CN204125180U - Process the system of thick trichlorosilane - Google Patents
Process the system of thick trichlorosilane Download PDFInfo
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- CN204125180U CN204125180U CN201420524551.3U CN201420524551U CN204125180U CN 204125180 U CN204125180 U CN 204125180U CN 201420524551 U CN201420524551 U CN 201420524551U CN 204125180 U CN204125180 U CN 204125180U
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Abstract
The utility model discloses a kind of system processing thick trichlorosilane, this system comprises: air-lift device; First purifying plant, has liquid outlet at the bottom of the first material inlet, the first overhead gas outlet and the first tower; Second purifying plant, have liquid outlet at the bottom of the second material inlet, the second overhead gas outlet and the second tower, the second material inlet exports with the first overhead gas and is connected; Mixing device, mixing device and liquid at the bottom of the first tower export to export with the second overhead gas and are connected; Anti-disproportionation device, has mixture entrance, the outlet of anti-disproportionation products and filter cap; 3rd purifying plant, has liquid outlet at the bottom of 3 material entrance and the 3rd tower; 4th purifying plant, have liquid outlet at the bottom of 4 materials entrance, the 4th overhead gas outlet and the 4th tower, 4 materials entrance export with liquid at the bottom of the second tower respectively to export with liquid at the bottom of the 3rd tower and is connected, and liquid at the bottom of the 4th tower exports and is connected with the first material inlet.This system effectively can solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane.
Description
Technical field
The utility model belongs to technical field of polysilicon production, and specifically, the utility model relates to a kind of system processing thick trichlorosilane.
Background technology
Synthesis in polysilicon production process, reduction and cold hydrogenation unit all can produce a certain amount of by product dichlorosilane, especially to be reduced to master.Dichlorosilane compared with trichlorosilane, easier reduction furnace wall on precipitate, produce amorphous silica powder, therefore to strictly control dichlorosilane below finite concentration.In actual production process, in reduction recovery trichlorosilane, the content of dichlorosilane reaches 9 ~ 11%, causes reduction furnace easily occur atomizating phenomenon in process of production and produce more unformed silicon, badly influences the normal operation of reduction furnace.Simultaneously because the boiling point of dichlorosilane is close with boron impurity, up-to-standard for ensureing trichlorosilane products, just trichlorosilane purifying column non-condensable gas need be disposed to three wastes operation drip washing process, but still containing a large amount of lower boiling chlorosilane in non-condensable gas, direct drip washing causes the problems such as material consumption is high, environmental protection pressure is large, increases production run cost.
Therefore, the thick trichlorosilane technology of existing process is further improved.
Utility model content
The utility model is intended to solve one of technical problem in correlation technique at least to a certain extent.For this reason, an object of the present utility model is to propose a kind of system processing thick trichlorosilane, and this system effectively can solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and can significantly improve trichlorosilane quality.
In one of the present utility model, the utility model proposes a kind of system processing thick trichlorosilane, comprising:
Air-lift device, described air-lift device has thick trichlorosilane entrance, mixture outlet and impurities outlet;
First purifying plant, described first purifying plant has liquid outlet at the bottom of the first material inlet, the first overhead gas outlet and the first tower, and wherein, described first material inlet is connected with described mixture outlet;
Second purifying plant, described second purifying plant has liquid outlet at the bottom of the second material inlet, the second overhead gas outlet and the second tower, and wherein, described second material inlet exports with described first overhead gas and is connected;
Mixing device, described mixing device has opening for feed and discharge port, and wherein, described opening for feed exports with liquid at the bottom of described first tower respectively to export with the second overhead gas and is connected;
Anti-disproportionation device, described anti-disproportionation device has mixture entrance and the outlet of anti-disproportionation products, and wherein, described mixture entrance is connected with described discharge port;
3rd purifying plant, described 3rd purifying plant has liquid outlet at the bottom of 3 material entrance, the 3rd overhead gas outlet and the 3rd tower, and wherein, described 3 material entrance exports with described anti-disproportionation products and is connected; And
4th purifying plant, described 4th purifying plant has liquid outlet at the bottom of 4 materials entrance, the 4th overhead gas outlet and the 4th tower, wherein, described 4 materials entrance exports with liquid at the bottom of described second tower respectively to export with liquid at the bottom of the 3rd tower and is connected, and liquid outlet at the bottom of described 4th tower is connected with described first material inlet.
The impurity containing boron phosphoric close with dichlorosilane boiling point in thick trichlorosilane removes by adopting air-lift device by the system according to the thick trichlorosilane of the process of the utility model embodiment, then pure dichlorosilane and silicon tetrachloride can be obtained by purifying plant, thus prepare high-quality trichlorosilane by anti-disproportionation device, in anti-disproportionation device, adopt the ion exchange resin of load as catalyzer simultaneously, not easily run off because this catalyzer has, not easy in inactivation, low price, easily and the advantage such as product separation, and carrier itself also can catalyzed reaction, thus significantly processing cost can be reduced while raising raw material availability, in addition, before carrying out anti-disproportionation reaction, the Homogeneous phase mixing in mixing device by dichlorosilane and silicon tetrachloride in advance, contacting between dichlorosilane with silicon tetrachloride can be increased, and then the transformation efficiency of dichlorosilane and silicon tetrachloride can be significantly improved, thus solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and obtain high-quality trichlorosilane.
