CN104058408B - The method of purification Silicon chloride. - Google Patents
The method of purification Silicon chloride. Download PDFInfo
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- CN104058408B CN104058408B CN201410299615.9A CN201410299615A CN104058408B CN 104058408 B CN104058408 B CN 104058408B CN 201410299615 A CN201410299615 A CN 201410299615A CN 104058408 B CN104058408 B CN 104058408B
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Abstract
A kind of method that the invention discloses purification Silicon chloride., including: (1) utilizes thick Silicon chloride. to absorb chlorine, in order to be absorbed saturated thick Silicon chloride., and wherein, thick Silicon chloride. contains trichlorosilane；(2) optical chlorinating reaction is carried out by absorbing saturated thick Silicon chloride., in order to obtaining optical chlorinating reaction product, wherein, optical chlorinating reaction makes trichlorosilane be converted into Silicon chloride.；(3) adopt nitrogen that optical chlorinating reaction product is carried out stripping process, in order to separate unreacted chlorine, and obtain Silicon chloride. after air stripping；(4) Silicon chloride. after air stripping is carried out the first rectification process, in order to obtain tower top tail gas and the Silicon chloride. through the first rectification process；And the Silicon chloride. through the first rectification process is carried out the second rectification process by (5), in order to obtain tower bottoms and purified Silicon chloride..The method can significantly improve the purity of Silicon chloride., thus obtaining the ultrapure silicon tetrachloride of optical fiber rank.
Description
Technical field
The invention belongs to field of polysilicon production, specifically, a kind of method that the present invention relates to purification Silicon chloride..
Background technology
In recent years, development along with China's informatization, the demand of fiber products is constantly increased by market, aggregate demand breaks through 100,000,000 core kilometers, market occurs in that the phenomenon that optical fiber is under-supply, and the important technology factor restricting the increase of optical fiber yield is exactly that China is too high to the degree of dependence of one of import preform and important source material thereof optical fiber ultrapure silicon tetrachloride (ultralow-hydrogen low content Silicon chloride .).So, for the development supporting national information to build, the technology of optical fiber ultrapure silicon tetrachloride is prepared in research and development becomes the task of top priority.
The method preparing optical fiber ultrapure silicon tetrachloride mainly includes rectification method, absorption process, partial hydrolysis method, complexometry, light chlorination process etc..Wherein rectifying column and absorption process belong to Physical, only can prepare the Silicon chloride. of certain purity, have problems when preparing optical fiber ultrapure silicon tetrachloride；Partial hydrolysis method, complexometry and light chlorination process belong to chemical method, by reacting the impurity removed in Silicon chloride., may be used for preparing optical fiber ultrapure silicon tetrachloride, but because partial hydrolysis method and complexometry have operating difficulties and cannot the shortcoming of large-scale production, its application is restricted, and light chlorination process is absent from the problems referred to above, therefore the present invention adopts light chlorination process to prepare optical fiber ultrapure silicon tetrachloride.
At present domestic in preparing optical fiber ultrapure silicon tetrachloride on a large scale also in blank.Beijing total institute of coloured research discloses a kind of rectification formula photochlorination apparatus (number of patent application: 200910260296.X), and this device is only applicable to laboratory research, it is impossible to realizes producing continuously and amplifies with effectively industry.Wuhan New Silicon Technology Co., Ltd. discloses the continuous distillation method of a kind of optical fiber high purity silicon tetrachloride, though solving continuous and large-scale production problem, but the purity of Silicon chloride. is unable to reach ultrapure requirement.
Therefore, the technology of existing purification Silicon chloride. need further research.
Summary of the invention
It is contemplated that solve one of above-mentioned technical problem at least to a certain extent or provide at a kind of useful business selection.For this, a kind of method that it is an object of the present invention to propose purification Silicon chloride., the method can significantly improve the purity of Silicon chloride., thus obtaining the ultrapure silicon tetrachloride of optical fiber rank.
