CN103449445B - A kind of direct method produces the production equipment of silicon tetrachloride - Google Patents
A kind of direct method produces the production equipment of silicon tetrachloride Download PDFInfo
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- CN103449445B CN103449445B CN201310360909.3A CN201310360909A CN103449445B CN 103449445 B CN103449445 B CN 103449445B CN 201310360909 A CN201310360909 A CN 201310360909A CN 103449445 B CN103449445 B CN 103449445B
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Abstract
The present invention relates to a kind of production equipment utilizing 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 fluidized-bed reactor, silica flour feeding device connects fluidized-bed reactor, fluidized-bed reactor top is connected with interchanger, interchanger connects cyclone separator, the discharge gate of cyclone separator bottom refluxes respectively and is connected to fluidized-bed reactor, the air outlet on cyclone separator top connects fiber bag precipitator, the air outlet on fiber bag precipitator top connects 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, silicon tetrachloride crude product storage tank connects rectifier unit, the air outlet of condenser connects soda-wash tower.Apparatus of the present invention structure is simple, and raw material utilization efficiency is high, and in crude product, silicon tetrachloride selectivity is more than 95%.
Description
Technical field
The invention belongs to organosilane monomer synthesis technical field, particularly relate to the production equipment that a kind of direct method produces silicon tetrachloride.
Background technology
Silicon tetrachloride, molecular formula: SiCl
4, for colourless, be corrosive, non-combustible liquid, have suffocative stink.Form dense smoke when being exposed to wet air, hydrogenchloride is released in hydrolysis rapidly.Boiling point 57.6 DEG C.Fusing point-70.0 DEG C.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 the material manufacturing 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, photovoltaic industry is due to the impact by external " two anti-", almost be in the situation of being annihilated, the raw material trichlorosilane device of polysilicon is also almost in full end-of-life state, and only have few device to run in carry-deficit, the silicon tetrachloride as by-product which results in this industry is fewer and feweri, silicon tetrachloride is become by the by product of giving it up tightly sells product, price, from freely, increases to more than 4000 yuan/ton, and market also can't buy.
Publication number is under the existence of the carbonaceous material of the ash that ash, the generating set that preferably ignition energy converted by organic compound combustion to electric power that the Chinese patent of CN102712485A discloses a kind of manufacture technique that generated electricity by organic compound combustion and produces produce, by silicon-containing material, the method for silicon-containing material chlorination production silicon tetrachloride preferably containing silicic acid biomass.Publication number be the Chinese patent of CN102686514A then also disclose a kind of utilize silicon-dioxide and carbonaceous material to form granulation body and chlorine, oxygen carry out common chlorination reaction, generate the chlorinating step of silicon tetrachloride, and then silicon tetrachloride reductive agent metallic reducing is generated polysilicon.Publication number is that the Chinese patent of CN101472839 also discloses a kind of method by use chlorine, the transformation of the mixture of fine and/or unbodied silicon-dioxide, carbon and energy donor being manufactured silicon tetrachloride.Energy donor is Pure Silicon Metal or silicon alloy, the interpolation of donor achieves the thermopositive reaction of self-supporting on the one hand, result in showing of reacting initial temperature on the other hand to reduce.
Patent USP4490344, USP4604272, USP4847059, DE3438444/A1 and EP00077138 are then by adding the mode of catalyzer, reduce the method that the temperature of silicon tetrachloride is produced in the reaction of chlorine, silicon-dioxide and carbon, the main group of catalyzer for the periodic table of elements the 5th used and the chlorine-containing compound of subgroup, preferably boron trichloride and phosphoryl chloride etc.