In addition, following additional technical characteristic can also be had according to the system of the thick trichlorosilane of the process of the utility model above-described embodiment:
In embodiments more of the present utility model, described air-lift device is gas stripping column, and described gas stripping column is made up of upper column and bottom tower two portions, wherein, the internal diameter of described upper column is 500 ~ 600mm, and stage number is 10 pieces, the internal diameter of described bottom tower is 1400 ~ 1600mm, and stage number is 20 pieces.Thus, can effectively remove in thick trichlorosilane containing boron phosphoric impurity.
In embodiments more of the present utility model, described first purifying plant is purification tower, and described purification tower is tray column, and the tower internal diameter of described tray column is 2800 ~ 3000mm, and stage number is 100 ~ 120 pieces.Thus, effectively can be separated and obtain silicon tetrachloride.
In embodiments more of the present utility model, described second purifying plant is purification tower, and described purification tower is tray column, and the stage number of described tray column is 80 ~ 100 pieces.Thus, being separated of dichlorosilane and trichlorosilane can effectively be realized.
In embodiments more of the present utility model, described mixture entrance is positioned at the bottom of described anti-disproportionation device.Thus, feed stock conversion can be significantly improved.
In embodiments more of the present utility model, described 3rd purifying plant is purification tower, and described purification tower is packing tower, and described packing tower is regular wire packing, and total volume is 36.5m
3.Thus, the lower-boiling impurity in anti-disproportionation products can effectively be removed.
In embodiments more of the present utility model, described 4th purifying plant is purification tower, and described purification tower is packing tower, and described packing tower is regular wire packing, and total volume is 300 ~ 400m
3.Thus, can be separated and obtain high-quality trichlorosilane.
Accompanying drawing explanation
Fig. 1 is the system architecture schematic diagram of the thick trichlorosilane of process according to the utility model embodiment;
Fig. 2 is the method flow schematic diagram of the thick trichlorosilane of system implementation process utilizing the thick trichlorosilane of the process of the utility model embodiment;
Fig. 3 is the system architecture schematic diagram according to the thick trichlorosilane of the process of another embodiment of the utility model.
Embodiment
Be described below in detail embodiment of the present utility model, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the utility model, and can not be interpreted as restriction of the present utility model.
In description of the present utility model, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end ", " interior ", " outward ", " clockwise ", " counterclockwise ", " axis ", " radial direction ", orientation or the position relationship of the instruction such as " circumference " are based on orientation shown in the drawings or position relationship, only the utility model and simplified characterization for convenience of description, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as restriction of the present utility model.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise at least one this feature.In description of the present utility model, the implication of " multiple " is at least two, such as two, three etc., unless otherwise expressly limited specifically.
In the utility model, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or integral; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements, unless otherwise clear and definite restriction.For the ordinary skill in the art, the concrete meaning of above-mentioned term in the utility model can be understood as the case may be.
In the utility model, unless otherwise clearly defined and limited, fisrt feature second feature " on " or D score can be that the first and second features directly contact, or the first and second features are by intermediary indirect contact.And, fisrt feature second feature " on ", " top " and " above " but fisrt feature directly over second feature or oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " can be fisrt feature immediately below second feature or tiltedly below, or only represent that fisrt feature level height is less than second feature.
In one of the present utility model, the utility model proposes a kind of system processing thick trichlorosilane, comprising:
Air-lift device, air-lift device is suitable for thick trichlorosilane to carry out stripping process, to obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride;
First purifying plant, first purifying plant is connected with air-lift device, and be suitable for the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride to carry out the first purification processes, to obtain liquid at the bottom of the first overhead gas and the first tower, wherein, first overhead gas contains dichlorosilane and trichlorosilicane, and at the bottom of the first tower, liquid contains silicon tetrachloride;
Second purifying plant, the second purifying plant is connected with the first purifying plant, and is suitable for the first overhead gas to carry out the second purification processes, to obtain liquid at the bottom of the second overhead gas and the second tower, wherein, the second overhead gas contains dichlorosilane, and at the bottom of the second tower, liquid contains trichlorosilicane;
Mixing device, mixing device is connected with the second purifying plant with the first purifying plant respectively, and is suitable for liquid at the bottom of the first tower and the second overhead gas to carry out combination treatment, to obtain the mixture containing dichlorosilane and silicon tetrachloride;
Anti-disproportionation device, anti-disproportionation device is connected with mixing device, and is suitable for, under the ion exchange resin of load exists, the mixture containing dichlorosilane and silicon tetrachloride being carried out anti-disproportionation process, to obtain anti-disproportionation products;
3rd purifying plant, the 3rd purifying plant is connected with anti-disproportionation device, and is suitable for anti-disproportionation products to carry out the 3rd purification processes, to obtain liquid at the bottom of the 3rd tower, wherein, at the bottom of the 3rd tower, liquid contains trichlorosilane; And
4th purifying plant, 4th purifying plant is connected with described 3rd purifying plant with the second purifying plant respectively, and be suitable for liquid at the bottom of liquid at the bottom of the second tower and the 3rd tower to carry out the 4th purification processes, to obtain liquid at the bottom of trichlorosilane and the 4th tower, and liquid at the bottom of the 4th tower is returned carry out the first purification processes.
