CN101537329A - Fluidized bed reactor and method for synthesizing methyl chlorosilane by using same - Google Patents
Fluidized bed reactor and method for synthesizing methyl chlorosilane by using same Download PDFInfo
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- CN101537329A CN101537329A CN200910029941A CN200910029941A CN101537329A CN 101537329 A CN101537329 A CN 101537329A CN 200910029941 A CN200910029941 A CN 200910029941A CN 200910029941 A CN200910029941 A CN 200910029941A CN 101537329 A CN101537329 A CN 101537329A
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Abstract
The invention relates to the field of environmental protection and chemical industry, in particular to a fluidized bed reactor. In the invention, a gas guiding device is additionally arranged between a distribution plate at the bottom of the fluidized bed reactor and a cylinder. The guiding device comprises a gas distribution pipe, a guiding pipe and a gas distribution flange. The gas distribution pipe comprises at least two sections of elbow pipes, the lower end of each elbow pipe is connected with the guiding pipe, the middle part at the outer end of each section of elbow pipe is connected with a gas inlet, and the other end of the guiding pipe is connected with the gas distribution flange. After the guiding device is additionally arranged, part of material gas can be shunted and tangentially enters a fluidized bed. Tangential gas inlet enables gas in the fluidized bed to be added with tangential speed on the basis of the prior upward axial speed, and gas and carried raw material particles spirally ascends to form a rotational flow field to enable contact time of reaction materials to be prolonged. The invention also relates to a method for synthesizing methyl chlorosilane by using the reactor.
Description
Technical field
The present invention relates to environmental protection and chemical field, be specifically related to a kind of fluidized-bed reactor, the invention still further relates to the method for utilizing this fluidized-bed reactor synthesizing methyl-chloro-silane.
Background technology
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.
During synthesizing methyl-chloro-silane, silica flour and the copper catalyst and the co-catalyst etc. of certain particle size are mixed, formed the composition that contains catalyst.The composition that subsequently this is contained catalyst is sent in the fluidized-bed reactor, makes its reaction, 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 copper catalyst is less relatively, has than big-difference with the silicon powder particle particle diameter.Therefore the principal character at organic silicon monomer 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.Key is the fluidisation problem that will solve wide distributed granule.
Generally conical bed is adopted in the bottom of fluid bed, improve all abundant fluidisation of material that fluidizing velocity makes different-grain diameter, and the amplification section is adopted at the top, makes the gas prompt drop low, thereby makes stream expect to be easy to deposit, and is difficult for being taken out of by gas the load of reduction piece-rate system thereafter.But dozens or even hundreds of heat exchanger tube arranged for very big large-scale fluidized bed of heat of reaction, the adding of heating surface bank, for equal cylinder fluid beds straight, can significantly reduce bed body net sectional area, cause empty tower gas velocity too high, thereby the little particle of granularity is blown easily, particularly in the organic silicon monomer production process, the granularity of catalyst is very little, makes catalyst be blown a body easily, thereby influences course of reaction.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art deficiency, a kind of adaptable fluidized-bed reactor that is applicable to wide particle diameter distribution fluidisation granular system with good guide functions and high conversion is provided.
Fluidized-bed reactor of the present invention, comprise cylindrical shell, be installed in the distribution grid of fluid bed bottom, inlet duct below distribution grid, thimble tube bundle in inner barrel, charge door, the slag-drip opening of bottom and last, bottom head, be connected air flow guiding device 20 16 of distribution grid and bottom cones, the lower end of guiding device is connected with the top of distribution grid 15, its upper end is connected with fluid bed bottom cone, guiding device comprises gas distribution tube 18, mozzle 17 and gas distribution orchid 19, gas distribution tube is made up of 2 sections bend pipes at least, the bend pipe lower end is connected with mozzle, every section bend pipe outer end mid portion is connected with gas feed 11, and the mozzle other end is connected with the distribution of gas flange.See Fig. 1, Fig. 2.
Preferred 1: 2.5～1: 35 of above-mentioned draft-tube diameter and gas distribution tube diameter ratio.
Go up used fluidized-bed reactor size, the preferred 8～200mm of the diameter of mozzle, more preferably 15～120mm by general production.
Go up used fluidized-bed reactor size, the preferred 0.2～2m of mozzle length, more preferably 0.3～1.2m by general production.
Mozzle quantity is 2～120, preferred 10～80.
Mozzle and distribution of gas flanged ends, mozzle are 5 ° of-80 ° of even angle and are distributed on the distribution of gas flange.Preferred angle is 10 °-50 °.