Publication number is that the Chinese patent of CN1114559C discloses a kind of chlorosilane by least having a HSi key in silicon, ferro-alloy metal or molecule, react, thus highly selective produces the method for silicon tetrachloride with hydrogenchloride under catalyst action.The invention provides a kind of catalyzer manufacturing the method for silicon tetrachloride comprises under at least one periodictable VIII race's metallic element or its compound and a kind of mixture being selected from periodictable VB race's period 3 and the element simple substance in cycle subsequently thereof exist, and makes chlorosilane and the hcl reaction at least in silicon metal or molecule with a HSi key.USP3754077, USP4130632 then disclose one and utilize silicon, aluminium alloy and hydrogenchloride or chlorine gas to react, and generate the method for trichlorosilane or silicon tetrachloride.USP4980143 then describes and a kind ofly reacts in the process generating trichlorosilane and silicon tetrachloride mixture at hydrogenchloride and silica flour, by changing the reaction conditionss such as temperature, can improve the content of silicon tetrachloride in mixed chlorosilane.Owing to there is multiple chlorosilane component in reaction process in these, later separation purification process step is comparatively loaded down with trivial details.
The people such as the Fu Xuehong (research of abandoned catalyst in direct synthesis methylchlorosilane synthesis silicon tetrachloride, organosilicon material, 2011, 25(6): 397-401, 13 Chinese organosilicon seminar collection of thesis in 2006), Yan Shicheng (the research of abandoned catalyst in direct synthesis methylchlorosilane synthesis silicon tetrachloride new technology, Northeast Electric Power University's journal, 2010, 30(6): 36-39.) Chinese patent CN1465524A etc. describe with the waste catalyst (Si of 75% in methyl chlorosilane monomer production process, the Cu of 10 ~ 15%) be main raw material, be synthesize the method for silicon tetrachloride with chlorine generation gas-solid reaction in the fluidized-bed reactor of 600mm at diameter.
Summary of the invention
In order to solve above-mentioned technical problem, the object of this invention is to provide the production equipment that a kind of direct method produces silicon tetrachloride, this apparatus structure is simple, and raw material utilization efficiency is high, and in crude product, silicon tetrachloride selectivity is more than 95%.
In order to realize above-mentioned object, present invention employs following technical scheme:
Utilize direct method to produce a production equipment for 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 fiber bag precipitator described in the connection of air outlet on cyclone separator top, the spray column described in the connection of air outlet on fiber bag precipitator top, 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, rectifier unit described in described silicon tetrachloride crude product storage tank connects, the soda-wash tower described in the connection of air outlet of described condenser.
As preferably, the bottom of described fiber bag precipitator is connected with thin powder recovery tank; The bottom of described spray column is connected with slag slurry storage tank.
As preferably, the discharge port of described condenser connects branch line, the silicon tetrachloride crude product storage tank described in branch line one end connects, the shower nozzle of the spray column described in the other end connects.
As preferably, described cyclone separator comprises primary cyclone and secondary cyclone, the secondary cyclone described in the connection of air outlet on primary cyclone top, the discharge gate of primary cyclone and secondary cyclone bottom refluxes respectively and is connected to described fluidized-bed reactor, the fiber bag precipitator described in the connection of air outlet on secondary cyclone top.
As preferably, described chlorine generating unit comprises liquid chlorine storage tank, chlorine liquid carburetor and vacuum buffer tank, is provided with canned-motor pump and is connected between the outlet of described liquid chlorine storage tank and the entrance of chlorine liquid carburetor, the vacuum buffer tank described in chlorine liquid carburetor connects.
As preferably, be connected with nitrogen pipeline above described silica flour feeding device, nitrogen pipeline is provided with valve, silica flour is added fluidized-bed reactor bottom.
As preferably, described heating jacket adopts oil bath heating, and heating jacket is provided with thermal oil entrance and thermal oil outlet.
As preferably, described heating jacket adopts oil bath heating, and heating jacket is provided with thermal oil entrance and thermal oil outlet.
The present invention, owing to have employed above-mentioned technical scheme, achieves and adopts chlorine and silica flour direct production silicon tetrachloride, and this apparatus structure is simple, and raw material utilization efficiency is high, and in crude product, silicon tetrachloride selectivity is more than 95%.
Accompanying drawing explanation
Fig. 1 is the structural representation of production equipment of the present invention.
1-liquid chlorine storage tank; 2-canned-motor pump; 3-chlorine liquid carburetor; 4-surge tank; 5-silica flour feeding device; 6-fluidized-bed reactor; 7-thermal oil exports; 8-heat conductive oil inlet; 9-interchanger; 10-primary cyclone; 11-secondary cyclone; 12-fiber bag precipitator; 13-thin powder recovery tank; 14-spray column; 15-slag slurry withdrawing can; 16-condenser; 17-silicon tetrachloride crude product storage tank; 18-soda-wash tower; 19-clorox storage tank; 20-drain.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is made a detailed explanation.
