CN103570025A - Silicon powder recycling device for producing silicon tetrachloride through direct method - Google Patents
Silicon powder recycling device for producing silicon tetrachloride through direct method Download PDFInfo
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Abstract
The invention relates to a silicon powder recycling device for producing silicon tetrachloride through a direct method. The silicon powder recycling device comprises a cyclone separation device and a cloth-bag dust collector, wherein the cyclone separation device comprises a primary cyclone separator and a secondary cyclone separator, the fixed inner wall of each of the primary cyclone separator and the secondary cyclone separator is respectively provided with a hexsteel, and corundum is respectively arranged on a lining of each hexsteel; a feeding port of the primary cyclone separator is connected with a fluidized bed reactor for producing the silicon tetrachloride, the primary cyclone separator is connected with the secondary cyclone separator, both the primary cyclone separator and the secondary cyclone separator are respectively connected to the fluidized bed reactor in a backflow manner, and an air outlet on the upper part of the secondary cyclone separator is connected with the cloth-bag dust collector. By adopting the silicon powder recycling device, a majority of silicon powder can be recycled, the dust removal in the subsequent process can be avoided, the utilization efficiency of raw materials can be improved, and the selectivity of the silicon tetrachloride in a crude product is more than 95 percent.
Description
Technical field
The invention belongs to organosilane monomer synthesis technical field, relate in particular to the silica powder recovering device that a kind of direct method is produced silicon tetrachloride.
Background technology
Silicon tetrachloride, molecular formula: SiCl
4, for colourless, be corrosive, non-combustible liquid, have suffocative stink.While being exposed to wet air, form dense smoke, hydrogenchloride is emitted in hydrolysis rapidly.57.6 ℃ of boiling points.Fusing point-70.0 ℃.Can be used for manufacturing silicoorganic compound, as thermal silica, tetraethoxy, organic silicone oil, high-temperature insulation paint, silicone resin, silicon rubber and heat resistant pad lining material.High purity silicon tetrachloride is for manufacturing the material of polysilicon, high-purity silicon dioxide and inorganic silicon compound, silica fiber, and war industry is for the manufacture of NC mixture, and metallurgical industry is for the manufacture of corrosion-resistant ferrosilicon, and foundary industry is used as releasing agent etc.At present, the impact of photovoltaic industry external owing to being subject to " two anti-", almost in the situation of being annihilated, the raw material trichlorosilane device of polysilicon, also almost in full end-of-life state, only has few device to move in carry-deficit, and this has just caused the silicon tetrachloride as by-product of this industry fewer and feweri, silicon tetrachloride becomes tight pin product by the by product of giving it up, price, from freely, increases to more than 4000 yuan/ton, and also can't buy on market.
Publication number be the Chinese patent of CN102712485A disclose a kind of by organic compound combustion generate electricity ash that manufacture technique produces, preferably organic compound combustion is converted to ignition energy under the existence of the grey carbonaceous material that the generating set of electric power produces to the method for the silicon-containing material chlorination production silicon tetrachloride that by silicon-containing material, preferably contains silicic acid biomass.Publication number is that the Chinese patent of CN102686514A also discloses a kind of granulation body and chlorine, oxygen that utilizes silicon-dioxide and carbonaceous material to form and carries out common chlorination reaction, generate the chlorinating step of silicon tetrachloride, and then silicon tetrachloride is generated to polysilicon with reductive agent metallic reducing.It is a kind of by the mixture of fine and/or unbodied silicon-dioxide, carbon and energy donor being changed to manufacture with chlorine the method for silicon tetrachloride that publication number is that the Chinese patent of CN101472839 also discloses.Energy donor is Pure Silicon Metal or silicon alloy, and the interpolation of donor has realized the thermopositive reaction of self-supporting on the one hand, has caused on the other hand showing of reacting initial temperature to be reduced.
Patent USP4490344, USP4604272, USP4847059, DE3438444/A1 and EP00077138 are by adding the mode of catalyzer, reduce chlorine, silicon-dioxide and carbon reaction and produce the method for the temperature of silicon tetrachloride, main group and the chlorine-containing compound of subgroup, preferably boron trichloride and phosphoryl chloride etc. that the catalyzer using is the periodic table of elements the 5th.