In of the embodiment of the present invention, the present invention proposes a kind of method of purification Silicon chloride., including:
(1) thick Silicon chloride. is utilized to absorb chlorine, in order to be absorbed saturated thick Silicon chloride., and wherein, described thick Silicon chloride. contains trichlorosilane；
(2) the saturated thick Silicon chloride. of the described absorption that step (1) obtained carries out optical chlorinating reaction, in order to obtaining optical chlorinating reaction product, wherein, described optical chlorinating reaction makes described trichlorosilane be converted into Silicon chloride.；
(3) adopt nitrogen described optical chlorinating reaction product that step (2) is obtained to carry out stripping process, in order to separate unreacted chlorine, and obtain Silicon chloride. after air stripping；
(4) after described air stripping step (3) obtained, Silicon chloride. carries out the first rectification process, in order to obtain tower top tail gas and the Silicon chloride. through the first rectification process；And
(5) the described Silicon chloride. through the first rectification process that step (4) obtains is carried out the second rectification process, in order to obtain tower bottoms and purified Silicon chloride..
The method of purification Silicon chloride. according to embodiments of the present invention is by combining absorption, optical chlorinating reaction, air stripping and rectification process, and ensure to carry out optical chlorinating reaction when Silicon chloride. absorption chlorine is saturated, optical chlorinating reaction efficiency can be significantly improved, and then can prepare the Silicon chloride. of optical fiber rank, thus it is low and cannot the problem of large-scale continuous production to solve optical chlorinating reaction efficiency.
It addition, the method for purification Silicon chloride. according to the above embodiment of the present invention can also have following additional technical characteristic:
In some embodiments of the invention, in step (1), the purity of described thick Silicon chloride. is 99.9～99.99%, and the purity of described chlorine is 99.99～99.9999%.Thus, it is possible to effectively prepare the Silicon chloride. of optical fiber rank.
In some embodiments of the invention, in step (1), utilizing thick Silicon chloride. to absorb chlorine and carry out in absorption tower, wherein, tower top temperature is 45～55 degrees Celsius, and pressure is 0.15～0.25MPa.Thus, it is possible to significantly improve absorption efficiency.
In some embodiments of the invention, in step (2), described optical chlorinating reaction is to carry out in multiple optical chlorinating reaction devices of series connection, it is preferred that described optical chlorinating reaction is to carry out in four optical chlorinating reaction devices of series connection.Thus, it is possible to significantly improve optical chlorinating reaction efficiency.
In some embodiments of the invention, before carrying out next stage optical chlorinating reaction, the photochemical chlorination product in advance upper level obtained carries out cooling process.Thus, it is possible to improve optical chlorinating reaction efficiency further.
In some embodiments of the invention, described cooling processes is carry out at the temperature of 25～45 degrees Celsius and 0.05～0.1MPa pressure condition.Thus, it is possible to significantly improve cooling treatment effeciency.
In some embodiments of the invention, in step (2), the light source utilizing wavelength to be 300～400 nanometers carries out described optical chlorinating reaction.
In some embodiments of the invention, described light source is high voltage mercury lamp or low pressure mercury lamp, it is preferable that high voltage mercury lamp.Thus, it is possible to improve optical chlorinating reaction efficiency further.
In some embodiments of the invention, in step (2), described optical chlorinating reaction is to carry out at the temperature of 25～45 degrees Celsius and the pressure of 0.05～0.1MPa.Thus, it is possible to improve optical chlorinating reaction efficiency further.
In some embodiments of the invention, in step (3), the purity of described nitrogen is 99.99～99.9999%.Thus, it is possible to effectively prepare optical fiber rank Silicon chloride. further.
In some embodiments of the invention, in step (3), described stripping process is to carry out in stripping tower, and wherein, tower top temperature is 15～25 degrees Celsius, and pressure is 0.35～0.45MPa.Thus, it is possible to significantly improve stripping process efficiency.
In some embodiments of the invention, in step (4), described first rectification process is to carry out when tower top temperature is 95～105 degrees Celsius and pressure is 0.3～0.4MPa.Thus, it is possible to significantly improve the first rectification process efficiency.
In some embodiments of the invention, in step (5), described second rectification process is to carry out when tower top temperature is 70～80 degrees Celsius and pressure is 0.15～0.25MPa.Thus, it is possible to significantly improve rectification process efficiency.Thus, it is possible to significantly improve the second rectification process efficiency.