A kind of production equipment utilizing 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 be connected with canned-motor pump 2 between the outlet of liquid chlorine storage tank 1 and the entrance of chlorine liquid carburetor 3, what be convenient to react carries out continuously.Be connected with vacuum buffer tank 4 between chlorine liquid carburetor 3 and fluidized-bed reactor 6, be convenient to stable being passed in fluidized-bed reactor 6 of gas velocity of the chlorine after vaporizing.Described silica flour feeding device 5 is connected with nitrogen pipeline 21 above, and nitrogen pipeline 21 is provided with valve, silica flour is added fluidized-bed reactor 6 bottom continuously by Valve controlling.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 top is connected with interchanger 9, the primary cyclone 10 described in discharge port connection of interchanger 9, the secondary cyclone 11 described in the connection of air outlet on primary cyclone 10 top, the discharge gate of primary cyclone 10 and secondary cyclone 11 bottom refluxes respectively and is connected to described fluidized-bed reactor 6.Fluidized-bed reactor 6 outlets products is after interchanger 9 is lowered the temperature, 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 fiber bag precipitator 12 described in the connection of air outlet on described secondary cyclone 11 top, the bottom of fiber bag precipitator 12 is connected with thin powder recovery tank 13, enters thin powder recovery tank 13 after thinner silica flour a small amount of in gas crude product is then reclaimed by sack cleaner 12.Sack cleaner 12 outlets products enters spray column 14, and spray liquid is the SiCl through the condensed partial reflux of condenser 16
4crude product, the air outlet on spray column 14 top 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 shower nozzle of the spray column 14 described in the other end connects, boil for liquid is high bottom spray column 14 slag slurry storage tank 15.Silicon tetrachloride crude product storage tank 17 is the SiCl gathered
4crude product, can be used for further rectification and purification and uses.Condenser 16 unreacted out chlorine gas mixture completely, react through soda-wash tower 18 and NaOH solution products such as generating clorox, product clorox enters clorox storage tank 19 and collects, and other noncondensable gas is discharged through drain 20.
Principle of work of the present invention is: the liquid chlorine in liquid chlorine storage tank 1 is input to through canned-motor pump 2 temperature that in chlorine liquid carburetor 3, vaporization is extremely certain, chlorine gas by surge tank 4 regulate laggard enter bottom fluidized-bed reactor 6, directly react in fluidized-bed reactor 6 with the raw material silica flour from silica flour feeding device 5.Fluidized-bed reactor 6 exports crude product after one 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.Thinner silica flour a small amount of in gas crude product enters thin powder recovery tank 13 after then being reclaimed by sack cleaner 12.Sack cleaner 12 outlets products enters spray column 14, and spray liquid is the SiCl through the condensed partial reflux of condenser 16
4crude product, boil for liquid is high bottom spray column 14 slag slurry storage tank 15.Storage tank 17 is the SiCl gathered
4crude product, can be used for further rectification and purification and uses.Condenser 16 unreacted out chlorine gas mixture completely, react through soda-wash tower 18 and NaOH solution products such as generating clorox, product clorox enters storage tank 19 and collects, and other noncondensable gas is discharged through drain 20.