Also the baffle layer can be installed in the cylindrical shell of top, the baffle layer is made of corrugated plating or spiral bar shape plate.See 1 and Fig. 3.The height of baffle layer is looked the 10-80% that the installation site is the cylindrical shell height.The baffle layer can be installed in the expanding reach cylindrical shell of top, also can be installed in the cone of top.
After fluid bed top cylindrical shell is installed the baffle layer, solid particle in the air-flow of rotation rising in the reactor has been played filtration, make unreacted particle return bed again and participate in reaction, increased the granule density in the bed, not only significantly reduce the drag-out of syngas outlet dust and returned the bed amount, the wearing and tearing of consersion unit have been reduced, and improved raw material availability, active constituent content in the product is increased, improved the economic benefit of device, and energy efficient has reduced the pollution of environment to external world.
The present invention has set up air flow guiding device between fluid bed bottom distribution grid and cylindrical shell, the splitter section unstripped gas also tangentially enters fluid bed with this portion gas amount, tangential admission makes the interior gas of fluid bed add tangential velocity on original axial velocity basis that makes progress, the feed particles spiral that makes gas and carry secretly rises, the time lengthening that the rotational flow field of formation makes the reaction mass contact.
The invention also discloses a kind of method for preparing methylchlorosilane, adopt fluidized-bed reactor of the present invention exactly, with accounting for gross weight is that the chloromethanes that 10-90% measures enters from guiding device air inlet 11, all the other methyl chloride gas enter fluid bed by fluid bed bottom air inlet 12, silicon powder particle and copper catalyst and co-catalyst add from fluid bed cylindrical shell charge door 8, solid particle mixes with methyl chloride gas and reacts, and synthesizing methyl-chloro-silane is synthetic discharges through exporting 1.Co-catalyst generally is to be selected from aluminium powder, zinc powder, the glass putty one or more.
Utilize fluid bed of the present invention, the feed particles spiral that makes chloromethanes and carry secretly rises, the rotational flow field that forms makes the time lengthening that silicon powder particle contacts with gas, and the air-flow of rotation not only can be avoided a large amount of particles settlings and withdraw from the Surface Renewal of reacting and can strengthen contact at a high speed, improve the macroreaction speed of methylchlorosilane, improved the device fabrication intensity of fluidized-bed reactor, thereby improved the conversion per pass of chloromethanes, prolong the synthetic production cycle, improved the economic benefit of device.With same supplementary material synthesizing methyl-chloro-silane, if with conventional fluidized-bed reactor, general chloromethanes conversion per pass is 25%, and the dimethyldichlorosilane selectivity is lower than 90%.And adopt fluidized-bed reactor of the present invention to carry out same reaction, and the chloromethanes conversion per pass is greater than 35%, and the dimethyldichlorosilane selectivity is greater than 90%.
Description of drawings
Fig. 1 is a fluidized-bed reactor structural representation of the present invention;
Fig. 2 is a guiding device schematic cross-section of the present invention;
Fig. 3 is a baffle layer cross section schematic diagram of the present invention
Each digitized representation among the figure: 1, syngas outlet, 2, upper cover, 3, the expanding reach cylindrical shell, 4, the baffle layer, 5, top cone, 6, thimble tube heat transferring medium import, 7, thimble tube heat transferring medium outlet, 8, the raw materials mouth, 9, cylindrical shell, 10, thimble tube bundle, 11, raw material gas inlet, 12, raw material gas inlet, 13, slag-drip opening, 14, low head, 15, distribution grid, 16, the bottom cone, 17, mozzle, 18, gas distribution tube, 19, the distribution of gas flange, 20, the unstripped gas guiding device.
The specific embodiment
Embodiment 1
Fluidized-bed reactor
As Fig. 1 and Fig. 2, fluidized-bed reactor comprises cylindrical shell 9, expanding reach cylindrical shell 3, top cone 5, be installed in the distribution grid 15 of fluid bed bottom, inlet duct 12 below distribution grid is a raw material gas inlet, thimble tube bundle 10 in inner barrel, charge door 8, the slag-drip opening 13 and the top end socket 2 of bottom, bottom head 14, guiding device is installed in the middle of distribution grid 15 and the thimble tube bundle 10, the lower end of guiding device is connected with the top of distribution grid 15, its upper end is connected with the fluid bed cylindrical shell, guiding device comprises gas distribution tube 18, mozzle 17 and gas distribution orchid 19, gas distribution tube 18 is made up of 2 sections bend pipes at least, be connected with mozzle 17 in the bend pipe lower end, every section bend pipe outer end mid portion is connected with gas feed 11, and the mozzle other end is connected with the distribution of gas flange.