The impurity containing boron phosphoric close with dichlorosilane boiling point in thick trichlorosilane removes by adopting air-lift device by the system according to the thick trichlorosilane of the process of the utility model embodiment, then pure dichlorosilane and silicon tetrachloride can be obtained by purifying plant, thus prepare high-quality trichlorosilane by anti-disproportionation device, in anti-disproportionation device, adopt the ion exchange resin of load as catalyzer simultaneously, not easily run off because this catalyzer has, not easy in inactivation, low price, easily and the advantage such as product separation, and carrier itself also can catalyzed reaction, thus significantly processing cost can be reduced while raising raw material availability, in addition, before carrying out anti-disproportionation reaction, the Homogeneous phase mixing in mixing device by dichlorosilane and silicon tetrachloride in advance, contacting between dichlorosilane with silicon tetrachloride can be increased, and then the transformation efficiency of dichlorosilane and silicon tetrachloride can be significantly improved, thus solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and obtain high-quality trichlorosilane.
System below with reference to the thick trichlorosilane of the process of Fig. 1 to the utility model embodiment is described in detail.According to embodiment of the present utility model, this thick trichlorosilane contains dichlorosilane, trichlorosilane, silicon tetrachloride and the impurity containing boron phosphoric.According to embodiment of the present utility model, this system comprises:
Gas device 100: according to embodiment of the present utility model, air-lift device 100 has thick trichlorosilane entrance 101, mixture outlet 102 and impurities outlet 103, and be suitable for thick trichlorosilane to carry out stripping process, thus the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride can be obtained.Thus, effectively can remove the impurity containing boron phosphoric close with dichlorosilane boiling point in thick trichlorosilane, thus the quality of trichlorosilane in subsequent processes can be significantly improved.
According to embodiment of the present utility model, thick trichlorosilane can obtain for cold hydrogen treatment.Thus, the recycle of material can be realized, thus reach energy-saving and cost-reducing, the object of protection of the environment, reduction production cost.
According to embodiment of the present utility model, the condition of stripping process is also not particularly limited, according to specific embodiment of the utility model, stripping process can be 0.5 ~ 0.8MPa at pressure, tower top temperature is carry out under 38 ~ 40 degrees Celsius and bottom temperature are 135 ~ 138 degrees Celsius.Contriver finds, can significantly improve the clearance of the impurity containing boron phosphoric in thick trichlorosilane, thus improve the quality of trichlorosilane in subsequent processes under this condition.
According to embodiment of the present utility model, air-lift device can be gas stripping column, wherein, stripping medium can be silicon tetrachloride, trichlorosilane, dichloro hydrogen silicon, hydrogen, hydrogenchloride or silica flour, gas stripping column is made up of upper column and bottom tower two portions, upper column internal diameter is 500 ~ 600mm, totally 10 blocks of column plates; Bottom tower internal diameter is 1400 ~ 1600mm, totally 20 blocks of column plates.
First purifying plant 200: according to embodiment of the present utility model, first purifying plant 200 has liquid outlet 203 at the bottom of the first material inlet 201, first overhead gas outlet 202 and the first tower, according to the utility model specific embodiment, first material inlet 201 is connected with mixture outlet 102, and be suitable for the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride obtained above to carry out the first purification processes, thus liquid at the bottom of the first overhead gas and the first tower can be obtained.According to specific embodiment of the utility model, the first overhead gas can contain dichlorosilane and trichlorosilicane, and liquid at the bottom of the first tower can contain silicon tetrachloride.Thus, effectively can realize being separated of silicon tetrachloride and dichlorosilane and trichlorosilane, thus can be separated and obtain silicon tetrachloride.
According to embodiment of the present utility model, the condition of the first purification processes is also not particularly limited, according to specific embodiment of the utility model, the first purification processes can be 0.4 ~ 0.6MPa at pressure, tower top temperature is carry out under 85 ~ 90 degrees Celsius and bottom temperature are 127 ~ 130 degrees Celsius.Contriver finds, can significantly improve the separation efficiency of silicon tetrachloride, obtain highly purified silicon tetrachloride, thus significantly improve the quality of subsequent process trichlorosilane under this condition.
