CN1321731C - Reactor of organic silicon fluidized bed with cyclone separator - Google Patents
Reactor of organic silicon fluidized bed with cyclone separator Download PDFInfo
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- CN1321731C CN1321731C CNB2005100492346A CN200510049234A CN1321731C CN 1321731 C CN1321731 C CN 1321731C CN B2005100492346 A CNB2005100492346 A CN B2005100492346A CN 200510049234 A CN200510049234 A CN 200510049234A CN 1321731 C CN1321731 C CN 1321731C
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Abstract
The present invention discloses an organic silicon fluidized bed reactor with cyclone separators, which is composed of an upper closed head, an upper cylinder body, a lower conical body, a gas predistribution chamber and a lower closed head, wherein a blast cap type gas distribution board is arranged between the lower conical body and the gas predistribution chamber; a silicon powder feed inlet and a returned material feed inlet are arranged outside the lower conical body; a raw material gas inlet is arranged outside the gas predistribution chamber; a drooping finger-shaped sleeve pipe bundle is arranged below the upper closed head; the first cyclone separator and the second cyclone separator which are respectively arranged in the upper closed head or on the outer top of the upper closed head are connected; an inlet of the first cyclone separator is connected with the reactor; each outlet of the bottom ends of the two cyclone separators is respectively provided with a particle discharge pipe; the bottom end of each particle discharge pipe is provided with a conical plug; the top end of the second cyclone separator is provided with a synthetic gas outlet. Due to the adoption of the inner cyclone separator or the outer cyclone separator, the present invention can effectively fluidize wide screening particles, enhances heat exchange by a spiral diversion type finger-shaped heat exchange pipe inner members, and is suitable for wide screening fluidized particle systems and gas-solid phase fluidized bed reactions.
Description
Technical field
The present invention relates to technical field of chemical, especially relate to a kind of organosilicon fluidized bed reactor that is applicable to the band cyclone separator of wide-size distribution fluidized particles system and strong heat release.
Background technology
Organic silicon monomer (methylchlorosilane) adopts the Rochow direct method synthetic usually, and the solid material in the synthetic reaction is a silicon powder particle, and catalyst is a copper powder particle, and chloromethanes and gaseous reaction products play the effect of fluidizing agent, Gu course of reaction is gas-solid-reaction.The methylchlorosilane of unreacted chloromethanes, gaseous state, the byproduct of gaseous state, catalyst component and fine dust leave reactor.Silica flour and copper powder fully contact and effectively withdraw from reaction heat to reaction important influence, the therefore industrial production of all adopting the continuous fluid bed bioreactor to realize methylchlorosilane.In order to obtain the selectivity of high as far as possible target product (dimethyldichlorosilane M2), not only need high as far as possible productive rate (the formed silane quantity of time per unit and reaction volume), and need the reliable and elastic operation of high as far as possible silicon conversion ratio and whole factory.
Problem one: particle diameter distributes wide, reduces with the reaction particle diameter, and fine powder and catalyst easily are blown;
Silicon powder particle itself has very wide particle diameter and distributes, and in process of production, silica flour is constantly consumed, and particle diameter changes, and constantly replenishes fresh silica flour to reactor simultaneously.In addition, the particle diameter of catalyst copper powder is less relatively, has than big-difference with the silica flour particle diameter.Therefore, the principal character of organosilicon fluidized bed reactor is that the solid grain size distribution is wide, contains more fine powder, needs to realize the abundant mixing of different-grain diameter particle.
In U.S. Pat-A4281149, introduced and comprised reactor, be furnished with the main cyclone separator of EGR and the system that is furnished with the back cyclone separator of dust collecting container.In the method, carry out surface treatment, subsequently again in the Returning reactor with being deposited in the cyclone separator of back the part of particulate.Like this, can reach very high silicon conversion ratio.The gaseous flow of leaving cyclone separator often still contains residual dust, and before carrying out the methylchlorosilane distillation, this dust must be separated.U.S. Pat-A4328353 once advised: the gaseous flow of the cyclone separator of flowing through is carried out hot gas filtration, and the flour of gained loops back in the reactor or discharges, and need not further processing.Also once disclosed hot gas filtration among European patent EP-A-900802, then the gained particulate had been circulated.
