occurrence of material accumulation and material leakage.
The gas distributor provided by the invention is applied to the fluidized bed, can eliminate channeling and dead zones in the fluidized bed, solves the problems of contact body sintering and untimely local heat transfer in the fluidized bed through high-speed jet injection and radial particle diversion, and improves the reaction activity in the fluidized bed. The distributor is reasonably arranged into a central area 12 and a side wall area 11, the central area passes through vertical air holes 13, and air flow is directly injected axially to ensure that the central area 12 of the fluidized bed is uniformly fluidized. The distribution plate is provided with a particle flow guide device 2, high-speed gas enters a jet flow air hole through a cone-shaped reducer after being input through an air inlet pipe of the particle flow guide device, jet air flow is jetted through the jet flow air hole, the jet air flow forms rotational flow at a gap between the jet flow air hole and the guide cylinder, and particles deposited on the side wall area are sucked into the rotational flow and enter the guide cylinder along with the rotational flow due to the effect of the rotational flow; thus, the particles forming the accumulation dead zone on the wall surface area of the fluidized bed can be sucked into the particle guide cylinder 22 through the high-speed gas jet; the particle jet direction is changed from axial direct injection to radial direction through the particle guide cylinder 22, so that the settling dead zone on the distribution plate is eliminated; meanwhile, because horizontal or approximately horizontal jet flow ejected by the guide shell is interwoven, collided and sheared with axial jet flow of the vertical air hole in the central area, heat transfer is improved through particle jet flow collision, the problems of material sintering and local heat transfer untimely in the fluidized bed are solved, the surface updating of particles is realized through particle shearing and collision, and the reaction activity in the fluidized bed is improved.
For industrial fluidized beds with larger diameters, it is easy to have high gas content in the center area and low gas content near the wall surface due to the sidewall effect, resulting in non-uniform fluidization and formation of a dead zone. The particle guide device 2 is arranged in the edge wall area 11 of the distribution plate, particle jet flow which forms an accumulation dead zone in the fluidization edge wall area is introduced into the particle guide cylinder 22 and is guided to change the direction of the particle jet flow from axial direct injection to radial direction, so that the sedimentation dead zone on the distribution plate is eliminated, and materials in the accumulation dead zone enter the fluidized bed again for reaction.
The gas distributor disclosed by the invention can be applied to an organosilicon monomer synthesis fluidized bed reactor which has strong heat release, strong system adhesion and high-boiling-point substances and carbon deposition generated by side reaction.
The gas distribution plate 1 provided by the invention is particularly suitable for an organic silicon fluidized bed reactor, so that the invention also provides the organic silicon fluidized bed reactor provided with the gas distributor; the main improvement of the reactor is that the gas distribution plate 1 of the present invention is adopted, and other structures of the reactor can adopt conventional designs in the art, which are not described in detail.
Specifically, as shown in fig. 1, a gas distribution plate 1 of the gas distributor is fixedly installed in an inner cavity of the reactor; for example, the reactor is fixedly connected with the lower seal head 3 of the reactor through a fastener. The particle diversion device 2 is fixedly connected with the inner wall of the reactor to fix the particle diversion device 2, specifically, as shown in fig. 1, the air inlet pipe 21 is extended into the lower end enclosure 3 and fixedly connected with the inner wall of the lower end enclosure 3, the diversion cylinder 22 is fixedly connected with the inner wall of the reactor above the gas distribution plate 1 through the connecting arm 14, for example, welded and fixed, and the diversion cylinder 22 is installed in a suspended manner relative to the gas distribution plate 1, that is, a gap is reserved between the air inlet of the diversion cylinder 22 and the air outlet of the jet flow air hole 15. The air inlet pipe 21 of the particle diversion device 2 is connected with the jet flow air hole 15 of the side wall area 11 through the cone-shaped reducing pipe 27.
The gas distributor according to the invention is illustrated by means of specific examples.
Example 1
A pilot scale organosilicon monomer fluidized bed synthesis reactor having a diameter of 1m and a height of 6m was fitted with a gas distributor according to the invention. As shown in fig. 1-6, the center region 12 accounts for 75% of the total area of the gas distribution plate 1, and the sidewall regions 11 account for 25% of the total area of the gas distribution plate 1. The central area is uniformly provided with equal-diameter vertical air holes 13, and the aperture ratio is 1.5%; the diameter D0 of the vertical air hole 13 is 3mm, and the air inlet pressure of the vertical air hole 13 is 0.35 MPa. And 3 particle flow guide devices 2 are symmetrically distributed along the circular annular side wall area 11 at equal intervals. The air outlet 25 of the guide shell 22 is disposed toward the upper side of the center region 12.
The air inlet pipe 21 is connected with the jet flow air hole 15 through the cone-shaped reducing pipe 27, the pressure of an air inlet is 1.5MPa, the cone angle alpha of the cone-shaped reducing pipe 27 is 60 degrees, and the diameter D1 is 30mm (the vertical pipe and the horizontal pipe are the same diameter).