According to embodiment of the present utility model, the first purifying plant can be purification tower, and wherein, this purification tower is tray column, and tower internal diameter is 2800 ~ 3000mm, stage number 100 ~ 120.
Second purifying plant 300: according to embodiment of the present utility model, second purifying plant 300 has liquid outlet 303 at the bottom of the second material inlet 301, second overhead gas outlet 302 and the second tower, according to specific embodiment of the utility model, second material inlet 301 and the first overhead gas export 202 and are connected, and be suitable for the first overhead gas obtained above to carry out the second purification processes, thus liquid at the bottom of the second overhead gas and the second tower can be obtained.According to specific embodiment of the utility model, the second overhead gas contains dichlorosilane, and at the bottom of the second tower, liquid contains trichlorosilane.Thus, effectively can realize being separated of dichlorosilane and trichlorosilane, thus can be separated and obtain dichlorosilane.
According to embodiment of the present utility model, the condition of the second purification processes is also not particularly limited, according to specific embodiment of the utility model, the second purification processes can be 0.3 ~ 0.5MPa at pressure, tower top temperature is carry out under 65 ~ 71 degrees Celsius and bottom temperature are 90 ~ 95 degrees Celsius.Contriver finds, can significantly improve the separation efficiency of dichlorosilane, obtain highly purified dichlorosilane under this condition, thus improves the quality of subsequent process trichlorosilane further.
According to embodiment of the present utility model, the second purifying plant can be purification tower, and wherein, this purification tower is tray column, stage number 80 ~ 100.
Mixing device 400: according to embodiment of the present utility model, mixing device 400 has opening for feed 401 and discharge port 402, according to specific embodiment of the utility model, opening for feed 401 exports 203 respectively and exports 302 with the second overhead gas and be connected with liquid at the bottom of the first tower, and be suitable for liquid and the second overhead gas at the bottom of the first tower obtained above to carry out combination treatment, thus the mixture containing dichlorosilane and silicon tetrachloride can be obtained.Contriver finds, before carrying out anti-disproportionation reaction, in advance by dichlorosilane and silicon tetrachloride Homogeneous phase mixing, contacting between dichlorosilane with silicon tetrachloride can be increased, and then the transformation efficiency of dichlorosilane and silicon tetrachloride can be significantly improved, thus solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and obtain high-quality trichlorosilane.
According to embodiment of the present utility model, in mixture, the ratio of dichlorosilane and silicon tetrachloride is also not particularly limited, and according to specific embodiment of the utility model, the mol ratio of dichlorosilane and silicon tetrachloride can be 1:3 ~ 5.Contriver finds, when ratio is too low, dichlorosilane low conversion rate, in 80%, does not reach expected effect; And although molar ratio is too high can improve 1 ~ 2% on the original basis, but add the load of equipment, higher requirement is had for the type selecting of Static Equipment and duct arrangement, entirety increases the input of front capital, thus by the comparative analysis to economic benefit, determine that molar ratio is optimum value in 1:3 ~ 5.
Anti-disproportionation device 500: according to embodiment of the present utility model, anti-disproportionation device 500 has mixture entrance 501, anti-disproportionation products outlet 502 and fills the filter cap (not shown) of loaded ion exchange resin, according to specific embodiment of the utility model, mixture entrance 501 is connected with discharge port 402, and be suitable under the ion exchange resin of load exists, mixture containing dichlorosilane obtained above is carried out anti-disproportionation process in anti-disproportionation device, thus anti-disproportionation products can be obtained.Contriver finds, adopt the ion exchange resin of load as catalyzer, not easily run off because this catalyzer has, not easy in inactivation, low price, easily and the advantage such as product separation, and carrier is alkalescence, carrier itself also can the anti-disproportionation reaction of catalysis, thus uses this catalyzer significantly can reduce processing cost while raising raw material availability in anti-disproportionation treating processes.
According to embodiment of the present utility model, by the mixture containing dichlorosilane and silicon tetrachloride from anti-disproportionation reactor bottom feed.Contriver finds, catalyzer is contained in the filter cap be positioned in the middle part of anti-disproportionation reactor, material and catalyst exposure can be made within the very first time from anti-disproportionation reactor bottom feed, and because density of catalyst is little, along with liquid level rises, catalyzer is also along with liquid level rises, arrive in the middle part of reactor, thus can effective reaction time be increased, the liquid of this external reflux contacts with ascending gas and carries out mass-and heat-transfer part gas-liquid and transform, intermediate and catalyst exposure can be improved, thus improve reaction conversion ratio further.
According to embodiment of the present utility model, the condition of anti-disproportionation reaction is also not particularly limited, according to specific embodiment of the utility model, anti-disproportionation process can be that 0.7 ~ 1.0MPa, tower top temperature and bottom temperature are under 65 ~ 70 degrees Celsius and carry out at pressure.Contriver finds, can significantly improve anti-disproportionation reaction efficiency under this condition, thus improves the quality of subsequent process trichlorosilane further.