Adopt the reactor external cyclone, atomic fine dust directly can be sent in the fluid bed reactor of synthetic chlorosilane or methylchlorosilane, but external cyclone insulation difficulty cause temperature of charge to reduce easily, and returning charge has considerable influence to the fluid bed bottom fluidization.In addition, these atomic thin dry silica flours be very easy to air and atmosphere in moisture react, that is when factory's operation was broken down, dieseling can take place in this product accident ingress of air.
Problem two: strong exothermal reaction
Be used for the gas and solid phase catalyzing exothermic reaction of chemical industry to the temperature requirement sensitivity, particularly be applied to produce the organosilicon important source material dimethyldichlorosilane synthesizer of (being called for short M2), this reaction is strong exothermal reaction (280kJ/mol).
Patent CN 2456835Y introduces existing M2 resultant current fluidized bed reactor two kinds, a kind of half cone bed bioreactor for water evaporation heat-obtaining; Another kind is the cylindrical bed reactor of simple oil heat-obtaining.The no heat-obtaining face conversion zone of suitable thickness is arranged at the half cone bed bottom of the half cone bed bioreactor of water evaporation heat-obtaining.It is to adopt to add water to finger-type nest of tubes bottom intermittence (or inhomogeneous), boiled water evaporation in very short zone, and the end of water evaporating area is cooled to contact (catalyst+silica flour) material below the reaction temperature.Bed particle up all is lower than reaction temperature again, and synthetic reaction does not take place these contacts.This class reactor production capacity is low, and bed end temperature fluctuation is frequent, and the steam flow of generation is extremely unstable, so be difficult to this part heat energy of comprehensive utilization.
The oil circulation heat-obtaining unit scale of the cylindrical bed reactor of simple oil heat-obtaining is big, and start-up time is long, and naked light is arranged, oily pre-heating system complexity, during operation, for just the wet attitude chloromethanes that prevents to collapse be preheating near entering the cylindrical bed reactor after the reaction temperature.The characteristics of oil heat-obtaining are that upper and lower heat-obtaining intensity differs very few.Though higher heat-obtaining intensity helps preventing strong reaction zone temperature runaway, make reaction zone very short, contact drops to soon and is lower than reaction temperature, so the chloromethanes conversion per pass is low during the simple oil heat-obtaining, the plant investment height, energy resource consumption and operating cost are big.
The direct method synthesizing methyl-chloro-silane is a strong exothermal reaction, for in time discharging the reaction liberated heat, U type pipe or thimble tube generally all are set as heat exchange structure in fluid bed, the every pipe that present U type pipe that uses or thimble tube have is connected with outer tube separately, what have organizes with several Guan Weiyi, is connected with outer tube then.
Summary of the invention
The purpose of this invention is to provide a kind of organosilicon fluidized bed reactor that is applicable to the band cyclone separator of wide-size distribution fluidized particles system and strong heat release.
The technical solution adopted for the present invention to solve the technical problems is:
The present invention includes successively and constitute by upper cover, simplified, up big and down small pre-distributing chamber of bottom cone, gas and the low head in top.Blast cap formula gas distribution grid is housed between the pre-distributing chamber of bottom cone and gas, the bottom cone is equipped with silica flour charge door, feed back charge door outward, the pre-outdoor raw material gas inlet that is equipped with that distributes of gas, droop thimble tube bundle is equipped with in upper cover below, is contained in the flexible supporting frames of top in simplified and supports droop thimble tube bundle; First, second particulate emission pipe is inserted into the bottom cone and is supported by flexible supporting frames, and first, second particulate emission pipe bottom is equipped with the taper plug; First cyclone separator that all is contained in the outer top of upper cover links to each other with second cyclone separator, the import of first cyclone separator is communicated with reactor, first order cyclone separator top exit links to each other with second level cyclone separator import, first, second particulate emission pipe is equipped with in first cyclone separator and the outlet of the second cyclone separator bottom respectively, and the top of second cyclone separator is a syngas outlet.