The additional aspect of the present invention and advantage will part provide in the following description, and part will become apparent from the description below, or is recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage are from conjunction with will be apparent from easy to understand the accompanying drawings below description to embodiment, wherein:
Fig. 1 is the method flow schematic diagram of purification Silicon chloride. according to an embodiment of the invention；
Fig. 2 is the system structure schematic diagram of the purification Silicon chloride. of the method for the purification Silicon chloride. implementing one embodiment of the invention；
Fig. 3 is the system structure schematic diagram of the purification Silicon chloride. of the method for the purification Silicon chloride. implementing another embodiment of the present invention.
Detailed description of the invention
Being 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 the element of same or like function from start to finish.The embodiment described below with reference to accompanying drawing is illustrative of, it is intended to is used for explaining the present invention, and is not considered as limiting the invention.
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 ", orientation or the position relationship of the instruction such as " counterclockwise " are based on orientation shown in the drawings or position relationship, it is for only for ease of the description present invention and simplifies description, rather than the device of instruction or hint indication or element must have specific orientation, with specific azimuth configuration and operation, therefore it is not considered as limiting the invention.
Additionally, term " first ", " second " are only for descriptive purposes, and it is not intended that indicate or imply relative importance or the implicit quantity indicating indicated technical characteristic.Thus, define " first ", the feature of " second " can express or implicitly include one or more these features.In describing the invention, " multiple " are meant that two or more, 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, for instance, it is possible to it is fixing connection, it is also possible to be removably connect, or connect integratedly；Can be mechanically connected, it is also possible to be electrical connection；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, it is possible to be the connection of two element internals.For the ordinary skill in the art, it is possible to understand above-mentioned term concrete meaning in the present invention as the case may be.
In one aspect of the invention, a kind of method that the present invention proposes purification Silicon chloride..Below with reference to Fig. 1, the method for the purification Silicon chloride. of the embodiment of the present invention is described in detail.According to embodiments of the invention, the method includes:
S100: absorb
According to embodiments of the invention, thick Silicon chloride. is utilized to absorb chlorine, such that it is able to the saturated thick Silicon chloride. that is absorbed.According to a particular embodiment of the invention, containing trichlorosilane in thick Silicon chloride..According to embodiments of the invention, the purity of thick Silicon chloride. and chlorine is not particularly restricted, and according to a particular embodiment of the invention, the purity of thick Silicon chloride. can be 99.9～99.99%, and the purity of chlorine can be 99.99～99.9999%.According to embodiments of the invention, the condition that thick Silicon chloride. absorbs chlorine is utilized to be not particularly restricted, according to a particular embodiment of the invention, utilize thick Silicon chloride. to absorb chlorine to carry out in absorption tower, for instance can carry out in high-purity chlorine gas absorption tower, the concrete example according to the present invention, absorption tower can be regular packed tower or random packing tower, theoretical cam curve can be 5～10, and tower top temperature can be 45～55 degrees Celsius, and pressure can be 0.15～0.25MPa.Specifically, Silicon chloride. enters from top, absorption tower, and chlorine enters bottom absorption tower, such that it is able to the saturated Silicon chloride. that is absorbed, wherein unabsorbed chlorine is discharged into exhaust treatment system from tower top.Inventor is had been surprisingly found that by great many of experiments, before carrying out optical chlorinating reaction, advance with thick Silicon chloride. and absorb chlorine, then the saturated Silicon chloride. that absorbs obtained is carried out follow-up series reaction, optical chlorinating reaction efficiency can be significantly improved, thus efficiently solving the inefficient problem of optical chlorinating reaction.