3rd purifying plant 600: according to embodiment of the present utility model, 3rd purifying plant 600 has liquid outlet 603 at the bottom of 3 material entrance 601, the 3rd overhead gas outlet 602 and the 3rd tower, according to specific embodiment of the utility model, 3 material entrance 601 and anti-disproportionation products export 502 and are connected, and be suitable for anti-disproportionation products obtained above to carry out the 3rd purification processes, thus liquid at the bottom of the 3rd overhead gas and the 3rd tower can be obtained.According to specific embodiment of the utility model, the 3rd overhead gas contains unreacted dichlorosilane, a small amount of trichlorosilane and other light constituents, and at the bottom of the 3rd tower, liquid contains trichlorosilane.Thus, effectively can remove the unreacted dichlorosilane in anti-disproportionation products and other lower-boiling impurities, thus improve the quality of trichlorosilane further.
According to embodiment of the present utility model, the condition of the 3rd purification processes is also not particularly limited, according to specific embodiment of the utility model, the 3rd purification processes can be 0.3 ~ 0.6MPa at pressure, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 103 ~ 108 degrees Celsius.Contriver finds, can significantly improve the clearance of lower-boiling impurity under this condition, thus improves the quality of subsequent process trichlorosilane further.
According to embodiment of the present utility model, the 3rd purifying plant can be purification tower, and this purification tower is packing tower, and filler is regular wire packing, and total volume is 36.5m
3, wherein, stripping medium can be chlorosilane, effectively can remove dichlorosilane and other light constituent.
4th purifying plant 700: according to embodiment of the present utility model, 4th purifying plant 700 has 4 materials entrance 701, 4th overhead gas outlet 702 and the 4th outlet of liquid at the bottom of tower 703, according to specific embodiment of the utility model, 4 materials entrance 701 exports 303 respectively and exports 603 with liquid at the bottom of the 3rd tower and be connected with liquid at the bottom of the second tower, liquid outlet 703 at the bottom of 4th tower is connected with the first material inlet 201, and be suitable for liquid at the bottom of liquid at the bottom of the second tower obtained above and the 3rd tower to carry out the 4th purification processes, thus liquid at the bottom of trichlorosilane and the 4th tower can be obtained, and liquid at the bottom of the 4th tower is returned carry out the first purifying plant.Thus, can be separated and obtain high-quality trichlorosilane products, thus significantly improve the quality of polysilicon, the recycle of material can be realized simultaneously, thus significantly reduce raw materials cost.
According to embodiment of the present utility model, the condition of the 4th purification processes is also not particularly limited, according to specific embodiment of the utility model, the 4th purification processes can be 0.2 ~ 0.5MPa at pressure, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 75 ~ 80 degrees Celsius.Contriver finds, can significantly improve the separation efficiency of trichlorosilane and other impurity under this condition, thus improves the quality of subsequent process trichlorosilane further.
According to embodiment of the present utility model, the 4th purifying plant can be purification tower, and wherein, this purification tower is packing tower, and wire feeding is regular wire packing, and total volume is 300 ~ 400m
3.
Above the system of the thick trichlorosilane of the process of the utility model embodiment is described in detail, conveniently understand, below with reference to Fig. 2, the method for the thick trichlorosilane of system implementation process utilizing the thick trichlorosilane of the process of the utility model embodiment is described in detail.According to embodiment of the present utility model, the method comprises:
S100: stripping process
According to embodiment of the present utility model, thick trichlorosilane is carried out stripping process, thus the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride can be obtained.Thus, effectively can remove the impurity containing boron phosphoric close with dichlorosilane boiling point in thick trichlorosilane, thus the quality of trichlorosilane in subsequent processes can be significantly improved.
According to embodiment of the present utility model, thick trichlorosilane can obtain for cold hydrogen treatment.Thus, the recycle of material can be realized, thus reach energy-saving and cost-reducing, the object of protection of the environment, reduction production cost.
According to embodiment of the present utility model, the condition of stripping process is also not particularly limited, according to specific embodiment of the utility model, stripping process can be 0.5 ~ 0.8MPa at pressure, tower top temperature is carry out under 38 ~ 40 degrees Celsius and bottom temperature are 135 ~ 138 degrees Celsius.Contriver finds, can significantly improve the clearance of the impurity containing boron phosphoric in thick trichlorosilane, thus improve the quality of trichlorosilane in subsequent processes under this condition.
S200: the first purification processes
According to embodiment of the present utility model, the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride obtained above is carried out the first purification processes, thus liquid at the bottom of the first overhead gas and the first tower can be obtained.According to specific embodiment of the utility model, the first overhead gas can contain dichlorosilane and trichlorosilicane, and liquid at the bottom of the first tower can contain silicon tetrachloride.Thus, effectively can realize being separated of silicon tetrachloride and dichlorosilane and trichlorosilane, thus can be separated and obtain silicon tetrachloride.
