CN102908795A - Processing method and processing system for trichlorosilane synthesis tail gas - Google Patents
Processing method and processing system for trichlorosilane synthesis tail gas Download PDFInfo
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- CN102908795A CN102908795A CN201210345927XA CN201210345927A CN102908795A CN 102908795 A CN102908795 A CN 102908795A CN 201210345927X A CN201210345927X A CN 201210345927XA CN 201210345927 A CN201210345927 A CN 201210345927A CN 102908795 A CN102908795 A CN 102908795A
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Abstract
The invention discloses a processing method and a processing system for trichlorosilane synthesis tail gas. The processing method comprises the following steps of: a) adding the trichlorosilane synthesis tail gas in a washing rectifying tower, washing and rectifying in order to remove solid and metal impurities from the tail gas, thereby obtaining washed gas; b) pre-cooling the washed gas, so as to obtain first condensate and pre-cooled gas; c) carrying out heat exchanging and condensation between the pre-cooled gas and a coolant to obtain second condensate and non-condensable gas, and heating the second condensate, mixing the second condensate and the first condensate to obtain a condensate material; d) carrying out buffer processing to the condensate material to obtain a buffed condensate material; and e) selecting a predetermined percent by mass of buffered condensate material as reflowing liquid to be returned to the washing and rectifying tower for washing and rectifying. According to the method disclosed by the invention, the washed gas exhausted from the upper part of the washing and rectifying tower only contains a very small quantity of metal impurities, so that the affect on subsequent operations, caused by the metal impurities, can be reduced, and the processing stability and continuity of the trichlorosilane synthesis tail gas are improved.
Description
Technical field
The present invention relates to the trichlorosilane synthesis technical field, more specifically, the present invention relates to a kind of processing method and system of technique of trichlorosilane synthetic tail gas.
Background technology
Polysilicon is the crucial raw material of integrated circuit and photovoltaic generation, is the important content of the preferential theme of National Program for Medium-to Long-term Scientific and Technological Development manufacture field basic raw material.The industrialization technology of world's production of polysilicon mainly contains two kinds of techniques, namely improves Siemens process and silane thermal decomposition process technique.With productivity ratio, the improvement Siemens process accounts for 82% of aggregated capacity, and silane thermal decomposition process accounts for 18%, and advanced production of polysilicon technology is monopolized by a few company of the states such as U.S., day, moral always.And trichlorosilane has another name called trichlorosilane (SiHCl
3) for improveing the primary raw material of Siemens process production polysilicon.
The method of at present technique of trichlorosilane synthetic tail gas processing is mainly dry method dust and the dry and wet way dedusting combines, the shortcoming of dry method dust is having relatively high expectations to gas-solid separation equipment, and metal impurities adhere to tube wall easily, affect the continuity of system's operation, and the mode that adopts the dry and wet way dedusting to combine, can suitably reduce the separation requirement of gas-solid separation equipment, but its wet dedusting tower mostly is greatly scrubbing tower, gas still contains a large amount of metal impurities after the washing, affects the continuous and steady operation of follow-up system.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or provides at least a kind of useful commerce to select.For this reason, one object of the present invention is to propose that a kind of stability is strong, continuity good, the processing method of the obvious technique of trichlorosilane synthetic tail gas of impurity-eliminating effect.
Processing method according to the technique of trichlorosilane synthetic tail gas of the embodiment of the invention may further comprise the steps: a) technique of trichlorosilane synthetic tail gas is added the washing rectifying column and wash rectifying to remove solid and metal impurities wherein, obtain washing rear gas; B) gas after the described washing is carried out precooling, obtain gas after the first condensate liquid and the precooling; C) with gas after the described precooling and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas, and with mixing with described the first condensate liquid after described the second condensate liquid intensification, obtain the condensation material; D) described condensation material is carried out buffered, obtain cushioning the condensation material; E) the buffering condensation material of selection predetermined quality percentage returns the washing rectifying column as phegma and washs rectifying.
Processing method according to the technique of trichlorosilane synthetic tail gas of the embodiment of the invention, adopting the washing rectifying column that the washing of synthesis tail gas is separated with rectifying combines, with less wash out amount solid impurity and metal impurities are discharged, reduced supplies consumption and subsequent treatment load; After the washing out of washing rectifier, only contain the denier metal impurities the gas, can reduce to have improved Treatment Stability and the continuity of technique of trichlorosilane synthetic tail gas because metal impurities deposit the impact on subsequent operation.