Embodiment 2
Synthesizing methyl-chloro-silane
As the fluidized-bed reactor of embodiment 1,20 of mozzles, mozzle 17 is 30 ° with the angle of distribution grid flange, and mozzle length is 50mm, and caliber DN is 20mm, and the caliber DN of gas distribution tube is 100mm.Regulate unstrpped gas chloromethanes gross weight 35% enter from fluid bed bottom air inlet 12, gas flow rate is 0.4m/s, form the air-flow of axial flow, remain 65% methyl chloride gas by gas feed 11 air inlets, gas flow rate is 30m/s, make air-flow on original axial velocity basis, add tangential velocity, when temperature is 280 ℃, raw silicon powder particles and copper catalyst and co-catalyst are added from fluid bed raw materials mouth 8, thereby cause the shape rising in the shape of a spiral of unstrpped gas entrained solids particle, entire reaction course feed particles and catalyst etc. and unstrpped gas prolong time of contact.
The chloromethanes conversion per pass is 35.2%, and the dimethyldichlorosilane selectivity is 91.5%.
Embodiment 3
Synthesizing methyl-chloro-silane
As the fluid bed of embodiment 1, baffle layer 4 is installed in fluid bed, the baffle layer is installed in the cylindrical shell top cone 5, and the height of baffle layer is 30% of a top cone height.Guiding device is installed in intrafascicular of distribution grid and thimble tube, 36 of mozzles, and the angle of mozzle and distribution grid flange is 10 °, and mozzle length is 50mm, and caliber DN is 20mm, and the caliber DN of gas distribution tube is 150mm.Regulating 50% of methyl chloride gas enters from fluid bed bottom air inlet 12, gas flow rate is 0.35m/s, form the air-flow of axial flow, remain 50% methyl chloride gas by gas feed 11 air inlets, gas flow rate is 20m/s, make air-flow on original axial velocity basis, add tangential velocity, when temperature is 310 ℃, raw silicon powder particles and copper catalyst and co-catalyst are added from fluid bed raw materials mouth 8, thereby cause the shape rising in the shape of a spiral of unstrpped gas entrained solids particle, the rising unstripped gas is met the baffle layer at expanding reach, and the part particle returns bed again and participates in reaction, and entire reaction course feed particles and catalyst etc. prolong with unstrpped gas time of contact.
The chloromethanes conversion per pass is 36.1%, and the dimethyldichlorosilane selectivity is 92.2%.
Embodiment 4
Synthesizing methyl-chloro-silane
As the fluidized-bed reactor of embodiment 1, be followed successively by upper cover 2, expanding reach cylindrical shell 3, baffle layer 4, top cone 5, cylindrical shell 9, thimble tube bundle 10, unstripped gas guiding device 20, distribution grid 15, bottom head 14 and inlet duct 12 from top to bottom.The baffle layer is installed in expanding reach cylindrical shell 3 bottoms in the fluid bed, and the height of baffle layer is 30% of an expanding reach cylindrical shell height.20 of mozzles, the angle of mozzle and distribution grid flange is 30 °, and mozzle length is 50mm, and caliber DN is 20mm, and the caliber DN of gas distribution tube is 100mm.Regulating 35% of unstrpped gas chloromethanes enters from fluid bed bottom air inlet 12, gas flow rate is 0.4m/s, form the air-flow of axial flow, remain 65% unstrpped gas by the side direction air inlet, gas flow rate is 30m/s, make air-flow on original axial velocity basis, add tangential velocity, when reaction temperature is 330 ℃, raw silicon powder particles and copper catalyst and co-catalyst are added from fluid bed raw materials mouth 8, thereby cause the shape rising in the shape of a spiral of unstrpped gas entrained solids particle, the rising unstripped gas is met the baffle layer at expanding reach, and the part particle returns bed again and participates in reaction, and entire reaction course feed particles and catalyst etc. prolong with unstrpped gas time of contact.
The chloromethanes conversion per pass is 40.6%, and the dimethyldichlorosilane selectivity is 91.8%.
Claims (8)
1, a kind of fluidized-bed reactor, comprise cylindrical shell, the expanding reach cylindrical shell, last lower cone, be installed in the distribution grid of fluid bed bottom, inlet duct below distribution grid, thimble tube bundle in inner barrel, charge door, the slag-drip opening of bottom and last, bottom head, it is characterized in that: between distribution grid and bottom cone (16), be connected air flow guiding device (20), the lower end of guiding device is connected with the top of distribution grid (15), its upper end is connected with the fluid bed cylindrical shell, guiding device comprises gas distribution tube (18), mozzle (17) and gas distribution orchid (19), gas distribution tube is made up of 2 sections bend pipes at least, the bend pipe lower end is connected with mozzle, every section bend pipe outer end mid portion is connected with gas feed (11), and the mozzle other end is connected with the distribution of gas flange.