According to embodiment of the present utility model, the condition of the first purification processes is also not particularly limited, according to specific embodiment of the utility model, the first purification processes can be 0.4 ~ 0.6MPa at pressure, tower top temperature is carry out under 85 ~ 90 degrees Celsius and bottom temperature are 127 ~ 130 degrees Celsius.Contriver finds, can significantly improve the separation efficiency of silicon tetrachloride, obtain highly purified silicon tetrachloride, thus significantly improve the quality of subsequent process trichlorosilane under this condition.
S300: the second purification processes
According to embodiment of the present utility model, the first overhead gas obtained above is carried out the second purification processes, thus liquid at the bottom of the second overhead gas and the second tower can be obtained.According to specific embodiment of the utility model, the second overhead gas contains dichlorosilane, and at the bottom of the second tower, liquid contains trichlorosilane.Thus, effectively can realize being separated of dichlorosilane and trichlorosilane, thus can be separated and obtain dichlorosilane.
According to embodiment of the present utility model, the condition of the second purification processes is also not particularly limited, according to specific embodiment of the utility model, the second purification processes can be 0.3 ~ 0.5MPa at pressure, tower top temperature is carry out under 65 ~ 71 degrees Celsius and bottom temperature are 90 ~ 95 degrees Celsius.Contriver finds, can significantly improve the separation efficiency of dichlorosilane, obtain highly purified dichlorosilane under this condition, thus improves the quality of subsequent process trichlorosilane further.
S400: combination treatment
According to embodiment of the present utility model, liquid and the second overhead gas at the bottom of the first tower obtained above are carried out combination treatment, thus the mixture containing dichlorosilane and silicon tetrachloride can be obtained.Contriver finds, before carrying out anti-disproportionation reaction, in advance by dichlorosilane and silicon tetrachloride Homogeneous phase mixing, contacting between dichlorosilane with silicon tetrachloride can be increased, and then the transformation efficiency of dichlorosilane and silicon tetrachloride can be significantly improved, thus solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and obtain high-quality trichlorosilane.
According to embodiment of the present utility model, in mixture, the ratio of dichlorosilane and silicon tetrachloride is also not particularly limited, and according to specific embodiment of the utility model, the mol ratio of dichlorosilane and silicon tetrachloride can be 1:3 ~ 5.Contriver finds, when ratio is too low, dichlorosilane low conversion rate, in 80%, does not reach expected effect; And although molar ratio is too high can improve 1 ~ 2% on the original basis, but add the load of equipment, higher requirement is had for the type selecting of Static Equipment and duct arrangement, entirety increases the input of front capital, thus by the comparative analysis to economic benefit, determine that molar ratio is optimum value in 1:3 ~ 5.
S500: anti-disproportionation process
According to embodiment of the present utility model, under the ion exchange resin of load exists, the mixture containing dichlorosilane obtained above is carried out anti-disproportionation process in anti-disproportionation reactor, thus anti-disproportionation products can be obtained.Contriver finds, adopt the ion exchange resin of load as catalyzer, not easily run off because this catalyzer has, not easy in inactivation, low price, easily and the advantage such as product separation, and carrier is alkalescence, carrier itself also can the anti-disproportionation reaction of catalysis, thus uses this catalyzer significantly can reduce processing cost while raising raw material availability in anti-disproportionation treating processes.
According to embodiment of the present utility model, by the mixture containing dichlorosilane and silicon tetrachloride from anti-disproportionation reactor bottom feed.Contriver finds, catalyzer is contained in the filter cap be positioned in the middle part of anti-disproportionation reactor, material and catalyst exposure can be made within the very first time from anti-disproportionation reactor bottom feed, and because density of catalyst is little, along with liquid level rises, catalyzer is also along with liquid level rises, arrive in the middle part of reactor, thus can effective reaction time be increased, the liquid of this external reflux contacts with ascending gas and carries out mass-and heat-transfer part gas-liquid and transform, intermediate and catalyst exposure can be improved, thus improve reaction conversion ratio further.
According to embodiment of the present utility model, the condition of anti-disproportionation reaction is also not particularly limited, and according to specific embodiment of the utility model, anti-disproportionation process can be carry out under 0.7 ~ 1.0MPa, tower top temperature and bottom temperature are 65 ~ 70 degrees Celsius at pressure.Contriver finds, can significantly improve anti-disproportionation reaction efficiency under this condition, thus improves the quality of subsequent process trichlorosilane further.
S600: the three purification processes
According to embodiment of the present utility model, anti-disproportionation products obtained above is carried out the 3rd purification processes, thus liquid at the bottom of the 3rd overhead gas and the 3rd tower can be obtained.According to specific embodiment of the utility model, the 3rd overhead gas contains unreacted dichlorosilane, a small amount of trichlorosilane and other light constituents, and at the bottom of the 3rd tower, liquid contains trichlorosilane.Thus, effectively can remove the unreacted dichlorosilane in anti-disproportionation products and other lower-boiling impurities, thus improve the quality of trichlorosilane further.