In addition, the processing method of technique of trichlorosilane synthetic tail gas according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention, described step c) comprises: c-1) with gas after the described precooling and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas; C-2) gas after described the second condensate liquid and the described washing is carried out heat exchange and process, make described the second condensate liquid be warming up to 30～40 ℃; C-3) the second condensate liquid after will heating up mixes with described the first condensate liquid, obtains the condensation material.
According to one embodiment of present invention, described step c) also comprises: described fixed gas is discharged, and the discharge temperature of control fixed gas is-20～-10 ℃.
According to one embodiment of present invention, described predetermined quality percentage is 15%～50%.
According to one embodiment of present invention, described washing rectifying column comprises tower body, described tower body bottom is provided with the synthesis tail gas import, gas exported after tower body top was provided with washing, comprise the column plate district, sieve plate district and the baffle plate district that connect successively from top to bottom in the described tower body, wherein, described baffle plate district is positioned at described synthesis tail gas import top, described baffle plate radially arranges the herringbone baffle plate in the district, and described herringbone baffle plate is provided with opening to remove the solid impurity in the synthesis tail gas; Described sieve plate is provided with sieve plate in the district, and described sieve plate will screen to remove solid impurity remaining in the synthesis tail gas through the synthesis tail gas that described baffle plate district processes; Described column plate is provided with the multilayer column plate in the district, is provided with downflow weir between the adjacent tray, and metal impurities wherein will wash to remove through the synthesis tail gas that described sieve plate district processes in described column plate district.
According to one embodiment of present invention, described herringbone baffle plate is provided with 3～5 layers, and each layer herringbone baffle plate axially is alternately distributed along tower body.
According to one embodiment of present invention, described sieve plate is provided with 5～10 layers.
According to one embodiment of present invention, the sieve diameter of described sieve plate is 8～14mm, and described sieve plate is along the tower body axial distribution, and the sieve diameter of the sieve plate that distributes from top to bottom increases successively.
According to one embodiment of present invention, column plate is sieve tray or solid tongue tower tray in the described column plate district.
According to one embodiment of present invention, described column plate is provided with 10～20 layers.
According to one embodiment of present invention, described tower body bottom is provided with leakage fluid dram to discharge the raffinate that produces through washing rectifying.
Another object of the present invention is to propose a kind for the treatment of system of technique of trichlorosilane synthetic tail gas, comprising: washing rectifying column, described washing rectifying column are used for synthesis tail gas is washed rectifying to remove solid and metal impurities wherein, obtain washing rear gas; Pre-cooler, described pre-cooler carries out precooling to washing rear gas, obtains gas after the first condensate liquid and the precooling; Cryogenic system, described cryogenic system with precooling after gas and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas, the second condensate liquid returns described pre-cooler and mixes with described the first condensate liquid, obtains the condensation material; And buffer unit, described buffer unit carries out buffered with described condensation material, obtain cushioning the condensation material, and select the buffering condensation material of predetermined quality percentage to return the washing rectifying column as phegma, wherein, the washing rectifying column of described washing rectifying column for using in the processing method according to the technique of trichlorosilane synthetic tail gas described in above-described embodiment.
In addition, the treatment system of technique of trichlorosilane synthetic tail gas according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention, described predetermined quality percentage is 15～50%.
According to one embodiment of present invention, described tower body bottom is provided with leakage fluid dram to discharge the raffinate that produces through washing rectifying.
According to one embodiment of present invention, the operating pressure of described washing rectifying column is 0.15～0.25MPa, and operating temperature is 50～90 ℃.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the process flow figure according to the technique of trichlorosilane synthetic tail gas of the embodiment of the invention;
Fig. 2 is the treatment system schematic diagram according to employed technique of trichlorosilane synthetic tail gas in the processing method of the technique of trichlorosilane synthetic tail gas of the embodiment of the invention;
Fig. 3 is the washing rectifying tower structure schematic diagram according to the treatment system of technique of trichlorosilane synthetic tail gas described in Fig. 2.
The specific embodiment
The below describes embodiments of the invention in detail, and the example of described embodiment is shown in the drawings, and wherein identical or similar label represents identical or similar element or the element with identical or similar functions from start to finish.Be exemplary below by the embodiment that is described with reference to the drawings, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, it will be appreciated that, term " " center "; " vertically "; " laterally "; " 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 indications such as " counterclockwise " are based on orientation shown in the drawings or position relationship, only be for convenience of description the present invention and simplified characterization, rather than device or the element of indication or hint indication must have specific orientation, with specific orientation structure and operation, therefore can not be interpreted as limitation of the present invention.