1. this reactor adopts cyclone separator to make reaction formed and by the fine dust that product is carried outside, can be used again effectively.The advantage that adopts inner cyclone separator is exactly to help prolonging the fine silica powder and the time of staying of copper powder catalyst in reactor, and need not to add in addition the insulation measure.In order to reduce the wearing and tearing of cyclone separator, also can adopt cyclone separator is installed in the outer top of reactor, it need be incubated measure, and the particulate emission pipe of cyclone separator is directly got back to reactor bottom from reactor head, need not to add in addition the insulation measure.
2. heat transferring medium (desalted water or heat exchange oil) enters the dactylethrae heat exchange component from reactor head, and (heat exchange oil still flows out with liquid state) discharged in vaporization after heat exchange, and steam or heat exchange oil are concentrated and discharged.Heat transferring medium evenly can be distributed, also make things convenient for the amplification design of reactor simultaneously.Adopt the spiral stream guidance formula finger-type heat exchanger tube inner member of innovation in addition, heat exchange efficiency is improved.
Can reach optimized mode of operation by above design and the concrete parameter of local adjustment.
The useful effect that the present invention has is:
Owing to adopt internal cyclone separators or external cyclone, so fluidized-bed reactor of the present invention can effectively be handled the fluidisation of solid with wide range particle; Adopt spiral stream guidance formula finger-type heat exchanger tube inner member, enhanced heat exchange; Be applicable to the big gas-solid of wide-size distribution fluidized particles system and thermal discharge fluidized-bed reaction mutually.
Description of drawings
Fig. 1 is the straight tube of the conical bottom fluidized-bed reactor structural representation of installation internal cyclone separators of the present invention;
Fig. 2 is the straight tube of the conical bottom fluidized-bed reactor structural representation of the outer whirlwind separator of installation of the present invention;
Fig. 3 is a spiral stream guidance formula dactylethrae heat exchange inner member structural representation of the present invention.
Among the figure: 1, syngas outlet, 2, second cyclone separator, 3, the import of thimble tube heat transferring medium, 4, the outlet of thimble tube heat transferring medium, 5, droop thimble tube bundle, 6, the top cylindrical shell, 7, the second particulate emission pipe, 8, the bottom cone, 9, the feed back charge door, 10, blast cap formula gas distribution grid, 11, the pre-distributing chamber of gas, 12, low head, 13, raw material gas inlet, 14, the silica flour charge door, 15, the taper plug, 16, the first particulate emission pipe, 17, first cyclone separator, 18, upper cover, 19, flexible supporting frames, 20, the first cyclone separator import, 21, outlet, 22, pipe in the heat exchanger tube, 23, spiral deflector, 24, import, 25, the heat exchanger tube outer tube.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
As shown in Figure 1 and Figure 2, the present invention includes successively and constitute by upper cover 18, top cylindrical shell 6, up big and down small pre-distributing chamber 11 of bottom cone 8, gas and low head 12.Blast cap formula gas distribution grid 10 is equipped with in 11 of the pre-distributing chamber of bottom cone 8 and gas, bottom cone 8 outer silica flour charge door 14, the feed back charge doors 9 of being equipped with, the pre-distributing chamber of the gas 11 outer raw material gas inlet 13 that are equipped with, droop thimble tube bundle 5 is equipped with in upper cover 18 belows, and the flexible supporting frames 19 that is contained in the top simplified 6 supports droop thimble tube bundle 5; All be contained in the upper cover 18, or first cyclone separator 17 that all is contained in upper cover 18 outer tops links to each other with second cyclone separator 2,2 imports link to each other first order cyclone separator 17 top exits with second level cyclone separator, the import 20 of first cyclone separator 17 is communicated with reactor, first cyclone separator 17 and the outlet of second cyclone separator, 2 bottoms are equipped with first respectively, the second particulate emission pipe 16,7, first, the second particulate emission pipe 16,7 are inserted into bottom cone 8 and are supported by flexible supporting frames 19, first, the second particulate emission pipe 16, the top that 7 bottoms are equipped with taper plug 15, the second cyclone separators 2 is a syngas outlet 1.
As shown in Figure 3, described droop thimble tube bundle 5 is made up of pipe 22 and heat exchanger tube outer tube 25 in the heat exchanger tube, is wound with spiral deflector 23 between pipe 22 and the heat exchanger tube outer tube 25 in the heat exchanger tube.