According to embodiment of the present utility model, the condition of the 3rd purification processes is also not particularly limited, according to specific embodiment of the utility model, the 3rd purification processes can be 0.3 ~ 0.6MPa at pressure, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 103 ~ 108 degrees Celsius.Contriver finds, can significantly improve the clearance of lower-boiling impurity under this condition, thus improves the quality of subsequent process trichlorosilane further.
S700: the four purification processes
According to embodiment of the present utility model, at the bottom of the 3rd tower that liquid and S600 at the bottom of the second tower obtained by S300 obtain, liquid carries out the 4th purification processes, thus can obtain liquid at the bottom of trichlorosilane and the 4th tower, and is returned by liquid at the bottom of the 4th tower and carry out the first purification processes.Thus, can be separated and obtain high-quality trichlorosilane products, thus significantly improve the quality of polysilicon, the recycle of material can be realized simultaneously, thus significantly reduce raw materials cost.
According to embodiment of the present utility model, the condition of the 4th purification processes is also not particularly limited, according to specific embodiment of the utility model, the 4th purification processes can be 0.2 ~ 0.5MPa at pressure, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 75 ~ 80 degrees Celsius.Contriver finds, can significantly improve the separation efficiency of trichlorosilane and other impurity under this condition, thus improves the quality of subsequent process trichlorosilane further.
The method of the thick trichlorosilane of system implementation process of the thick trichlorosilane of the process of the utility model embodiment is utilized to be removed by the impurity containing boron phosphoric close with dichlorosilane boiling point in thick trichlorosilane by adopting air-lift device, then pure dichlorosilane and silicon tetrachloride can be obtained by purifying plant, thus prepare high-quality trichlorosilane by anti-disproportionation device, in anti-disproportionation device, adopt the ion exchange resin of load as catalyzer simultaneously, not easily run off because this catalyzer has, not easy in inactivation, low price, easily and the advantage such as product separation, and carrier itself also can catalyzed reaction, thus significantly processing cost can be reduced while raising raw material availability, in addition, before carrying out anti-disproportionation reaction, the Homogeneous phase mixing in mixing device by dichlorosilane and silicon tetrachloride in advance, contacting between dichlorosilane with silicon tetrachloride can be increased, and then the transformation efficiency of dichlorosilane and silicon tetrachloride can be significantly improved, thus solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and obtain high-quality trichlorosilane.
Below with reference to specific embodiment, be described the utility model, it should be noted that, these embodiments are only descriptive, and limit the utility model never in any form.
Embodiment
Thick trichlorosilane composition: the silicon tetrachloride of the dichlorosilane of 36.69wt%, the trichlorosilane of 1.01wt%, 62.3wt% and the impurity of trace containing boron phosphoric;
Treatment process: with reference to figure 3, it is 0.6MPa that the thick trichlorosilane A obtained by cold hydrogenation units to pass in air-lift device 100 at pressure, bottom temperature is 137 degrees Celsius, tower top temperature is carry out stripping process under 38.5 degrees Celsius, obtain containing dichlorosilane, the mixture of trichlorosilane and silicon tetrachloride, then will containing dichlorosilane, it is 0.48MPa that the mixture of trichlorosilane and silicon tetrachloride to pass in the first purifying plant 200 at pressure, tower top temperature is 89 degrees Celsius and bottom temperature is carry out the first purification processes under 129 degrees Celsius, obtain the first overhead gas containing dichlorosilane and trichlorosilane and containing liquid at the bottom of the first tower of silicon tetrachloride, then being passed into by the first overhead gas containing dichlorosilane and trichlorosilane in the second gas device 300 at pressure is 0.41MPa, tower top temperature is 70 degrees Celsius and bottom temperature is carry out the second purification processes under 91 degrees Celsius, obtain the second overhead gas containing dichlorosilane and containing liquid at the bottom of the second tower of trichlorosilane, in mixing device 400, combination treatment is carried out (wherein by containing liquid at the bottom of the first tower of silicon tetrachloride and the second overhead gas containing dichlorosilane, dichlorosilane inlet amount is 200kg/h, the inlet amount of silicon tetrachloride is 2800kg/h), obtain the mixture containing dichlorosilane and silicon tetrachloride, then delivered to bottom anti-disproportionation device 500 by mixture anti-disproportionation device 500 is 0.85MPa at pressure under the ion exchange resin of load exists, tower top temperature is 70 degrees Celsius and bottom temperature is carry out anti-disproportionation process under 60 degrees Celsius, obtain anti-disproportionation products, then being delivered to by anti-disproportionation products in the 3rd purifying plant 600 at pressure is 0.45MPa, tower top temperature is 75 degrees Celsius and bottom temperature is carry out the 3rd purification processes under 106 degrees Celsius, obtain the 3rd overhead gas containing lower-boiling impurity and containing liquid at the bottom of the 3rd tower of trichlorosilane, and the 3rd overhead gas containing lower-boiling impurity is delivered to flare system process, be 0.35MPa by what obtain containing at the bottom of the 3rd tower of trichlorosilane, liquid to be delivered in the 4th purifying plant 700 at pressure, tower top temperature is 72 degrees Celsius and bottom temperature is carry out the 4th purification processes under 77 degrees Celsius, obtain liquid and high-quality trichlorosilane products B at the bottom of the 4th tower containing silicon tetrachloride, and carry out the first purification processes by being back in the first purifying plant 100 containing liquid at the bottom of the 4th tower of silicon tetrachloride.