Publication number is that the Chinese patent of CN1114559C discloses and a kind ofly by by least having the chlorosilane of a HSi key in silicon, ferro-alloy metal or molecule, reacts under catalyst action with hydrogenchloride, thereby highly selective is produced the method for silicon tetrachloride.The invention provides a kind of catalyzer of manufacturing the method for silicon tetrachloride comprises at least one periodictable VIII family's metallic element or its compound and is a kind ofly selected from periodictable VB family's period 3 and under the mixture of the element simple substance in cycle exists subsequently, makes at least to have in silicon metal or molecule chlorosilane and the hcl reaction of a HSi key.USP3754077, USP4130632 disclose a kind of silicon, aluminium alloy and hydrogenchloride or chlorine gas of utilizing and have reacted, and generate the method for trichlorosilane or silicon tetrachloride.USP4980143 has introduced a kind of reaction with silica flour at hydrogenchloride in the process that generates trichlorosilane and silicon tetrachloride mixture, by changing the reaction conditionss such as temperature, can improve the content of silicon tetrachloride in mixed chlorosilane.Owing to there are a plurality of chlorosilane components in reaction process in these, later separation purifying process step is comparatively loaded down with trivial details.
The people such as the Fu Xuehong (research of the synthetic silicon tetrachloride of abandoned catalyst in direct synthesis methylchlorosilane, organosilicon material, 2011, 25(6): 397-401, the 13 Chinese organosilicon seminar collection of thesis in 2006), Yan Shicheng (the research of the synthetic silicon tetrachloride new technology of abandoned catalyst in direct synthesis methylchlorosilane, Northeast Electric Power University's journal, 2010, 30(6): 36-39.) Chinese patent CN1465524A etc. has introduced with (75% the Si of the waste catalyst in methyl chlorosilane monomer production process, 10 ~ 15% Cu) be main raw material, in the fluidized-bed reactor that is 600mm at diameter, synthesize the method for silicon tetrachloride with chlorine generation gas-solid reaction.
Applicant has applied for Chinese invention patent (number of patent application: 2013103609093, patent application day: 2013-8-19) disclose a kind of production equipment that utilizes direct method to produce silicon tetrachloride, this device comprises chlorine generating unit, silica flour feeding device, fluidized-bed reactor, cyclone separator, fiber bag precipitator, spray column and soda-wash tower, chlorine generating unit connects the inlet mouth of fluidized-bed reactor, silica flour feeding device connects the charging opening of fluidized-bed reactor, the skin of fluidized-bed reactor is provided with heating jacket, the air outlet on fluidized-bed reactor top is connected with interchanger, the discharge port of interchanger connects cyclone separator, the discharge gate of cyclone separator bottom refluxes respectively and is connected to described fluidized-bed reactor, the air outlet on cyclone separator top connects described fiber bag precipitator, the air outlet on fiber bag precipitator top connects described spray column, the air outlet on spray column top is connected with condenser, the discharge port of condenser is connected with silicon tetrachloride crude product storage tank, described silicon tetrachloride crude product storage tank connects described rectifier unit, the air outlet of described condenser connects described soda-wash tower.
Summary of the invention
The object of this invention is to provide a kind of direct method and produce the silica powder recovering device of silicon tetrachloride, this device is recycled silica flour in silicon tetrachloride crude product gas effectively, improves the prepared using efficiency of knowing clearly.
In order to realize above-mentioned object, the present invention has adopted following technical scheme:
A kind of direct method is produced the silica powder recovering device of silicon tetrachloride, this device comprises cyclone separator and fiber bag precipitator, described cyclone separator comprises primary cyclone and secondary cyclone, the fixedly inwall of described primary cyclone and secondary cyclone is provided with hexsteel, is lined with corundum in hexsteel; The opening for feed of primary cyclone connects the fluidized-bed reactor of producing silicon tetrachloride, the air outlet on primary cyclone top connects described secondary cyclone, the discharge gate of primary cyclone and secondary cyclone bottom refluxes respectively and is connected to described fluidized-bed reactor, and the air outlet on secondary cyclone top connects described fiber bag precipitator; Described fiber bag precipitator comprises body skin and a plurality of cloth bag device, in body skin, be provided with dividing plate, dividing plate is divided into dedusting chamber and outlet chamber by body skin, outer side wall in dedusting chamber is provided with heating jacket, and above dedusting chamber, be provided with fly-ash separator inlet mouth, fly-ash separator inlet mouth connects the air outlet on secondary cyclone top, in dedusting chamber, the inner side of fly-ash separator inlet mouth, is provided with gas block panel; Described a plurality of cloth bag devices all adopt high temperature resistant material, and cloth bag device is fixedly installed on dividing plate, and dust outlet is set in the bottom in dedusting chamber, and dust outlet below is provided with fine powder withdrawing can, and the sidewall of described outlet chamber is provided with fly-ash separator air outlet.