The diameter D2 of the air inlet of the jet flow air hole 15 is 7mm, the length L of the vertical section 16 is 10mm, the diameter D3 of the outlet is 8mm, and the angle beta of the flaring section 17 is 24 degrees.
The air inlet of the guide cylinder 22 is coaxial with the air outlet of the jet flow air hole 15, the vertical distance between the air inlet and the air outlet is 6mm, the angle gamma of the truncated cone-shaped reducing port 26 is 120 degrees, the inlet diameter D4 of the truncated cone-shaped reducing port 26 is 100mm, the inlet diameter D5 of the guide vertical pipe section 23 is 75mm, the length L1 of the guide vertical pipe section 23 is 60mm, the diameter of the guide bent pipe section 24 is the same as that of the guide vertical pipe section 23, the included angle delta between the guide bent pipe section 24 and the horizontal direction is 60 degrees, and the included angle between the outlet direction of the guide bent pipe section 24 and the horizontal direction is 0 degree.
In the fluidized bed reactor, continuous exothermic reaction of methyl chloride (CH3C l) and silicon powder to synthesize methyl chlorosilane is carried out, and CuC l is used as a catalyst. The reaction pressure is 0.3MPa, the temperature is 295 ℃, and the material feeding temperature is 170 ℃.
The reactor is continuously operated for 31 days, the bed temperatures of the fluidized bed at different heights are not obviously fluctuated in the process (the temperature fluctuation range is not more than +/-4 ℃), and the once-through conversion rate of the chloromethane is maintained to be more than 55%. And after the reactor is stopped, a manhole is opened for inspection, no hardened material is found in the fluidized bed, and the vertical air holes 13 of the distribution plate are not blocked.
Comparative example 1
This comparative example differs from example 1 in that: a pilot plant organosilicon monomer fluidized bed synthesis reactor with the diameter of 1m and the height of 6m is provided with a common sieve pore gas distribution plate 1 with the aperture ratio of 1.5 percent, the structure size of the air inlet is the same as that of the vertical air hole 13 in the embodiment 1, the air inlet is uniformly distributed on the whole gas distribution plate 1, and the diameter of the orifice is 3 mm; the particle deflector 2 of example 1 was not installed.
Continuous exothermic reaction of methyl chloride and silicon powder to synthesize methyl chlorosilane is carried out in the fluidized bed reactor, and CuC l is used as a catalyst. The reaction pressure is 0.3MPa, the temperature is 295 ℃, and the material feeding temperature is 170 ℃.
The reactor is operated for 31 days, the once-through conversion rate of the chloromethane is maintained to be more than 40% at the initial stage of the reaction, the temperature fluctuation of a fluidized bed layer is obvious when the reactor is operated for 10 days, the once-through conversion rate of the chloromethane is continuously reduced, and the sampling rate is reduced to 34% when the reactor is operated for 30 days.
After the reactor is stopped, a manhole is opened for inspection, some plate material blocks with high carbon content are found in the fluidized bed, about 20-30% of air inlet holes are blocked, about 50% of air inlet holes of the distribution plate close to the wall of the fluidized bed are blocked, and meanwhile, a large amount of catalyst leaks to a gas distribution chamber below the gas distribution plate 1 and must be cleaned manually.
The use effects of example 1 and comparative example 1 show that: the gas distribution plate 1 of the invention not only improves the heat transfer and mass transfer efficiency of the organic silicon fluidized bed, but also can continuously update the surface of silicon powder materials, solves the problems of contact body sintering and untimely local heat transfer in the fluidized bed, and improves the reaction activity in the fluidized bed.
It will be appreciated by those skilled in the art that modifications or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (19)
1. A gas distributor for an organosilicon fluidized bed, which is characterized by comprising a gas distribution plate (1) and a particle diversion device (2), wherein the gas distribution plate (1) is divided into a central area (12) and a side wall area (11) positioned at the periphery of the central area (12), and a plurality of vertical air holes (13) are distributed in the central area (12); the particle diversion device (2) is arranged on the side wall area (11), and the particle diversion device (2) is used for sucking particles deposited on the side wall area (11) and spraying the particles above the gas distribution plate (1) in a horizontal direction or a roughly horizontal direction and at least above the central area (12);
the particle diversion device (2) comprises an air inlet pipe (21), a truncated cone-shaped reducer pipe (27) and a diversion cylinder (22); the side wall area (11) is provided with jet flow air holes (15);
the air inlet pipe (21) is communicated with the jet flow air hole (15) through the cone frustum-shaped reducing pipe (27); the inner diameter of the truncated cone-shaped variable-diameter pipe (27) is gradually reduced along the direction from the joint of the truncated cone-shaped variable-diameter pipe (27) and the air inlet pipe (21) to the joint of the truncated cone-shaped variable-diameter pipe (27) and the jet air hole (15);
the guide cylinder (22) is arranged right above the jet flow air hole (15), an air inlet of the guide cylinder (22) is positioned at the lower end of the guide cylinder and is right opposite to an air outlet of the jet flow air hole (15), and a gap is formed between the air inlet of the guide cylinder (22) and the air outlet of the jet flow air hole (15); the air outlet (25) of the guide shell (22) is arranged to enable air flow to be ejected in a horizontal direction or a roughly horizontal direction.