Claims (6)
1. utilize direct method to produce a production equipment for silicon tetrachloride, it is characterized in that: this device comprises chlorine generating unit, silica flour feeding device (5), fluidized-bed reactor (6), cyclone separator (10,11), fiber bag precipitator (12), spray column (14) and soda-wash tower (18), chlorine generating unit connects the inlet mouth of fluidized-bed reactor (6), silica flour feeding device (5) connects the charging opening of fluidized-bed reactor (6), the skin of fluidized-bed reactor (6) is provided with heating jacket, the air outlet on fluidized-bed reactor (6) top is connected with interchanger (9), the discharge port of interchanger (9) connects cyclone separator (10, 11), cyclone separator (10, 11) discharge gate of bottom refluxes respectively and is connected to described fluidized-bed reactor (6), cyclone separator (10, 11) fiber bag precipitator (12) described in the connection of air outlet on top, described cyclone separator comprises primary cyclone (10) and secondary cyclone (11), the secondary cyclone (11) described in the connection of air outlet on primary cyclone (10) top, the discharge gate of primary cyclone (10) and secondary cyclone (11) bottom refluxes respectively and is connected to described fluidized-bed reactor (6), the fiber bag precipitator (12) described in the connection of air outlet on secondary cyclone (11) top, the spray column (14) described in the connection of air outlet on fiber bag precipitator (12) top, the air outlet on spray column (14) top is connected with condenser (16), the discharge port of condenser (16) is connected with silicon tetrachloride crude product storage tank (17), the discharge port of described condenser (16) connects branch line, silicon tetrachloride crude product storage tank (17) described in branch line one end connects, the shower nozzle of the spray column (14) described in the other end connects, the soda-wash tower (18) described in the connection of air outlet of described condenser (16).
2. a kind of production equipment utilizing direct method to produce silicon tetrachloride according to claim 1, is characterized in that: the bottom of fiber bag precipitator (12) is connected with thin powder recovery tank (13).
3. a kind of production equipment utilizing direct method to produce silicon tetrachloride according to claim 1, is characterized in that: the bottom of described spray column (14) is connected with slag slurry storage tank (15).
4. a kind of production equipment utilizing direct method to produce silicon tetrachloride according to claim 1, it is characterized in that: chlorine generating unit comprises liquid chlorine storage tank (1), chlorine liquid carburetor (3) and vacuum buffer tank (4), be provided with canned-motor pump (2) between the outlet of described liquid chlorine storage tank (1) and the entrance of chlorine liquid carburetor (3) to be connected, the vacuum buffer tank (4) described in chlorine liquid carburetor (3) connects.
5. a kind of production equipment utilizing direct method to produce silicon tetrachloride according to claim 1, it is characterized in that: silica flour feeding device (5) is connected with nitrogen pipeline (21) above, nitrogen pipeline (21) is provided with valve, silica flour is added fluidized-bed reactor (6) bottom.
6. a kind of production equipment utilizing direct method to produce silicon tetrachloride according to claim 1, it is characterized in that: heating jacket adopts oil bath heating, heating jacket is provided with thermal oil entrance (8) and thermal oil outlet (7).
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106946225A (en) * | 2017-05-19 | 2017-07-14 | 河北冀衡集团有限公司 | A kind of fluidized bed plant and method for producing chlorine monoxide |
| CN107416841B (en) * | 2017-06-22 | 2020-07-07 | 唐山三孚硅业股份有限公司 | Method and device for producing silicon tetrachloride |
| JP6941243B2 (en) * | 2018-12-27 | 2021-09-29 | 株式会社トクヤマ | Method for producing chlorosilanes |
| CN110817884A (en) * | 2019-12-10 | 2020-02-21 | 唐山三孚硅业股份有限公司 | Silicon tetrachloride synthetic furnace of high conversion |
| CN111268683B (en) * | 2019-12-30 | 2023-10-27 | 武汉新硅科技潜江有限公司 | Reaction ignition device and ignition method for preparing silicon tetrachloride by chlorination of silicon powder |
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| JP2002173313A (en) * | 2000-12-04 | 2002-06-21 | Denki Kagaku Kogyo Kk | Method for producing silicon tetrachloride |
| CN1465524A (en) * | 2002-06-28 | 2004-01-07 | 中国石油天然气股份有限公司 | SiC1 synthesized by waste contact4Method (2) |
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| BR9002380A (en) * | 1990-05-17 | 1991-11-19 | Fundacao Centro Tecnologico De | PROCESS AND EQUIPMENT FOR SYNTHESIS OF CHLOROSILANS IN A FLUIDIZED BED TYPE REACTOR |
| JP2002173313A (en) * | 2000-12-04 | 2002-06-21 | Denki Kagaku Kogyo Kk | Method for producing silicon tetrachloride |
| CN1465524A (en) * | 2002-06-28 | 2004-01-07 | 中国石油天然气股份有限公司 | SiC1 synthesized by waste contact4Method (2) |
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