The top cylindrical shell 6 of described reactor highly is 3～20 meters, and cylindrical shell 6 diameters in top are 0.5～6 meter.The height of bottom cone 8 can be 1～4 meter, and cone angle can be 5～30 °;
After unstripped gas (chloromethanes) preheating through raw material gas inlet 13 back the pre-distributing chamber 11 of gas in to around distribution, enter blast cap formula gas distribution grid 10 then, distribution of gas is even.The percent opening of blast cap formula gas distribution grid 10, perforate number, nozzle angle degree and aperture, the structural parameters and the bed pressure drop of association reaction device come optimal design, guarantee that fluidized-bed reactor is in the optimization mode of operation.
Solid reaction raw material (silica flour and copper powder catalyst) adds reactor in advance, by reacting after the unstripped gas fluidisation.The gas-phase reaction product is discharged from syngas outlet 1.Need the fresh silica flour that replenishes in reaction, enter reactor from silica flour charge door 14, the fine grained that reclaims from external separator is from feed back charge door 9 Returning reactors.The synthetic required silica flour of direct method had specific particle diameter before synthetic, preferably be no more than 2000 microns, more preferably no more than 500 microns.The synthesis gas that generates in this reaction comprises gaseous silane, other gaseous reaction products, unreacted chloromethanes and contains silica soot, and synthesis gas enters by the first cyclone separator import 20 and enters first cyclone separator 17.Separate the back to the small part dust by the first inner cyclone separator 17 and send into fluid bed bottom cone 8 reaction zones by end toper plug 15 under the first particulate emission pipe 16 and the particulate emission pipe, the unsegregated dust of part enters second cyclone separator 2 again separate after, send into fluid bed bottom cone 8 reaction zones by the second particulate emission pipe 7, the remaining dust that can't separate leaves fluidized-bed reactor by the syngas outlet 1 at the second cyclone separator top.In the method, even very fine contain silica soot and also can be handled safely, total thereby can reach high silicon conversion ratio.During synthesizing methyl-chloro-silane, can avoid shortcomings such as selectivity attenuating and reactor operating time shortening.
Described fluidized-bed reactor inside is equipped with many droop dactylethrae heat exchange components 5, is used to shift out reaction heat.The introducing of droop dactylethrae heat exchange component 5 can be so that this fluidized-bed reactor be specially adapted to the reaction system of strong heat release.The dactylethrae distribution mode of droop dactylethrae heat exchange component 5 can adopt equilateral triangle or square uniform, and the top is fixed by welding on the ring flange of reactor head, and the bottom adopts flexible supporting frames 19 to locate diametrically.Reasonably the dactylethrae distribution mode can effectively play the effect of bubble crushing, raising fluidizing performance.Heat exchange can be adopted the mode of desalted water vaporization, perhaps adopts the mode of conduction oil heat exchange.Can adjust the number of heat exchange component according to actual exchange capability of heat.Fig. 3 is a spiral stream guidance formula dactylethrae heat exchange inner member structural representation of the present invention.Heat transferring medium (desalted water or conduction oil) evenly flows into every finger-type heat exchanger tube from thimble tube heat transferring medium import 3, as shown in Figure 3, by carrying out heat exchange in the helix chuck between the pipe 22 in import 24 inflow finger-type heat exchanger tube outer tubes 25 and the heat exchanger tube, steam or conduction oil enter and manage 22 in the heat exchanger tube after heat exchange, discharge from exporting 21, import thimble tube heat transferring medium outlet 4 again and flow out fluidized-bed reactor.