As preferably, described fiber bag precipitator is also connected with cloth bag pulsed dust-removing device, cloth bag pulsed dust-removing device comprises compressed air tank, a plurality of Venturi meter, pulse control instrument and a plurality of pulse valve, described a plurality of pulse valves are arranged on a plurality of pipelines that are connected to compressed air tank and by pulse control instrument, are controlled respectively, a plurality of Venturi meters connect described a plurality of pipelines, and the air outlet of a plurality of Venturi meters is connected respectively to the inside of described cloth bag device.
As preferably, described fiber bag precipitator is also provided with pressure detection module, and described pressure detection module is connected with pulse control instrument.
As preferably, described heating jacket adopts heat-conducting oil heating, on the top of heating jacket, is provided with oil-in, and bottom is provided with oil outlet.
As preferably, the top in described dedusting chamber is right cylinder, and bottom is cone, at the outer side wall of cone, is provided with access hole.
The present invention is owing to having adopted above-mentioned technical scheme, the two-stage dedusting of the cyclone separator that the silica flour of the silicon tetrachloride crude product gas of producing for fluidized-bed reactor first passes through, most silica flour is recycled, how for thinner silica flour a small amount of in gas crude product, by sack cleaner, to reclaim, like this can most of silica flour of removing silicon tetrachloride crude product gas, avoided carrying out in subsequent technique dedusting, improved prepared using efficiency high, in crude product, silicon tetrachloride selectivity is more than 95% simultaneously.
Accompanying drawing explanation
Fig. 1 is the structural representation of silicon tetrachloride production equipment of the present invention.
Fig. 2 is the structural representation of cyclone separator.
Fig. 3 is the vertical view of Fig. 2.
Fig. 4 is the structural representation of sack cleaner.
Fig. 5 is the vertical view of Fig. 4.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is made a detailed explanation.
A kind of production equipment that utilizes direct method to produce silicon tetrachloride as shown in Figure 1, this device comprises liquid chlorine storage tank 1, chlorine liquid carburetor 3, silica flour feeding device 5, fluidized-bed reactor 6, primary cyclone 10, secondary cyclone 11, fiber bag precipitator 12, spray column 14, soda-wash tower 18 etc.Wherein between the entrance of the outlet of liquid chlorine storage tank 1 and chlorine liquid carburetor 3, with canned-motor pump 2, be connected, be convenient to carrying out continuously of reaction.Between chlorine liquid carburetor 3 and fluidized-bed reactor 6, be connected with vacuum buffer tank 4, be convenient to stable being passed in fluidized-bed reactor 6 of gas velocity of the chlorine after vaporization.Described silica flour feeding device 5 is connected with nitrogen pipeline 21 above, and nitrogen pipeline 21 is provided with valve, by valve, is controlled and continuously silica flour is added to fluidized-bed reactor 6 bottoms.Fluidized-bed reactor adopts the heating jacket of oil bath heating, and heating jacket is provided with thermal oil entrance 8 and thermal oil outlet 7.The air outlet on fluidized-bed reactor 6 tops is connected with interchanger 9, and the discharge port of interchanger 9 connects described primary cyclone 10.As shown in Figure 2 and Figure 3, the air outlet on primary cyclone 10 tops connects described secondary cyclone 11, and the discharge gate of primary cyclone 10 and secondary cyclone 11 bottoms refluxes respectively and is connected to described fluidized-bed reactor 6.Fluidized-bed reactor 6 outlet products are after interchanger 9 coolings, gas crude product is after primary cyclone 10 is separated with secondary cyclone 11, and the most of solid fine silica powder in gas crude product reclaims to enter in fluidized-bed reactor 6 and continues as raw material reaction.The air outlet on described secondary cyclone 11 tops connects described fiber bag precipitator 12, the bottom of fiber bag precipitator 12 is connected with fine powder withdrawing can 13, makes thinner silica flour a small amount of in gas crude product by entering fine powder withdrawing can 13 after sack cleaner 12 recovery.Sack cleaner 12 outlet products enter spray column 14, the SiCl of spray liquid for using through the condensed partial reflux of condenser 16
4crude product, the air outlet on spray column 14 tops is connected with condenser 16, and the discharge port of condenser 16 connects branch line, and branch line one end is connected with silicon tetrachloride crude product storage tank 17, the other end connects the shower nozzle of described spray column 14, and spray column 14 bottoms are the high slag slurry storage tank 15 that boils of liquid.The SiCl of silicon tetrachloride crude product storage tank 17 for gathering
4crude product, can be used for further rectification and purification and uses.Condenser 16 unreacted is out chlorine gas mixture completely, generates the products such as clorox through soda-wash tower 18 with NaOH solution reaction, and product clorox enters clorox storage tank 19 and collects, and other noncondensable gas is discharged through drain 20.
