CN104261412A - Method and system for treating crude trichlorosilane - Google Patents
Method and system for treating crude trichlorosilane Download PDFInfo
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- CN104261412A CN104261412A CN201410464371.5A CN201410464371A CN104261412A CN 104261412 A CN104261412 A CN 104261412A CN 201410464371 A CN201410464371 A CN 201410464371A CN 104261412 A CN104261412 A CN 104261412A
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Abstract
The invention discloses a method and a system for treating crude trichlorosilane. The method comprises the following steps: (1) carrying out air stripping treatment on crude trichlorosilane to obtain a mixture; (2) purifying the mixture for the first time to obtain a first top gas and a first bottom liquid; (3) purifying the first top gas for the second time to obtain a second top gas and a second bottom liquid; (4) mixing the first bottom liquid with the second bottom liquid to obtain a mixed material; (5) disproportionating the mixed material in the presence of supported ion exchange resin to obtain a disproportionated product; (6) purifying the disproportionated product for the third time to obtain a third bottom liquid; and (7) purifying the second bottom liquid and the third bottom liquid for the fourth time to obtain trichlorosilane and a fourth bottom liquid and returning the fourth bottom liquid for purification for the first time. By adopting the method, the problem of the enrichment of dichlorosilane and silicon tetrachloride in crude trichlorosilane can be effectively solved and the quality of trichlorosilane can be significantly improved.
Description
Technical field
The invention belongs to technical field of polysilicon production, specifically, the present invention relates to a kind of method and 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.
Summary of the invention
The present invention is intended to solve one of technical problem in correlation technique at least to a certain extent.For this reason, one object of the present invention is to propose a kind of method and system processing thick trichlorosilane, and the method effectively can solve the enrichment problem of dichlorosilane and silicon tetrachloride in thick trichlorosilane, and can significantly improve trichlorosilane quality.
In one aspect of the invention, the present invention proposes a kind of method processing thick trichlorosilane, described thick trichlorosilane contains dichlorosilane, trichlorosilane, silicon tetrachloride and the impurity containing boron phosphoric, comprising:
(1) described thick trichlorosilane is carried out stripping process, to obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride;
(2) the described mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride is carried out the first purification processes, to obtain liquid at the bottom of the first overhead gas and the first tower, wherein, described first overhead gas contains dichlorosilane and trichlorosilicane, and at the bottom of described first tower, liquid contains silicon tetrachloride;
(3) described first overhead gas is carried out the second purification processes, to obtain liquid at the bottom of the second overhead gas and the second tower, wherein, described second overhead gas contains dichlorosilane, and at the bottom of described second tower, liquid contains trichlorosilicane;
(4) liquid at the bottom of described first tower and described second overhead gas are carried out combination treatment, to obtain the mixture containing dichlorosilane and silicon tetrachloride;
(5) under the ion exchange resin of load exists, the described mixture containing dichlorosilane and silicon tetrachloride is carried out anti-disproportionation process, to obtain anti-disproportionation products in anti-disproportionation reactor;
(6) described anti-disproportionation products is carried out the 3rd purification processes, to obtain liquid at the bottom of the 3rd tower, wherein, at the bottom of described 3rd tower, liquid contains trichlorosilane; And
(7) liquid at the bottom of liquid at the bottom of described second tower and described 3rd tower is carried out the 4th purification processes, to obtain liquid at the bottom of trichlorosilane and the 4th tower, and liquid at the bottom of described 4th tower is returned carry out described first purification processes.
The impurity containing boron phosphoric close with dichlorosilane boiling point in thick trichlorosilane removes by adopting stripping process by the method according to the thick trichlorosilane of the process of the embodiment of the present invention, then pure dichlorosilane and silicon tetrachloride can be obtained by purification processes, thus prepare high-quality trichlorosilane by anti-disproportionation process, in anti-disproportionation treating processes, 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, 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.
In addition, the method for the thick trichlorosilane of process according to the above embodiment of the present invention can also have following additional technical characteristic:
In some embodiments of the invention, described stripping process pressure be 0.5 ~ 0.8MPa, tower top temperature is carry out under 38 ~ 40 degrees Celsius and bottom temperature are 135 ~ 138 degrees Celsius.Thus, can effectively remove in thick trichlorosilane containing boron phosphoric impurity.
In some embodiments of the invention, described first purification processes pressure be 0.4 ~ 0.6MPa, tower top temperature is carry out under 85 ~ 90 degrees Celsius and bottom temperature are 127 ~ 130 degrees Celsius.Thus, effectively can be separated and obtain silicon tetrachloride.