S200: optical chlorinating reaction
According to embodiments of the invention, by obtained as above to the saturated Silicon chloride. that absorbs carry out optical chlorinating reaction, in order to make the trichlorosilane in Silicon chloride. be converted into Silicon chloride., thus obtaining the optical chlorinating reaction product containing Silicon chloride..According to embodiments of the invention, the condition of optical chlorinating reaction is not particularly restricted, and according to a particular embodiment of the invention, optical chlorinating reaction can carry out at the temperature of 25～45 degrees Celsius and 0.05～0.1MPa pressure condition.According to embodiments of the invention, the light conditions of optical chlorinating reaction is not particularly restricted, according to a particular embodiment of the invention, it is possible to use the light source that wavelength is 300～400 nanometers carries out optical chlorinating reaction.According to embodiments of the invention, the particular type of light source is not particularly restricted, and according to a particular embodiment of the invention, light source can be high voltage mercury lamp or low pressure mercury lamp, it is preferable that high voltage mercury lamp.In this step, optical chlorinating reaction can carry out in multiple optical chlorinating reaction devices of series connection, for instance optical chlorinating reaction can carry out in four optical chlorinating reaction devices of series connection.nullWherein，Optical chlorinating reaction device includes borosilicate glass tube and the light source of hollow，Borosilicate glass tube limits optical chlorinating reaction space，Light source is arranged in optical chlorinating reaction space，The length of borosilicate glass tube is 500～1500 millimeters，And light source and borosilicate glass tube are coaxial clyinder，Distance between outer wall and the inwall of borosilicate glass tube of light source is 3～5 millimeters，This gap can pass into air to take away the partial heat that light source sends，Simultaneously，Before carrying out next stage optical chlorinating reaction，The optical chlorinating reaction product that upper level is obtained carries out cooling process，Specifically，Optical chlorinating reaction includes one-level to level Four optical chlorinating reaction，Absorb saturated Silicon chloride. and first carry out one-level optical chlorinating reaction，The one-level optical chlorinating reaction product obtained is carried out cooling process through cooling unit，Then the one-level optical chlorinating reaction product processed through supercooling is carried out secondary light chlorination reaction，The secondary light chlorination reaction product obtained is carried out cooling process，Then the secondary light chlorination reaction product processed through supercooling is carried out three grades of optical chlorinating reactions，The three grades of optical chlorinating reaction products obtained are carried out cooling process，Then the three grades of optical chlorinating reaction products processed through supercooling are carried out level Four optical chlorinating reaction，Obtain level Four optical chlorinating reaction product.According to embodiments of the invention, the condition that cooling processes is not particularly restricted, and according to a particular embodiment of the invention, cooling processes and can carry out at the temperature of 25～45 degrees Celsius and 0.05～0.1MPa pressure condition.It is for instance possible to use cooling water jecket carries out cooling process.Inventor have found that, too high the carrying out being unfavorable for reaction of temperature in optical chlorinating reaction process, and temperature is too low makes reaction rate be decreased obviously, although existing optical chlorinating reaction technology adopting and carrying out optical chlorinating reaction at a lower temperature, exothermic reaction is belonged to yet with optical chlorinating reaction, and optical chlorinating reaction product absorbs heat of light source makes temperature of charge rising be unfavorable for reaction equally, therefore inventor finds to carry out optical chlorinating reaction classification by big quantity research, and carry out next stage optical chlorinating reaction after upper level optical chlorinating reaction product is carried out cooling process again, it is possible not only to solve the too high problem being unfavorable for reaction of temperature of charge, and optical chlorinating reaction efficiency can be significantly improved.
S300: stripping process
According to embodiments of the invention, adopt nitrogen to obtained as above to optical chlorinating reaction product carry out stripping process, to separate unreacted chlorine, such that it is able to obtain the Silicon chloride. after air stripping, and the gas stripping gas (unreacted chlorine) obtained is passed into follow-up vent gas treatment operation.According to embodiments of the invention, stripping process can carry out in stripping tower, such as can carry out in high pure nitrogen stripping tower, concrete example according to the present invention, it is possible to adopt regular packed tower or random packing tower to carry out stripping process, wherein, theoretical cam curve can be 5～10, operation pressure limit can be 0.35～0.45MPa, and tower top operating temperature range can be 15～25 DEG C, and the purity of nitrogen can be 99.99～99.9999%.In this step, specifically, high pure nitrogen enters bottom stripping tower, and gas stripping gas is discharged into exhaust treatment system from tower top, and the Silicon chloride. after air stripping is discharged from stripper-overhead.
S400: the first rectification process
According to embodiments of the invention, by obtained as above to air stripping after Silicon chloride. carry out the first rectification process, such that it is able to obtain tower top tail gas and the Silicon chloride. through the first rectification process, according to a particular embodiment of the invention, tower top tail gas can contain nitrogen, chlorine and a small amount of Silicon chloride..In this step, specifically, first rectification process can adopt lights removal tower, such as can adopt regular packed tower, theoretical cam curve is 80～100 pieces, operation pressure limit is 0.3～0.4MPa, and tower top operating temperature range is 95～105 DEG C, and after reflux entry ratio and backflow and air stripping, the mass flowrate ratio of Silicon chloride. ranges for 6～10.