As shown in Figure 4, described fiber bag precipitator 12 comprises body skin 21 and a plurality of cloth bag device 32, in body skin 21, be provided with dividing plate 22, dividing plate 22 is divided into dedusting chamber 23 and outlet chamber 24 by body skin 21, outer side wall in dedusting chamber 23 is provided with heating jacket 29, heating jacket 29 adopts heat-conducting oil heating, on the top of heating jacket 29, be provided with oil-in 30, bottom is provided with oil outlet 31, because silicon tetrachloride crude product gas is being lowered the temperature through primary cyclone 10 and secondary cyclone 11, if temperature is too low in fiber bag precipitator, can condense into liquid and stop up cloth bag device 32, therefore need to keep silicon tetrachloride crude product gas to mend by heating jacket 29 condenses.The top in dedusting chamber 23 is right cylinder, bottom is cone, the top in dedusting chamber 23 is provided with fly-ash separator inlet mouth 25, fly-ash separator inlet mouth 25 connects the air outlet on secondary cyclone 11 tops, in dedusting chamber, the inner side of fly-ash separator inlet mouth 25 23, be provided with gas block panel 36, at the outer side wall of cone, be provided with access hole 28.Described a plurality of cloth bag devices 32 all adopt high temperature resistant material, cloth bag device 32 is fixedly installed on dividing plate 22, dust outlet 27 is set in the bottom in dedusting chamber 23, and dust exports 27 belows and is provided with fine powder withdrawing can 13, and the sidewall of described outlet chamber 24 is provided with fly-ash separator air outlet 26.
As shown in Figure 5, described fiber bag precipitator 12 is also connected with cloth bag pulsed dust-removing device, cloth bag pulsed dust-removing device comprises compressed air tank 33, a plurality of Venturi meter 35, pulse control instrument and a plurality of pulse valve 34, described a plurality of pulse valves 34 are arranged on a plurality of pipelines that are connected to compressed air tank and by pulse control instrument, are controlled respectively, a plurality of Venturi meters 35 connect described a plurality of pipelines, and the air outlet of a plurality of Venturi meters 35 is connected respectively to the inside of described cloth bag device 32.And being also provided with pressure detection module at fiber bag precipitator 12, described pressure detection module is connected with pulse control instrument.In the process that dusty gas purifies by filter bag, along with the increase of time, the long-pending dust being attached on cloth bag device 32 is more and more, thereby the resistance of cloth bag device 32 is increased gradually, cause processing air quantity to reduce gradually, for normal operation, control resistance within the specific limits, by pressure detection module, detect the pressure in fiber bag precipitator, at this moment when pressure is raised to limited range, by pulse control instrument, send instruction and trigger in order each control valve unbalanced pulse valve, pressurized air in gas bag is ejected in each corresponding cloth bag device 32 by each aperture Venturi meter 35 of injection tube, 32 moments of cloth bag device sharply expand, make the long-pending dust releasing that is attached to cloth bag device 32 surfaces, cloth bag device 32 is regenerated.