In some embodiments of the invention, described second purification processes pressure be 0.3 ~ 0.5MPa, tower top temperature is carry out under 65 ~ 71 degrees Celsius and bottom temperature are 90 ~ 95 degrees Celsius.Thus, being separated of dichlorosilane and trichlorosilane can effectively be realized.
In some embodiments of the invention, contain in the mixture of dichlorosilane and silicon tetrachloride described, the mol ratio of described dichlorosilane and described silicon tetrachloride is 1:3 ~ 5.Thus, the transformation efficiency of dichlorosilane can be significantly improved.
In some embodiments of the invention, by the described mixture containing dichlorosilane and silicon tetrachloride from described anti-disproportionation reactor bottom feed.Thus, feed stock conversion can be significantly improved.
In some embodiments of the invention, described anti-disproportionation process is carry out under 0.7 ~ 1.0MPa, tower top temperature and bottom temperature are 65 ~ 70 degrees Celsius at pressure.Thus, effectively trichlorosilane can be prepared.
In some embodiments of the invention, described 3rd purification processes pressure be 0.3 ~ 0.6MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 103 ~ 108 degrees Celsius.Thus, the lower-boiling impurity in anti-disproportionation products can effectively be removed.
In some embodiments of the invention, described 4th purification processes pressure be 0.2 ~ 0.5MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 75 ~ 80 degrees Celsius.Thus, can be separated and obtain high-quality trichlorosilane.
In some embodiments of the invention, described thick silicon tetrachloride is that cold hydrogen treatment obtains.Thus, the recycle of material can be realized.
In another aspect of the present invention, the present invention proposes a kind of system processing thick trichlorosilane, comprising:
Air-lift device, described air-lift device is suitable for described thick trichlorosilane being carried out stripping process, to obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride;
First purifying plant, described first purifying plant is connected with described air-lift device, and be suitable for the described 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, described first overhead gas contains dichlorosilane and trichlorosilicane, and at the bottom of described first tower, liquid contains silicon tetrachloride;
Second purifying plant, described second purifying plant is connected with described first purifying plant, and be suitable for described 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, described second overhead gas contains dichlorosilane, and at the bottom of described second tower, liquid contains trichlorosilicane;
Mixing device, described mixing device is connected with described second purifying plant with described first purifying plant respectively, and be suitable for liquid at the bottom of described first tower and described second overhead gas being carried out combination treatment, to obtain the mixture containing dichlorosilane and silicon tetrachloride;
Anti-disproportionation device, described anti-disproportionation device is connected with described mixing device, and is suitable for, under the ion exchange resin of load exists, the described mixture containing dichlorosilane and silicon tetrachloride being carried out anti-disproportionation process, to obtain anti-disproportionation products;
3rd purifying plant, described 3rd purifying plant is connected with described anti-disproportionation device, and is suitable for described 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 described 3rd tower, liquid contains trichlorosilane; And
4th purifying plant, described 4th purifying plant is connected with described 3rd purifying plant with described second purifying plant respectively, and be suitable for liquid at the bottom of liquid at the bottom of described second tower and described 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 described 4th tower is returned carry out described 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 embodiment of the present invention, 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, the system of the thick trichlorosilane of process according to the above embodiment of the present invention can also have following additional technical characteristic:
In some embodiments of the invention, described stripping process pressure be 0.5 ~ 0.8MPa, tower top temperature is carry out under 38 ~ 40 degrees Celsius and bottom temperature are 135 ~ 138 degrees Celsius.Thus, can effectively remove in thick trichlorosilane containing boron phosphoric impurity.
In some embodiments of the invention, described first purification processes pressure be 0.4 ~ 0.6MPa, tower top temperature is carry out under 85 ~ 90 degrees Celsius and bottom temperature are 127 ~ 130 degrees Celsius.Thus, effectively can be separated and obtain silicon tetrachloride.
In some embodiments of the invention, described second purification processes pressure be 0.3 ~ 0.5MPa, tower top temperature is carry out under 65 ~ 71 degrees Celsius and bottom temperature are 90 ~ 95 degrees Celsius.Thus, being separated of dichlorosilane and trichlorosilane can effectively be realized.
In some embodiments of the invention, contain in the mixture of dichlorosilane and silicon tetrachloride described, the mol ratio of described dichlorosilane and described silicon tetrachloride is 1:3 ~ 5.Thus, the transformation efficiency of dichlorosilane can be significantly improved.