Claims (2)
1, a kind of organosilicon fluidized bed reactor with cyclone separator is made of upper cover (18), top cylindrical shell (6), up big and down small bottom cone (8), the pre-distributing chamber of gas (11) and low head (12) successively; Between bottom cone (8) and the pre-distributing chamber of gas (11) blast cap formula gas distribution grid (10) is housed, outer silica flour charge door (14), the feed back charge door (9) of being equipped with of bottom cone (8), the outer raw material gas inlet (13) that is equipped with of the pre-distributing chamber of gas (11), droop thimble tube bundle (5) is equipped with in upper cover (18) below, and the flexible supporting frames (19) that is contained in the top cylindrical shell (6) supports droop thimble tube bundle (5); First, second particulate emission pipe (16,7) is inserted into bottom cone (8) and is supported by flexible supporting frames (19), and first, second particulate emission pipe (16,7) bottom is equipped with taper plug (15); It is characterized in that: first cyclone separator (17) that all is contained in the outer top of upper cover (18) links to each other with second cyclone separator (2), the import (20) of first cyclone separator (17) is communicated with reactor, import links to each other first cyclone separator (17) top exit with second cyclone separator (2), first, second particulate emission pipe (16,7) is equipped with in first cyclone separator (17) and the outlet of second cyclone separator (2) bottom respectively, and the top of second cyclone separator (2) is syngas outlet (1).
2, a kind of organosilicon fluidized bed reactor according to claim 1 with cyclone separator, it is characterized in that: described droop thimble tube bundle (5) is made up of pipe (22) and heat exchanger tube outer tube (25) in the heat exchanger tube, is wound with spiral deflector (23) between pipe (22) and the heat exchanger tube outer tube (25) in the heat exchanger tube.
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| CNB2005100492346A CN1321731C (en) | 2005-01-26 | 2005-01-26 | Reactor of organic silicon fluidized bed with cyclone separator |
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| CNB2005100492346A CN1321731C (en) | 2005-01-26 | 2005-01-26 | Reactor of organic silicon fluidized bed with cyclone separator |
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| CN1321731C true CN1321731C (en) | 2007-06-20 |
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| CN100341614C (en) * | 2006-08-29 | 2007-10-10 | 闫慧光 | Organosilicon fluidized bed reactor |
| CN101125858B (en) * | 2007-09-05 | 2011-04-13 | 青岛科技大学 | Method for directly reclaiming catalyst of organic silicon monomer fluidized bed reactor and device thereof |
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| CN110283202B (en) * | 2018-03-19 | 2021-03-23 | 浙江新安化工集团股份有限公司 | System and method for preparing methylphosphonite from aluminum methylchloride |
| CN110283205B (en) * | 2018-03-19 | 2021-03-23 | 浙江新安化工集团股份有限公司 | System and method for preparing methylphosphonite |
| CN109482120A (en) * | 2018-12-14 | 2019-03-19 | 南通三圣石墨设备科技股份有限公司 | Graphite heat exchanger and method built in a kind of novel reaction kettle |
| CN110449093B (en) * | 2019-09-11 | 2024-01-26 | 江苏江锅智能装备股份有限公司 | Fluidization reaction system |
| CN113351129B (en) * | 2021-04-29 | 2022-12-20 | 湖北君邦新材料科技有限公司 | Organic silicon thermal synthesis equipment |
| CN114832730B (en) * | 2022-05-06 | 2023-08-01 | 聊城市鲁西化工工程设计有限责任公司 | Fluidized bed reaction device and method for synthesizing organochlorosilane monomer |
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| CN2494698Y (en) * | 2001-07-24 | 2002-06-12 | 中蓝晨光化工研究院 | Fluid bed reactor |
| CN1382690A (en) * | 2001-04-12 | 2002-12-04 | 瓦克化学有限公司 | Dust circulation when directly synthetizing silane chhloride and silane methyl chloride in fluidized bed |
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2005
- 2005-01-26 CN CNB2005100492346A patent/CN1321731C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4281149A (en) * | 1980-03-24 | 1981-07-28 | General Electric Company | Process for treating silicon particles within a silicone reactor system |
| CN1052688A (en) * | 1989-12-18 | 1991-07-03 | 中国石油化工总公司洛阳石油化工工程公司 | The two-stage oxidizing regenerative method of fluid catalyst |
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| CN2494698Y (en) * | 2001-07-24 | 2002-06-12 | 中蓝晨光化工研究院 | Fluid bed reactor |
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Assignee: Zhejiang Kaihua Synthetic Materials Co., Ltd. Assignor: Zhejiang University| Zhejiang Xin'an chemical industry group, Limited by Share Ltd Contract record no.: 2011330000802 Denomination of invention: Reactor of organic silicon fluidized bed with cyclone separator Granted publication date: 20070620 License type: Exclusive License Open date: 20051012 Record date: 20110624 |