In addition, term " first ", " second " only are used for describing purpose, and can not be interpreted as indication or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more these features can be expressed or impliedly be comprised to the feature that is limited with " first ", " second ".In description of the invention, the implication of " a plurality of " is two or more, unless clear and definite concrete restriction is arranged in addition.
In the present invention, unless clear and definite regulation and restriction are arranged in addition, broad understanding should be done in the terms such as term " installation ", " linking to each other ", " connection ", " fixing ", for example, can be to be fixedly connected with, and also can be to removably connect, or connect integratedly; Can be mechanical connection, also can be to be electrically connected; Can be directly to link to each other, also can indirectly link to each other by intermediary, can be the connection of two element internals.For the ordinary skill in the art, can understand as the case may be above-mentioned term concrete meaning in the present invention.
In the present invention, unless clear and definite regulation and restriction are arranged in addition, First Characteristic Second Characteristic it " on " or D score can comprise that the first and second features directly contact, can comprise that also the first and second features are not directly contacts but by the other feature contact between them.And, First Characteristic Second Characteristic " on ", " top " and " above " comprise First Characteristic directly over Second Characteristic and oblique upper, or only represent that the First Characteristic level height is higher than Second Characteristic.First Characteristic Second Characteristic " under ", " below " and " below " comprise First Characteristic directly over Second Characteristic and oblique upper, or only represent that the First Characteristic level height is less than Second Characteristic.
The processing method that the below at first describes according to technique of trichlorosilane synthetic tail gas of the present invention with reference to figure 1.
Particularly, as shown in Figure 1, specifically may further comprise the steps according to the processing method of the technique of trichlorosilane synthetic tail gas of the embodiment of the invention:
A) technique of trichlorosilane synthetic tail gas is added the washing rectifying column and wash rectifying to remove solid and metal impurities wherein, obtain washing rear gas;
B) gas after the described washing is carried out precooling, obtain gas after the first condensate liquid and the precooling;
C) with gas after the described precooling and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas, and with mixing with described the first condensate liquid after described the second condensate liquid intensification, obtain the condensation material;
D) described condensation material is carried out buffered, obtain cushioning the condensation material;
E) the buffering condensation material of selection predetermined quality percentage returns the washing rectifying column as phegma and washs rectifying.
Thus, processing method according to the technique of trichlorosilane synthetic tail gas of the embodiment of the invention, adopt the washing rectifying column that the washing of synthesis tail gas is separated with rectifying and combine, with less wash out amount solid impurity and metal impurities are discharged, reduced supplies consumption and subsequent treatment load; After the washing out of washing rectifier, only contain the denier metal impurities the gas, can reduce to have improved Treatment Stability and the continuity of technique of trichlorosilane synthetic tail gas because metal impurities deposit the impact on subsequent operation.
Processing method about described technique of trichlorosilane synthetic tail gas it will be appreciated that, used equipment is the treatment system of technique of trichlorosilane synthetic tail gas in the described processing method.
Preferably, as shown in Figure 2, in one example, the treatment system of technique of trichlorosilane synthetic tail gas comprises: washing rectifying column, pre-cooler 50, cryogenic system 60 and buffer unit 70.
Described washing rectifying column is used for synthesis tail gas is washed rectifying to remove solid and metal impurities wherein, obtains washing rear gas.
Gas carries out precooling after 50 pairs of washings of pre-cooler, obtains gas after the first condensate liquid and the precooling.
Further, as shown in Figure 3, in one example, comprise for the treatment of the washing rectifying column of technique of trichlorosilane synthetic tail gas: tower body 10.
Thus, adopt the treatment system of above-mentioned technique of trichlorosilane synthetic tail gas, the washing rectifying column separates the washing of synthesis tail gas and combines with rectifying, with less wash out amount solid impurity and metal impurities are discharged, and has reduced the processing load of supplies consumption and follow-up system; After the washing out of washing rectifier, only contain the denier metal impurities the gas, can reduce because the metal impurities deposition to the obstruction of follow-up system, has improved operational stability and the continuity of washing rectifying column.
About step a), particularly, the concrete processing procedure of technique of trichlorosilane synthetic tail gas in described washing rectifying column can for:
The technique of trichlorosilane synthetic tail gas that with air pressure is 0.2～0.25MPa enters in the tower from the synthesis tail gas import 11 of tower body 10 bottoms, and operating pressure is 0.15～0.25MPa in the control tower, and operating temperature is 50～90 ℃, and the cat head operating temperature is 30～50 ℃.Solid impurity in the technique of trichlorosilane synthetic tail gas and metal impurities are removed after the enrichment by baffle plate district 40, sieve plate district 30 and column plate district 20 respectively, and discharge from leakage fluid dram 13 with raffinate and to enter subsequent handling, gas then enters pre-cooler 50 and carries out precooling treatment after the washing.