In some embodiments of the invention, by the described mixture containing dichlorosilane and silicon tetrachloride from described anti-disproportionation device bottom feed.Thus, feed stock conversion can be significantly improved.
In some embodiments of the invention, described anti-disproportionation process is carry out under 0.7 ~ 1.0MPa, tower top temperature and bottom temperature are separately 65 ~ 70 degrees Celsius at pressure.Thus, effectively trichlorosilane can be prepared.
In some embodiments of the invention, described 3rd purification processes pressure be 0.3 ~ 0.6MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 103 ~ 108 degrees Celsius.Thus, the lower-boiling impurity in anti-disproportionation products can effectively be removed.
In some embodiments of the invention, described 4th purification processes pressure be 0.2 ~ 0.5MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 75 ~ 80 degrees Celsius.Thus, can be separated and obtain high-quality trichlorosilane.
In some embodiments of the invention, described thick silicon tetrachloride is that cold hydrogen treatment obtains.Thus, the recycle of material can be realized.
Accompanying drawing explanation
Fig. 1 is the method flow schematic diagram processing thick trichlorosilane according to an embodiment of the invention;
Fig. 2 is the system architecture schematic diagram processing thick trichlorosilane according to an embodiment of the invention;
Fig. 3 is the system architecture schematic diagram according to the thick trichlorosilane of the process of another embodiment of the present invention.
Embodiment
Be described below in detail embodiments of the invention, 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 present invention, and can not limitation of the present invention be interpreted as.
In describing the invention, 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 present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore limitation of the present invention can not be interpreted as.
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 describing the invention, the implication of " multiple " is at least two, such as two, three etc., unless otherwise expressly limited specifically.
In the present invention, 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, above-mentioned term concrete meaning in the present invention can be understood as the case may be.
In the present invention, 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 aspect of the invention, the present invention proposes a kind of method processing thick trichlorosilane, this thick trichlorosilane contains dichlorosilane, trichlorosilane, silicon tetrachloride and the impurity containing boron phosphoric, and the method comprises:
(1) thick trichlorosilane is carried out stripping process, to obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride;
(2) mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride is carried out the first purification processes, to obtain liquid at the bottom of the first overhead gas and the first tower, wherein, the first overhead gas contains dichlorosilane and trichlorosilicane, and at the bottom of the first tower, liquid contains silicon tetrachloride;
(3) the first overhead gas is carried 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;
(4) liquid at the bottom of the first tower and the second overhead gas are carried out combination treatment, to obtain the mixture containing dichlorosilane and silicon tetrachloride;
(5) under the ion exchange resin of load exists, the mixture containing dichlorosilane and silicon tetrachloride is carried out anti-disproportionation process in anti-disproportionation reactor, to obtain anti-disproportionation products;
(6) anti-disproportionation products is carried 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
(7) liquid at the bottom of liquid at the bottom of the second tower and described 3rd tower is carried 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 stripping process by the method according to the thick trichlorosilane of the process of the embodiment of the present invention, then pure dichlorosilane and silicon tetrachloride can be obtained by purification processes, thus prepare high-quality trichlorosilane by anti-disproportionation process, in anti-disproportionation treating processes, 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, 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.
Method below with reference to the thick trichlorosilane of the process of Fig. 1 to the embodiment of the present invention is described in detail.According to embodiments of the invention, the method comprises:
S100: stripping process
According to embodiments of the invention, 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 embodiments of the invention, 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 embodiments of the invention, the condition of stripping process is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 a particular embodiment of the invention, 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 embodiments of the invention, the condition of the first purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 a particular embodiment of the invention, 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 embodiments of the invention, the condition of the second purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 embodiments of the invention, in mixture, the ratio of dichlorosilane and silicon tetrachloride is also not particularly limited, and according to a particular embodiment of the invention, 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 embodiments of the invention, 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 embodiments of the invention, 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 embodiments of the invention, the condition of anti-disproportionation reaction is also not particularly limited, and according to a particular embodiment of the invention, 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 embodiments of the invention, 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 a particular embodiment of the invention, 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 embodiments of the invention, the condition of the 3rd purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 embodiments of the invention, the condition of the 4th purification processes is also not particularly limited, according to a particular embodiment of the invention, 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.