Principle of work of the present invention is: the liquid chlorine in liquid chlorine storage tank 1 is input in chlorine liquid carburetor 3 and vaporizes to certain temperature through canned-motor pump 2, chlorine gas regulates laggard fluidized-bed reactor 6 bottoms that enter by surge tank 4, directly reacts in fluidized-bed reactor 6 with the raw material silica flour from silica flour feeding device 5.Fluidized-bed reactor 6 outlet crude products are after one-level cyclonic separation 10 is separated with secondary cyclone 11, and the most of solid fine silica powder in gas crude product reclaims to enter in fluidized-bed reactor 6 and continues as raw material reaction.In gas crude product, a small amount of thinner silica flour enters fine powder withdrawing can 13 after reclaiming by sack cleaner 12.Sack cleaner 12 outlet products enter spray column 14, the SiCl of spray liquid for using through the condensed partial reflux of condenser 16
4crude product, spray column 14 bottoms are the high slag slurry storage tank 15 that boils of liquid.The SiCl of storage tank 17 for gathering
4crude product, can be used for further rectification and purification and uses.Condenser 16 unreacted is out chlorine gas mixture completely, generates the products such as clorox through soda-wash tower 18 with NaOH solution reaction, and product clorox enters storage tank 19 and collects, and other noncondensable gas is discharged through drain 20.
Claims (5)
1. a direct method is produced the silica powder recovering device of silicon tetrachloride, it is characterized in that: this device comprises cyclone separator (10,11) and fiber bag precipitator (12), described cyclone separator (10,11) comprises primary cyclone (10) and secondary cyclone (11), the fixedly inwall of primary cyclone (10) and secondary cyclone (11) is provided with hexsteel, is lined with corundum in hexsteel, the opening for feed of primary cyclone (10) connects the fluidized-bed reactor (6) of producing silicon tetrachloride, the air outlet on primary cyclone (10) top connects described secondary cyclone (11), the discharge gate of primary cyclone (10) and secondary cyclone (11) bottom refluxes respectively and is connected to described fluidized-bed reactor (6), and the air outlet on secondary cyclone (11) top connects described fiber bag precipitator (12), described fiber bag precipitator (12) comprises body skin (21) and a plurality of cloth bag device (32), in body skin (21), be provided with dividing plate (22), dividing plate (22) is divided into dedusting chamber (23) and outlet chamber (24) by body skin (21), outer side wall in dedusting chamber (23) is provided with heating jacket (29), and be provided with fly-ash separator inlet mouth (25) in the top of dedusting chamber (23), fly-ash separator inlet mouth (25) connects the air outlet on secondary cyclone (11) top, in the dedusting chamber, inner side (23) of fly-ash separator inlet mouth (25), be provided with gas block panel (36), described a plurality of cloth bag devices (32) all adopt high temperature resistant material, cloth bag device (32) is fixedly installed on dividing plate (22), dust outlet (27) is set in the bottom of dedusting chamber (23), dust outlet (27) below is provided with fine powder withdrawing can (13), and the sidewall of described outlet chamber (24) is provided with fly-ash separator air outlet (26).
2. a kind of direct method according to claim 1 is produced the silica powder recovering device of silicon tetrachloride, it is characterized in that: fiber bag precipitator (12) is also connected with cloth bag pulsed dust-removing device, cloth bag pulsed dust-removing device comprises compressed air tank (33), a plurality of Venturi meters (35), pulse control instrument and a plurality of pulse valve (34), described a plurality of pulse valves (34) are arranged on a plurality of pipelines that are connected to compressed air tank (33) and by pulse control instrument, are controlled respectively, a plurality of Venturi meters (35) connect described a plurality of pipelines, the air outlet of a plurality of Venturi meters (35) is connected respectively to the inside of described cloth bag device (32).
3. a kind of direct method according to claim 2 is produced the silica powder recovering device of silicon tetrachloride, it is characterized in that: fiber bag precipitator (12) is also provided with pressure detection module, and described pressure detection module is connected with pulse control instrument.
4. a kind of direct method according to claim 1 is produced the silica powder recovering device of silicon tetrachloride, it is characterized in that: heating jacket (29) adopts heat-conducting oil heating, on the top of heating jacket (29), be provided with oil-in (30), bottom is provided with oil outlet (31).
5. a kind of direct method according to claim 1 is produced the silica powder recovering device of silicon tetrachloride, it is characterized in that: the top of dedusting chamber (23) is right cylinder, and bottom is cone, at the outer side wall of cone, is provided with access hole (28).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112210669A (en) * | 2020-09-04 | 2021-01-12 | 鲁西化工集团股份有限公司硅化工分公司 | Continuous purification device and process for organic silicon copper-containing contact |
| CN114409695A (en) * | 2022-01-26 | 2022-04-29 | 云南能投硅材科技发展有限公司 | Comprehensive utilization method of waste silicon powder in organic silicon monomer synthesis process |
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