In step c), the operation of gas after the described precooling and refrigerant heat exchange condensation specifically can be comprised:
C-1) with gas after the described precooling and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas;
C-2) gas after described the second condensate liquid and the described washing is carried out heat exchange and process, make described the second condensate liquid be warming up to 30～40 ℃;
C-3) the second condensate liquid after will heating up mixes with described the first condensate liquid, obtains the condensation material.
In addition, do not have particular restriction about the processing method of described fixed gas, it can be discharged, and to control its discharge temperature be-20～-10 ℃.
D) described condensation material is carried out buffered, obtain cushioning the condensation material.
In order to improve the rate of recovery of technique of trichlorosilane synthetic tail gas, the buffering condensation material that can select predetermined quality percentage returns the washing rectifying column as phegma and washs rectifying.Preferably, according to one embodiment of present invention, described predetermined quality percentage is 15%～50%, and all the other condensate liquids are discharged and entered the subsequent purification separation circuit.
Specifically describe employed washing rectifying column in above-described embodiment below in conjunction with Fig. 3.
Preferably, in one example, baffle plate district 40 is positioned at synthesis tail gas import 11 tops, and herringbone baffle plate 41 radially is set in the baffle plate district 40, and herringbone baffle plate 41 is provided with opening 411 to remove the solid impurity in the synthesis tail gas.
Be provided with sieve plate 31 in the sieve plate district 30, sieve plate 31 will screen to remove solid impurity remaining in the synthesis tail gas through the synthesis tail gas that baffle plate district 40 processes.
Be provided with multilayer column plate 21 in the column plate district 20, be provided with downflow weir 22 between the adjacent tray 21, metal impurities wherein will wash to remove through the synthesis tail gas that sieve plate district 30 processes in column plate district 20.
In one example, herringbone baffle plate 41 is provided with 3～5 layers, and each layer herringbone baffle plate 41 axially is alternately distributed along tower body 10.Thus, most solid particle polluter in the technique of trichlorosilane synthetic tail gas can be removed in this zone, it is entered in the cleaning solution discharge as raffinate.
Further, in one example, sieve plate 31 is provided with 5～10 layers.Advantageously, according to one embodiment of present invention, the sieve diameter of sieve plate 31 is 8～14mm, and sieve plate 31 is along tower body 10 axial distribution, and the sieve diameter of the sieve plate 31 that distributes from top to bottom increases successively.Thus, solid impurity remaining in the technique of trichlorosilane synthetic tail gas and the metal impurities of fraction can be removed in this zone, can avoid the solid particle polluter in the synthesis tail gas that its upper area is resulted in blockage simultaneously.
Selection about the column plate 21 in the column plate district 20 does not have particular restriction, sieve tray or the solid tongue tower tray that for example can commonly use for those of ordinary skills.Preferably, in one example, column plate 21 is provided with 10～20 layers.Thus, the most of metal impurities in the technique of trichlorosilane synthetic tail gas can be removed in this zone, the metals content impurity that washs in the rear gas is enough hanged down consequently still can not deposit and blocking pipe under the state of deep cooling.
Advantageously, in one example, tower body 10 bottoms are provided with leakage fluid dram 13 to discharge the raffinate that produces through washing rectifying.Thus, the solid particle polluter of removing in the baffle plate district 40 enters and can be used as raffinate behind the cleaning solution and discharge from leakage fluid dram 13.
In order to guarantee that the present invention washs the normal operation of rectifying column, and guarantee dust removal rate, preferably, in one example, the operating pressure that can control described washing rectifying column is 0.15～0.25MPa, and operating temperature is 50～90 ℃.
In the description of this specification, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or the example in conjunction with specific features, structure, material or the characteristics of this embodiment or example description.In this manual, the schematic statement of above-mentioned term not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or characteristics can be with suitable mode combinations in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple variation, modification, replacement and modification to these embodiment in the situation that does not break away from principle of the present invention and aim, scope of the present invention is limited by claim and equivalent thereof.
Claims (15)
1. the processing method of a technique of trichlorosilane synthetic tail gas is characterized in that, may further comprise the steps:
A) technique of trichlorosilane synthetic tail gas is added the washing rectifying column and wash rectifying to remove solid and metal impurities wherein, obtain washing rear gas;
B) gas after the described washing is carried out precooling, obtain gas after the first condensate liquid and the precooling;
C) with gas after the described precooling and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas, and with mixing with described the first condensate liquid after described the second condensate liquid intensification, obtain the condensation material;
D) described condensation material is carried out buffered, obtain cushioning the condensation material;
E) the buffering condensation material of selection predetermined quality percentage returns the washing rectifying column as phegma and washs rectifying.
2. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1 is characterized in that, described step c) comprises:
C-1) with gas after the described precooling and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas;
C-2) gas after described the second condensate liquid and the described washing is carried out heat exchange and process, make described the second condensate liquid be warming up to 30～40 ℃;
C-3) the second condensate liquid after will heating up mixes with described the first condensate liquid, obtains the condensation material.
3. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1 is characterized in that, described step c) also comprises: described fixed gas is discharged, and the discharge temperature of control fixed gas is-20～-10 ℃.
4. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1 is characterized in that, described predetermined quality percentage is 15%～50%.
5. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, it is characterized in that, described washing rectifying column comprises tower body, described tower body bottom is provided with the synthesis tail gas import, gas exported after tower body top was provided with washing, comprise the column plate district, sieve plate district and the baffle plate district that connect successively from top to bottom in the described tower body
Wherein, described baffle plate district is positioned at described synthesis tail gas import top, and described baffle plate radially arranges the herringbone baffle plate in the district, and described herringbone baffle plate is provided with opening to remove the solid impurity in the synthesis tail gas;
Described sieve plate is provided with sieve plate in the district, and described sieve plate will screen to remove solid impurity remaining in the synthesis tail gas through the synthesis tail gas that described baffle plate district processes;
Described column plate is provided with the multilayer column plate in the district, is provided with downflow weir between the adjacent tray, and metal impurities wherein will wash to remove through the synthesis tail gas that described sieve plate district processes in described column plate district.
6. the processing method of technique of trichlorosilane synthetic tail gas according to claim 5 is characterized in that, described herringbone baffle plate is provided with 3～5 layers, and each layer herringbone baffle plate axially is alternately distributed along tower body.
7. the processing method of technique of trichlorosilane synthetic tail gas according to claim 5 is characterized in that, described sieve plate is provided with 5～10 layers.
8. the processing method of technique of trichlorosilane synthetic tail gas according to claim 7 is characterized in that, the sieve diameter of described sieve plate is 8～14mm, and described sieve plate is along the tower body axial distribution, and the sieve diameter of the sieve plate that distributes from top to bottom increases successively.
9. the processing method of technique of trichlorosilane synthetic tail gas according to claim 5 is characterized in that, column plate is sieve tray or solid tongue tower tray in the described column plate district.
10. the processing method of technique of trichlorosilane synthetic tail gas according to claim 9 is characterized in that, described column plate is provided with 10～20 layers.
11. the processing method of technique of trichlorosilane synthetic tail gas according to claim 5 is characterized in that, described tower body bottom is provided with leakage fluid dram to discharge the raffinate that produces through washing rectifying.
12. the treatment system of a technique of trichlorosilane synthetic tail gas is characterized in that, comprising:
Washing rectifying column, described washing rectifying column are used for synthesis tail gas is washed rectifying to remove solid and metal impurities wherein, obtain washing rear gas;
Pre-cooler, described pre-cooler carries out precooling to washing rear gas, obtains gas after the first condensate liquid and the precooling;
Cryogenic system, described cryogenic system with precooling after gas and refrigerant heat exchange condensation, obtain the second condensate liquid and fixed gas, the second condensate liquid returns described pre-cooler and mixes with described the first condensate liquid, obtains the condensation material; With
Buffer unit, described buffer unit carries out buffered with described condensation material, obtains cushioning the condensation material, and selects the buffering condensation material of predetermined quality percentage to return the washing rectifying column as phegma,
Wherein, described washing rectifying column is the washing rectifying column that uses in the processing method of according to claim 1-11 technique of trichlorosilane synthetic tail gas described in each.
13. the treatment system of technique of trichlorosilane synthetic tail gas according to claim 12 is characterized in that, described predetermined quality percentage is 15～50%.
14. the treatment system of technique of trichlorosilane synthetic tail gas according to claim 12 is characterized in that, described tower body bottom is provided with leakage fluid dram to discharge the raffinate that produces through washing rectifying.
15. the treatment system of technique of trichlorosilane synthetic tail gas according to claim 12 is characterized in that, the operating pressure of described washing rectifying column is 0.15～0.25MPa, and operating temperature is 50～90 ℃.
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| CN102908795B (en) | 2015-08-05 |
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