The polycrystalline silicon production line of 5000t/a, dichlorosilane inlet amount 0.2t/h, silicon tetrachloride feeding amount 2800t/h, run calculating in 8000 hours, 1 year recyclable 2168 tons of trichlorosilane according to annual, save white lime and consume 9570 tons, save and produce water 44695m
3; According to existing market price, trichlorosilane 5400 yuan/ton, white lime 600 yuan/ton, produces water 4.5 yuan/m
3calculate:
Reclaim trichlorosilane=2186 ton × 5400 yuan/ton=11707200 yuan;
Save white lime consumption costs=9570 ton × 600 yuan/ton=5742000 yuan;
Save production water consumption expense=44695m
3× 4.5 yuan/m
3=201127 yuan;
Then save economic benefit=saving trichlorosilane expense+saving white lime consumption costs+saving production water consumption expense=1248.03 ten thousand yuan.
In the description of this specification sheets, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present utility model or example.In this manual, to the schematic representation of above-mentioned term not must for be identical embodiment or example.And the specific features of description, structure, material or feature can combine in one or more embodiment in office or example in an appropriate manner.In addition, when not conflicting, the feature of the different embodiment described in this specification sheets or example and different embodiment or example can carry out combining and combining by those skilled in the art.
Although illustrate and described embodiment of the present utility model above, be understandable that, above-described embodiment is exemplary, can not be interpreted as restriction of the present utility model, those of ordinary skill in the art can change above-described embodiment, revises, replace and modification in scope of the present utility model.
Claims (7)
1. process a system for thick trichlorosilane, it is characterized in that, comprising:
Air-lift device, described air-lift device has thick trichlorosilane entrance, mixture outlet and impurities outlet;
First purifying plant, described first purifying plant has liquid outlet at the bottom of the first material inlet, the first overhead gas outlet and the first tower, and wherein, described first material inlet is connected with described mixture outlet;
Second purifying plant, described second purifying plant has liquid outlet at the bottom of the second material inlet, the second overhead gas outlet and the second tower, and wherein, described second material inlet exports with described first overhead gas and is connected;
Mixing device, described mixing device has opening for feed and discharge port, and wherein, described opening for feed exports with liquid at the bottom of described first tower respectively to export with the second overhead gas and is connected;
Anti-disproportionation device, described anti-disproportionation device has mixture entrance, the outlet of anti-disproportionation products and fills the filter cap of loaded ion exchange resin, and wherein, described mixture entrance is connected with described discharge port;
3rd purifying plant, described 3rd purifying plant has liquid outlet at the bottom of 3 material entrance, the 3rd overhead gas outlet and the 3rd tower, and wherein, described 3 material entrance exports with described anti-disproportionation products and is connected; And
4th purifying plant, described 4th purifying plant has liquid outlet at the bottom of 4 materials entrance, the 4th overhead gas outlet and the 4th tower, wherein, described 4 materials entrance exports with liquid at the bottom of described second tower respectively to export with liquid at the bottom of the 3rd tower and is connected, and liquid outlet at the bottom of described 4th tower is connected with described first material inlet.
2. the system of the thick trichlorosilane of process according to claim 1, it is characterized in that, described air-lift device is gas stripping column, described gas stripping column is made up of upper column and bottom tower two portions, wherein, the internal diameter of described upper column is 500 ~ 600mm, and stage number is 10 pieces, the internal diameter of described bottom tower is 1400 ~ 1600mm, and stage number is 20 pieces.
3. the system of the thick trichlorosilane of process according to claim 1, is characterized in that, described first purifying plant is purification tower, and described purification tower is tray column, and the tower internal diameter of described tray column is 2800 ~ 3000mm, and stage number is 100 ~ 120 pieces.
4. the system of the thick trichlorosilane of process according to claim 1, is characterized in that, described second purifying plant is purification tower, and described purification tower is tray column, and the stage number of described tray column is 80 ~ 100 pieces.
5. the system of the thick trichlorosilane of process according to claim 1, is characterized in that, described mixture entrance is positioned at the bottom of described anti-disproportionation device.
6. the system of the thick trichlorosilane of process according to claim 1, is characterized in that, described 3rd purifying plant is purification tower, and described purification tower is packing tower, and described packing tower is regular wire packing, and total volume is 36.5m
3.
7. the system of the thick trichlorosilane of process according to claim 1, is characterized in that, described 4th purifying plant is purification tower, and described purification tower is packing tower, and described packing tower is regular wire packing, and total volume is 300 ~ 400m
3.
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