2. The gas distributor for fluidized beds of silicones according to claim 1, characterized in that the central zone (12) represents 70-80% of the total area of the gas distribution plate (1) and the sidewall zone (11) represents 20-30% of the total area of the gas distribution plate (1).
3. The gas distributor for fluidized beds of silicone according to claim 2, characterized in that the gas distribution plate (1) is circular and the diameter of the gas distribution plate (1) is 0.8-3.5 m.
4. The gas distributor for a fluidized bed of silicone according to claim 1 or 2,
the air inlet of the guide cylinder (22) is coaxial with the air outlet of the jet flow air hole (15), and the vertical distance between the air inlet of the guide cylinder (22) and the air outlet of the jet flow air hole (15) is 5-20 mm.
5. The gas distributor for fluidized beds of organosilicon according to claim 1 or 2, characterized in that the cone angle α of the cone-shaped reducer (27) is 30-60 °.
6. The gas distributor according to claim 1 or 2, wherein the gas outlets of the guide shell (22) are arranged towards the central area (12) and inject a gas flow in a horizontal or substantially horizontal direction.
7. The gas distributor for fluidized beds of silicone according to claim 1 or 2, characterized in that the jet gas holes (15) are divided into a vertical section (16) and a flared section (17) in the vertical direction from bottom to top in sequence.
8. The gas distributor for fluidized beds of silicones, according to claim 7, characterized in that the flaring angle β of the flaring section (17) of the jet air holes (15) is 20-26 °;
the diameter D2 of the vertical section (16) of the jet air hole (15) is 5-9mm, the length L of the vertical section (16) is 2-15mm, and the maximum diameter D3 of the flaring section (17) of the jet air hole (15) is 6-10 mm.
9. A gas distributor according to claim 4, wherein the sidewall area (11) is provided with a plurality of particle deflector devices (2); the particle diversion devices (2) are distributed in a radial shape around the center of the gas distribution plate (1).
10. The gas distributor according to claim 9, wherein the particle deflector devices (2) are arranged at equal intervals, and the particle deflector devices (2) are symmetrically arranged in the sidewall region (11).
11. The gas distributor according to claim 10, wherein each of the particle deflector (2) is symmetrically distributed with respect to the center of the gas distribution plate (1); the side wall area (11) is annular as a whole; the number of the particle diversion devices (2) is 2-16.
12. The gas distributor according to claim 10, wherein the gas flow injection direction of the gas outlets (25) of the guide shell (22) of at least some of the particle guide devices (2) intersects the gas flow injection direction of the vertical gas holes (13) of the central zone (12) above the gas distribution plate (1).
13. The gas distributor for fluidized beds of silicone according to claim 4, characterized in that said inlet pipe (21) comprises an upright pipe section (28) and a horizontal pipe section (29) connected to said upright pipe section (28); the vertical pipe section (28) is connected with the circular truncated cone-shaped reducer pipe (27).
14. The gas distributor for a fluidized bed of silicone according to claim 13,
the diameter D1 of intake pipe (21) is 30-50mm, and the gas inlet pressure of intake pipe (21) is 1.0-1.6 MPa.
15. The gas distributor for fluidized beds of organosilicon according to claim 4, characterized in that the gas inlet of the guide shell (22) is provided as a truncated cone-shaped reducing opening (26), the guide shell (22) comprises a guide vertical pipe section (23) connected with the truncated cone-shaped reducing opening (26) and a guide bent pipe section (24) connected with the guide vertical pipe section (23);
the inner diameter of the truncated cone-shaped reducing port (26) is gradually reduced from bottom to top.
16. The gas distributor for fluidized beds of organosilicon according to claim 15, characterized in that the cone angle γ of the frustoconical reduction (26) is 90-120 °, the maximum diameter D4 of the frustoconical reduction (26) being 40-170 mm;
the diameter D5 of the flow guide vertical pipe section (23) is 20-150mm, and the length L1 of the flow guide vertical pipe section (23) is 50-200 mm;
the included angle delta between the flow guide bent pipe section (24) and the horizontal direction is 30-60 degrees.
17. The gas distributor for fluidized beds of organosilicon according to any of claims 1-2, characterized in that said central zone (12) is uniformly perforated with said vertical air holes (13) of constant diameter, with a hole ratio of 1-5%; the diameter D0 of the vertical air hole (13) is 2-4mm, and the air inlet pressure of the vertical air hole (13) is 0.2-0.5 MPa.
18. A fluidized bed reactor for organosilicon, characterized in that the reactor is equipped with a gas distributor according to any one of claims 1 to 17;
the gas distribution plate (1) of the gas distributor is fixedly arranged in the inner cavity of the reactor; the particle diversion device (2) is fixedly connected with the inner wall of the reactor.
19. The silicone fluidized bed reactor according to claim 18, wherein the gas distribution plate (1) and the reactor lower head (3) are fixedly connected by fasteners.
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