S500: the second rectification process
According to embodiments of the invention, by obtained as above to the Silicon chloride. through the first rectification process carry out the second rectification process, such that it is able to obtain tower bottoms and purified Silicon chloride., according to a particular embodiment of the invention, tower bottoms can contain the methylchlorosilane of chlorination and a small amount of Silicon chloride..According to embodiments of the invention, the purity of purified Silicon chloride. can reach 99.9999%.In this step, specifically, second rectification process can adopt heavies removal column, such as can adopt regular packed tower, theoretical cam curve is 100～120 pieces, operation pressure limit is 0.15～0.25MPa, and tower top operating temperature range is 70～80 DEG C, and the mass flowrate ratio of reflux entry ratio and backflow and the Silicon chloride. through the first rectification process ranges for 8～12.
As it has been described above, the method for purification Silicon chloride. according to embodiments of the present invention can have selected from following advantage at least one:
The method of purification Silicon chloride. according to embodiments of the present invention is by combining absorption, optical chlorinating reaction, air stripping and distillation technology, optical chlorinating reaction is carried out guaranteeing to absorb under saturated premise, ensure that reaction efficiency, air stripping and distillation technology are applied to the post processing of logistics after reacting simultaneously, thus being further ensured that the purity of ultrapure silicon tetrachloride product；
The method of purification Silicon chloride. according to embodiments of the present invention easily realizes extensive and continuous prodution.
Above the method for the purification Silicon chloride. of the embodiment of the present invention being described in detail, understood in order to convenient, the system below with reference to the purification Silicon chloride. of the method for the Fig. 2 purification Silicon chloride. to implementing the embodiment of the present invention is described in detail.According to embodiments of the invention, this system includes:
Absorption plant 100: according to embodiments of the invention, absorption plant 100 is suitable to utilize thick Silicon chloride. to absorb chlorine, such that it is able to the saturated thick Silicon chloride. that is absorbed.According to a particular embodiment of the invention, containing trichlorosilane in thick Silicon chloride..According to embodiments of the invention, the purity of thick Silicon chloride. and chlorine is not particularly restricted, and according to a particular embodiment of the invention, the purity of thick Silicon chloride. can be 99.9～99.99%, and the purity of chlorine can be 99.99～99.9999%.According to embodiments of the invention, absorption plant can be absorption tower, for example with high-purity chlorine gas absorption tower, according to a particular embodiment of the invention, absorption tower can be regular flavoring agent tower or random packing tower, theoretical cam curve can be 5～10, and tower top temperature can be 45～55 degrees Celsius, and pressure can be 0.15～0.25MPa.Specifically, Silicon chloride. enters from top, absorption tower, and chlorine enters bottom absorption tower, such that it is able to the saturated Silicon chloride. that is absorbed, wherein unabsorbed chlorine is discharged into exhaust treatment system from tower top.Inventor is had been surprisingly found that by great many of experiments, before carrying out optical chlorinating reaction, advance with thick Silicon chloride. and absorb chlorine, then the saturated Silicon chloride. that absorbs obtained is carried out follow-up series reaction, optical chlorinating reaction efficiency can be significantly improved, thus efficiently solving the inefficient problem of optical chlorinating reaction.