In another aspect of the present invention, the present invention 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 embodiment of the present invention, 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. 2 to the embodiment of the present invention is described in detail.According to embodiments of the invention, this system comprises:
Air-lift device 100: according to embodiments of the invention, air-lift device 100 is suitable for thick trichlorosilane to carry out stripping process, thus can obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride.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 embodiments of the invention, 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 embodiments of the invention, the condition of stripping process is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 and lower two portions, and 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 embodiments of the invention, first purifying plant 200 is connected with air-lift device 100, 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 a particular embodiment of the invention, 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 embodiments of the invention, the condition of the first purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 embodiments of the invention, the second purifying plant 300 is connected with the first purifying plant 200, and is suitable for the first overhead gas obtained above to carry out the second purification processes, thus can obtain liquid at the bottom of the second overhead gas and the second tower.According to a particular embodiment of the invention, 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 embodiments of the invention, the condition of the second purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 embodiments of the invention, mixing device 400 is connected with the second purifying plant 300 with the first purifying plant 200 respectively, 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 embodiments of the invention, in mixture, the ratio of dichlorosilane and silicon tetrachloride is also not particularly limited, and according to a particular embodiment of the invention, 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 embodiments of the invention, anti-disproportionation device 500 is connected with mixing device 400, 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 embodiments of the invention, 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 embodiments of the invention, the condition of anti-disproportionation reaction is also not particularly limited, and according to a particular embodiment of the invention, 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 embodiments of the invention, the 3rd purifying plant 600 is connected with anti-disproportionation device 500, and is suitable for anti-disproportionation products obtained above to carry out the 3rd purification processes, thus can obtain liquid at the bottom of the 3rd overhead gas and the 3rd tower.According to a particular embodiment of the invention, 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 embodiments of the invention, the condition of the 3rd purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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 embodiments of the invention, 4th purifying plant 700 is connected with the 3rd purifying plant 600 with the second purifying plant 300 respectively, 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 200.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 embodiments of the invention, the condition of the 4th purification processes is also not particularly limited, according to a particular embodiment of the invention, 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 embodiments of the invention, 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.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiments are only descriptive, and do not limit the present invention in any way.
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 invention 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 describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, and those of ordinary skill in the art can change above-described embodiment within the scope of the invention, revises, replace and modification.
Claims (20)
1. process a method for thick trichlorosilane, described thick trichlorosilane contains dichlorosilane, trichlorosilane, silicon tetrachloride and the impurity containing boron phosphoric, it is characterized in that, comprising:
(1) described thick trichlorosilane is carried out stripping process, to obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride;
(2) the described mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride is carried out the first purification processes, to obtain liquid at the bottom of the first overhead gas and the first tower, wherein, described first overhead gas contains dichlorosilane and trichlorosilicane, and at the bottom of described first tower, liquid contains silicon tetrachloride;
(3) described first overhead gas is carried out the second purification processes, to obtain liquid at the bottom of the second overhead gas and the second tower, wherein, described second overhead gas contains dichlorosilane, and at the bottom of described second tower, liquid contains trichlorosilicane;
(4) liquid at the bottom of described first tower and described second overhead gas are carried out combination treatment, to obtain the mixture containing dichlorosilane and silicon tetrachloride;
(5) under the ion exchange resin of load exists, the described mixture containing dichlorosilane and silicon tetrachloride is carried out anti-disproportionation process, to obtain anti-disproportionation products in anti-disproportionation reactor;
(6) described anti-disproportionation products is carried out the 3rd purification processes, to obtain liquid at the bottom of the 3rd tower, wherein, at the bottom of described 3rd tower, liquid contains trichlorosilane; And
(7) liquid at the bottom of liquid at the bottom of described second tower and described 3rd tower is carried out the 4th purification processes, to obtain liquid at the bottom of trichlorosilane and the 4th tower, and liquid at the bottom of described 4th tower is returned carry out described first purification processes.
2. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described stripping process pressure be 0.5 ~ 0.8MPa, tower top temperature is carry out under 38 ~ 40 degrees Celsius and bottom temperature are 135 ~ 138 degrees Celsius.
3. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described first purification processes pressure be 0.4 ~ 0.6MPa, tower top temperature is carry out under 85 ~ 90 degrees Celsius and bottom temperature are 127 ~ 130 degrees Celsius.
4. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described second purification processes pressure be 0.3 ~ 0.5MPa, tower top temperature is carry out under 65 ~ 71 degrees Celsius and bottom temperature are 90 ~ 95 degrees Celsius.
5. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, contain in the mixture of dichlorosilane and silicon tetrachloride described, the mol ratio of described dichlorosilane and described silicon tetrachloride is 1:3 ~ 5.
6. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, by the described mixture containing dichlorosilane and silicon tetrachloride from described anti-disproportionation reactor bottom feed.
7. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described anti-disproportionation process is carry out under 0.7 ~ 1.0MPa, tower top temperature and bottom temperature are 65 ~ 70 degrees Celsius at pressure.
8. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described 3rd purification processes pressure be 0.3 ~ 0.6MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 103 ~ 108 degrees Celsius.
9. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described 4th purification processes pressure be 0.2 ~ 0.5MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 75 ~ 80 degrees Celsius.
10. the method for the thick trichlorosilane of process according to claim 1, is characterized in that, described thick silicon tetrachloride is that cold hydrogen treatment obtains.
The system of 11. 1 kinds of thick trichlorosilanes of process, is characterized in that, comprising:
Air-lift device, described air-lift device is suitable for described thick trichlorosilane being carried out stripping process, to obtain the mixture containing dichlorosilane, trichlorosilane and silicon tetrachloride;
First purifying plant, described first purifying plant is connected with described air-lift device, and be suitable for the described 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, described first overhead gas contains dichlorosilane and trichlorosilicane, and at the bottom of described first tower, liquid contains silicon tetrachloride;
Second purifying plant, described second purifying plant is connected with described first purifying plant, and be suitable for described 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, described second overhead gas contains dichlorosilane, and at the bottom of described second tower, liquid contains trichlorosilicane;
Mixing device, described mixing device is connected with described second purifying plant with described first purifying plant respectively, and be suitable for liquid at the bottom of described first tower and described second overhead gas being carried out combination treatment, to obtain the mixture containing dichlorosilane and silicon tetrachloride;
Anti-disproportionation device, described anti-disproportionation device is connected with described mixing device, and is suitable for, under the ion exchange resin of load exists, the described mixture containing dichlorosilane and silicon tetrachloride being carried out anti-disproportionation process, to obtain anti-disproportionation products;
3rd purifying plant, described 3rd purifying plant is connected with described anti-disproportionation device, and is suitable for described 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 described 3rd tower, liquid contains trichlorosilane; And
4th purifying plant, described 4th purifying plant is connected with described 3rd purifying plant with described second purifying plant respectively, and be suitable for liquid at the bottom of liquid at the bottom of described second tower and described 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 described 4th tower is returned carry out described first purifying plant.
The system of the thick trichlorosilane of 12. process according to claim 11, is characterized in that, described stripping process pressure be 0.5 ~ 0.8MPa, tower top temperature is carry out under 38 ~ 40 degrees Celsius and bottom temperature are 135 ~ 138 degrees Celsius.
The system of the thick trichlorosilane of 13. process according to claim 11, is characterized in that, described first purification processes pressure be 0.4 ~ 0.6MPa, tower top temperature is carry out under 85 ~ 90 degrees Celsius and bottom temperature are 127 ~ 130 degrees Celsius.
The system of the thick trichlorosilane of 14. process according to claim 11, is characterized in that, described second purification processes pressure be 0.3 ~ 0.5MPa, tower top temperature is carry out under 65 ~ 71 degrees Celsius and bottom temperature are 90 ~ 95 degrees Celsius.
The system of the thick trichlorosilane of 15. process according to claim 11, is characterized in that, contain in the mixture of dichlorosilane and silicon tetrachloride described, the mol ratio of described dichlorosilane and described silicon tetrachloride is 1:3 ~ 5.
The system of the thick trichlorosilane of 16. process according to claim 11, is characterized in that, by the described mixture containing dichlorosilane and silicon tetrachloride from described anti-disproportionation device bottom feed.
The system of the thick trichlorosilane of 17. process according to claim 11, is characterized in that, described anti-disproportionation process is carry out under 0.7 ~ 1.0MPa, tower top temperature and bottom temperature are 65 ~ 70 degrees Celsius at pressure.
The system of the thick trichlorosilane of 18. process according to claim 11, is characterized in that, described 3rd purification processes pressure be 0.3 ~ 0.6MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 103 ~ 108 degrees Celsius.
The system of the thick trichlorosilane of 19. process according to claim 11, is characterized in that, described 4th purification processes pressure be 0.2 ~ 0.5MPa, tower top temperature is carry out under 70 ~ 75 degrees Celsius and bottom temperature are 75 ~ 80 degrees Celsius.
The system of the thick trichlorosilane of 20. process according to claim 11, is characterized in that, described thick silicon tetrachloride is that cold hydrogen treatment obtains.
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