2, fluidized-bed reactor according to claim 1 is characterized in that: draft-tube diameter and gas distribution tube diameter ratio are 1: 2.5～1: 35.
3, fluidized-bed reactor according to claim 1 is characterized in that: mozzle quantity is 2～120.
4, fluidized-bed reactor according to claim 1 is characterized in that: draft-tube diameter is 8～200mm.
5, fluidized-bed reactor according to claim 1 is characterized in that: mozzle length is 0.2～2m.
6, fluidized-bed reactor according to claim 1 is characterized in that: mozzle and distribution of gas flanged ends, mozzle are 5 °～80 ° even angle and are distributed on the distribution of gas flange.
7, fluidized-bed reactor according to claim 1 is characterized in that: the top cylindrical shell is installed the baffle layer, and the baffle layer is made of corrugated plating or spiral bar shape plate.
8, a kind of method for preparing methylchlorosilane, it is characterized in that: the fluidized-bed reactor that utilizes claim 1, with accounting for gross weight is that the chloromethanes that 10-90% measures enters from guiding device air inlet (11), all the other methyl chloride gas enter fluid bed by fluid bed bottom air inlet (12), silicon powder particle and copper catalyst and co-catalyst add from fluid bed cylindrical shell charge door (8), mix with methyl chloride gas and react, the methylchlorosilane mixture is discharged through outlet (1).
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| CN2009100299417A CN101537329B (en) | 2009-03-24 | 2009-03-24 | Fluidized bed reactor and method for synthesizing methyl chlorosilane by using same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276641A (en) * | 2011-09-15 | 2011-12-14 | 江苏弘博新材料有限公司 | Method for producing methylchlorosilane |
| CN103055769A (en) * | 2012-12-24 | 2013-04-24 | 南京工业大学 | Organic silicon monomer fluidized bed membrane reactor and process thereof |
| CN106749380A (en) * | 2017-02-23 | 2017-05-31 | 镇江江南化工有限公司 | A kind of methyl chlorosilane monomer synthesizes circulating reaction system |
| CN108138992A (en) * | 2015-10-05 | 2018-06-08 | 各星有限公司 | For the isostatic pressing formed graphite liner of fluidized-bed reactor |
| CN109701459A (en) * | 2019-01-18 | 2019-05-03 | 淮阴工学院 | A kind of uniform inlet duct of fluidized-bed reactor |
| CN109821483A (en) * | 2019-03-28 | 2019-05-31 | 合盛硅业股份有限公司 | The automatic continuous adding method of catalyst and device |
| CN110982072A (en) * | 2019-12-21 | 2020-04-10 | 安徽科翌新材料有限公司 | Preparation method of magnesium-calcium ramming liquid binder |
| CN115430370A (en) * | 2022-09-30 | 2022-12-06 | 浙江开化合成材料有限公司 | Chlorosilane synthesizer |
-
2009
- 2009-03-24 CN CN2009100299417A patent/CN101537329B/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276641A (en) * | 2011-09-15 | 2011-12-14 | 江苏弘博新材料有限公司 | Method for producing methylchlorosilane |
| CN103055769A (en) * | 2012-12-24 | 2013-04-24 | 南京工业大学 | Organic silicon monomer fluidized bed membrane reactor and process thereof |
| CN103055769B (en) * | 2012-12-24 | 2015-04-22 | 南京工业大学 | Organic silicon monomer fluidized bed membrane reactor and process thereof |
| CN108138992A (en) * | 2015-10-05 | 2018-06-08 | 各星有限公司 | For the isostatic pressing formed graphite liner of fluidized-bed reactor |
| CN106749380A (en) * | 2017-02-23 | 2017-05-31 | 镇江江南化工有限公司 | A kind of methyl chlorosilane monomer synthesizes circulating reaction system |
| CN106749380B (en) * | 2017-02-23 | 2020-04-07 | 镇江江南化工有限公司 | Methyl chlorosilane monomer synthesis circulation reaction system |
| CN109701459A (en) * | 2019-01-18 | 2019-05-03 | 淮阴工学院 | A kind of uniform inlet duct of fluidized-bed reactor |
| CN109821483A (en) * | 2019-03-28 | 2019-05-31 | 合盛硅业股份有限公司 | The automatic continuous adding method of catalyst and device |
| CN110982072A (en) * | 2019-12-21 | 2020-04-10 | 安徽科翌新材料有限公司 | Preparation method of magnesium-calcium ramming liquid binder |
| CN115430370A (en) * | 2022-09-30 | 2022-12-06 | 浙江开化合成材料有限公司 | Chlorosilane synthesizer |
| CN115430370B (en) * | 2022-09-30 | 2023-10-20 | 浙江开化合成材料有限公司 | Chlorosilane synthesizer |
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