Optical chlorinating reaction unit 200: according to embodiments of the invention, optical chlorinating reaction unit 200 is connected with absorption plant 100, and be suitable to by obtained as above to absorb saturated Silicon chloride. carry out optical chlorinating reaction, so that the trichlorosilane in Silicon chloride. is converted into Silicon chloride., thus obtaining the optical chlorinating reaction product containing Silicon chloride..According to embodiments of the invention, the condition of optical chlorinating reaction is not particularly restricted, and according to a particular embodiment of the invention, optical chlorinating reaction can carry out at the temperature of 25～45 degrees Celsius and 0.05～0.1MPa pressure condition.According to embodiments of the invention, the light conditions of optical chlorinating reaction is not particularly restricted, and according to a particular embodiment of the invention, the light source utilizing wavelength to be 300～400 nanometers carries out optical chlorinating reaction.According to embodiments of the invention, the particular type of light source is not particularly restricted, and according to a particular embodiment of the invention, light source can be high voltage mercury lamp or low pressure mercury lamp, it is preferable that high voltage mercury lamp.According to a particular embodiment of the invention, optical chlorinating reaction unit can include multiple optical chlorinating reaction devices of series connection, for instance optical chlorinating reaction unit can include four optical chlorinating reaction devices of series connection.nullWherein，Optical chlorinating reaction device includes borosilicate glass tube and the light source of hollow，Borosilicate glass tube limits optical chlorinating reaction space，Light source is arranged in optical chlorinating reaction space，The length of borosilicate glass tube is 500～1500 millimeters，And light source and borosilicate glass tube are coaxial clyinder，Distance between outer wall and the inwall of borosilicate glass tube of light source is 3～5 millimeters，This gap can pass into air to take away the partial heat that light source sends，Simultaneously，Between two adjacent optical chlorinating reaction devices, cooling unit is set，Specifically，Optical chlorinating reaction unit includes one-level to level Four optical chlorinating reaction device，Absorb saturated Silicon chloride. and first in one-level optical chlorinating reaction device, carry out one-level optical chlorinating reaction，The one-level optical chlorinating reaction product obtained is carried out cooling process through cooling unit，Then the one-level optical chlorinating reaction product processed through supercooling is carried out secondary light chlorination reaction in secondary light chlorination reactor，The secondary light chlorination reaction product obtained is carried out cooling process through cooling unit，Then the secondary light chlorination reaction product processed through supercooling is carried out three grades of optical chlorinating reactions in three grades of optical chlorinating reaction devices，The three grades of optical chlorinating reaction products obtained are carried out cooling process through cooling unit，Then the three grades of optical chlorinating reaction products processed through supercooling are carried out level Four optical chlorinating reaction in level Four optical chlorinating reaction device，Obtain level Four optical chlorinating reaction product.According to embodiments of the invention, the condition that cooling processes is not particularly restricted, and according to a particular embodiment of the invention, cooling processes and can carry out at the temperature of 25～45 degrees Celsius and 0.05～0.1MPa pressure condition.According to embodiments of the invention, cooling unit can be cooling water jecket.Inventor have found that, too high the carrying out being unfavorable for reaction of temperature in optical chlorinating reaction process, and temperature is too low makes reaction rate be decreased obviously, although existing optical chlorinating reaction technology adopting and carrying out optical chlorinating reaction at a lower temperature, exothermic reaction is belonged to yet with optical chlorinating reaction, and optical chlorinating reaction product absorbs heat of light source makes temperature of charge rising be unfavorable for reaction equally, therefore by big quantity research, inventor finds that the optical chlorinating reaction device adopting series connection carries out optical chlorinating reaction process, and between adjacent light greening reactor, cooling unit is set, it is possible not only to solve the too high problem being unfavorable for reaction of temperature of charge, and optical chlorinating reaction efficiency can be significantly improved.
Air-lift device 300: according to embodiments of the invention, air-lift device 300 is connected with optical chlorinating reaction unit 200, and be suitable for use with nitrogen to obtained as above to optical chlorinating reaction product carry out stripping process, to separate unreacted chlorine, such that it is able to obtain the Silicon chloride. after air stripping, and the gas stripping gas (unreacted chlorine) obtained is passed into follow-up vent gas treatment operation.According to embodiments of the invention, air-lift device can be stripping tower, it can be such as high pure nitrogen stripping tower, concrete example according to the present invention, it is possible to adopt regular packed tower or random packing tower to carry out stripping process, wherein, theoretical cam curve can be 5～10, operation pressure limit can be 0.35～0.45MPa, and tower top operating temperature range can be 15～25 DEG C, and the purity of nitrogen can be 99.99～99.9999%.Specifically, high pure nitrogen enters bottom stripping tower, and gas stripping gas is discharged into exhaust treatment system from tower top, and the Silicon chloride. after air stripping is discharged from stripper-overhead.
First rectifier unit 400: according to embodiments of the invention, first rectifier unit 400 is connected with air-lift device 300, and be suitable to by obtained as above to air stripping after Silicon chloride. carry out the first rectification process, such that it is able to obtain tower top tail gas and the Silicon chloride. through the first rectification process, according to a particular embodiment of the invention, tower top tail gas can contain nitrogen, chlorine and a small amount of Silicon chloride..Specifically, first rectifier unit can be lights removal tower, it can be such as regular packed tower, theoretical cam curve is 80～100 pieces, operation pressure limit is 0.3～0.4MPa, tower top operating temperature range is 95～105 DEG C, and after reflux entry ratio and backflow and air stripping, the mass flowrate ratio of Silicon chloride. ranges for 6～10.
Second rectifier unit 500: according to embodiments of the invention, second rectifier unit 500 is connected with the first rectifier unit 400, and be suitable to by obtained as above to the Silicon chloride. through the first rectification process carry out the second rectification process, such that it is able to obtain tower bottoms and purified Silicon chloride., according to a particular embodiment of the invention, tower bottoms contains the methylchlorosilane of chlorination and a small amount of Silicon chloride..According to embodiments of the invention, the purity of purified Silicon chloride. can reach 99.9999%.Specifically, second rectification process device can be heavies removal column, it can be such as regular packed tower, theoretical cam curve is 100～120 pieces, operation pressure limit is 0.15～0.25MPa, tower top operating temperature range is 70～80 DEG C, and the mass flowrate ratio of reflux entry ratio and backflow and the Silicon chloride. through the first rectification process ranges for 8～12.
Below with reference to specific embodiment, present invention is described, it is necessary to explanation, and these embodiments are only illustrative, and do not limit the present invention in any way.
Embodiment
nullWith reference to Fig. 3，Silicon chloride. A is passed into from top, absorption tower 100，High-purity chlorine B enters bottom absorption tower 100，Absorption tower carries out absorption process，The not adsorbed high-purity chlorine obtained is discharged into exhaust treatment system 600 from tower top，The saturated Silicon chloride. of chlorine absorption is from entering one-level optical chlorinating reaction device 210 by potential difference at the bottom of tower and carrying out optical chlorinating reaction，The one-level optical chlorinating reaction product obtained is carried out cooling process through the first cooling unit 220，Then the one-level optical chlorinating reaction product processed through supercooling is carried out secondary light chlorination reaction in secondary light chlorination reactor 230，The secondary light chlorination reaction product obtained is carried out cooling process in the second cooling unit 240，Then the secondary light chlorination reaction product processed through supercooling is carried out three grades of optical chlorinating reactions in three grades of optical chlorinating reaction devices 250，Obtain three grades of optical chlorinating reaction products are carried out cooling process in the 3rd cooling unit 260，Then the three grades of optical chlorinating reaction products processed through supercooling are carried out level Four optical chlorinating reaction in level Four optical chlorinating reaction device 270，Obtain optical chlorinating reaction product，Obtained optical chlorinating reaction product is entered from stripping tower 300 top，High pure nitrogen enters bottom stripping tower 300，The unreacted chlorine obtained and nitrogen mixture are discharged into exhaust treatment system 600 from tower top，After the air stripping obtained, Silicon chloride. enters in the middle part of the first rectifier unit 400 from discharging pressured difference at the bottom of tower，Obtain tower overhead gas and the Silicon chloride. through the first rectification process，Wherein，Tower overhead gas containing light component is discharged from tower top，Silicon chloride. through the first rectification process enters in the middle part of the second rectifier unit 500 from discharging pressured difference at the bottom of tower，Obtain tower bottoms and purification Silicon chloride. that purity is 99.9999%，Wherein，Tower bottoms containing heavy constituent is discharged from the bottom of tower，Ultrapure silicon tetrachloride product tower top is discharged into subsequent handling.
In the description of this specification, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means in conjunction with this embodiment or example describe are contained at least one embodiment or the example of the present invention.In this manual, the schematic representation of above-mentioned term is not necessarily referring to identical embodiment or example.And, the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiments or example.
Although above it has been shown and described that embodiments of the invention, it is understandable that, above-described embodiment is illustrative of, being not considered as limiting the invention, above-described embodiment can be changed when without departing from principles of the invention and objective, revises, replace and modification by those of ordinary skill in the art within the scope of the invention.
Claims (11)
1. the method for a purification Silicon chloride., it is characterised in that including:
(1) thick Silicon chloride. is utilized to absorb chlorine, in order to be absorbed saturated thick Silicon chloride., and wherein, described thick Silicon chloride. contains trichlorosilane；The thick Silicon chloride. of described utilization absorbs chlorine to carry out in absorption tower, and described thick Silicon chloride. enters from top, described absorption tower, and described chlorine enters bottom described absorption tower, and wherein, tower top temperature is 45～55 degrees Celsius, and pressure is 0.15～0.25MPa；
(2) the saturated thick Silicon chloride. of the described absorption that step (1) obtained carries out optical chlorinating reaction, to obtain optical chlorinating reaction product, wherein, described optical chlorinating reaction makes described trichlorosilane be converted into Silicon chloride., described optical chlorinating reaction is to carry out in multiple optical chlorinating reaction devices of series connection, and before carrying out next stage optical chlorinating reaction, the photochemical chlorination product in advance upper level obtained carries out cooling process；
(3) adopt nitrogen described optical chlorinating reaction product that step (2) is obtained to carry out stripping process, in order to separate unreacted chlorine, and obtain Silicon chloride. after air stripping；
(4) after described air stripping step (3) obtained, Silicon chloride. carries out the first rectification process, in order to obtain tower top tail gas and the Silicon chloride. through the first rectification process；And
(5) the described Silicon chloride. through the first rectification process that step (4) obtains is carried out the second rectification process, in order to obtain tower bottoms and purified Silicon chloride..
2. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (1), the purity of described thick Silicon chloride. is 99.9～99.99%, and the purity of described chlorine is 99.99～99.9999%.
3. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (2), described optical chlorinating reaction is to carry out in four optical chlorinating reaction devices of series connection.
4. the method for purification Silicon chloride. according to claim 1, it is characterised in that it is carry out at the temperature of 25～45 degrees Celsius and 0.05～0.1MPa pressure condition that described cooling processes.
5. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (2), the light source utilizing wavelength to be 300～400 nanometers carries out described optical chlorinating reaction.
6. the method for purification Silicon chloride. according to claim 5, it is characterised in that described light source is high voltage mercury lamp or low pressure mercury lamp.
7. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (2), described optical chlorinating reaction is to carry out at the temperature of 25～45 degrees Celsius and the pressure condition of 0.05～0.1MPa.
8. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (3), the purity of described nitrogen is 99.99～99.9999%.
9. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (3), described stripping process is to carry out in stripping tower, and wherein, tower top temperature is 15～25 degrees Celsius, and pressure is 0.35～0.45MPa.
10. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (4), described first rectification process is to carry out when tower top temperature is 95～105 degrees Celsius and pressure is 0.3～0.4MPa.
11. the method for purification Silicon chloride. according to claim 1, it is characterised in that in step (5), described second rectification process is to carry out when tower top temperature is 70～80 degrees Celsius and pressure is 0.15～0.25MPa.
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| CN107720759A (en) * | 2017-11-13 | 2018-02-23 | 亚洲硅业（青海）有限公司 | The processing method of tail gas is reduced in a kind of preparation method and production of polysilicon of optical fiber level silicon tetrachloride |
| CN109534345A (en) * | 2019-01-14 | 2019-03-29 | 天津中科拓新科技有限公司 | A kind of method for cleaning and device for trichlorosilane tail gas processing |
| CN111961205B (en) * | 2020-08-13 | 2021-12-14 | 江西蓝星星火有机硅有限公司 | Process for continuously producing various low-viscosity methyl silicone oils by comprehensively utilizing methyl silicone oil polymerization material |
| CN113666378A (en) * | 2021-09-03 | 2021-11-19 | 徐州金琳光电材料产业研究院有限公司 | Preparation method of high-purity silicon dioxide for optical coating |
| CN114247180B (en) * | 2021-12-24 | 2023-07-04 | 亚洲硅业(青海)股份有限公司 | Application of activated carbon containing oxygen group in removal of impurities in silicon tetrachloride |
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| CN103183350A (en) * | 2011-12-29 | 2013-07-03 | 北京有色金属研究总院 | Preparation method of silicon tetrachloride for optical fiber |
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| CN102642839A (en) * | 2012-05-09 | 2012-08-22 | 特变电工新疆硅业有限公司 | Processing process of industrial grade silicon tetrachloride |
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