CN115738382A - Method and system for removing impurities from trichlorosilane - Google Patents
Method and system for removing impurities from trichlorosilane Download PDFInfo
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- CN115738382A CN115738382A CN202211480624.9A CN202211480624A CN115738382A CN 115738382 A CN115738382 A CN 115738382A CN 202211480624 A CN202211480624 A CN 202211480624A CN 115738382 A CN115738382 A CN 115738382A
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- 239000012535 impurity Substances 0.000 title claims abstract description 133
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 46
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- 238000011069 regeneration method Methods 0.000 claims abstract description 211
- 238000001179 sorption measurement Methods 0.000 claims abstract description 145
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- 239000003463 adsorbent Substances 0.000 claims abstract description 140
- 239000007787 solid Substances 0.000 claims abstract description 126
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- 239000012752 auxiliary agent Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002808 molecular sieve Substances 0.000 claims description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 6
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- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 claims description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 230000002238 attenuated effect Effects 0.000 description 1
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- 238000011044 inertial separation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
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- 238000000746 purification Methods 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a method for adsorbing and removing impurities from trichlorosilane, which comprises the following steps: introducing trichlorosilane liquid containing impurities into a liquid-solid fluidized bed, adding an adsorbent, and carrying out adsorption impurity removal on the trichlorosilane liquid; discharging the adsorbent after adsorbing the impurities to a regeneration reactor for regeneration treatment; and returning the regenerated adsorbent to the liquid-solid fluidized bed for adsorption and impurity removal again. The invention also discloses a system for adsorbing and removing impurities from trichlorosilane. The method can optimize the trichlorosilane impurity removal process, realize on-line continuous regeneration and greatly improve the adsorption impurity removal efficiency.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon production, and particularly relates to a method and a system for adsorbing and removing impurities from trichlorosilane.
Background
In the prior art, the production of polysilicon uses an improved Siemens method for 90 percent, namely trichlorosilane (SiHCL) 3 TCS) and hydrogen are deposited in a chemical vapor deposition reactor to produce polycrystalline silicon. Trace impurities such as boron, phosphorus, metal, carbon and the like in the trichlorosilane can have great influence on the purity of the polycrystalline silicon product. At present, the technology for purifying trichlorosilane mainly comprises rectification, adsorption rectification, reaction rectification and extraction rectification technologies combining rectification and adsorption, reaction or extraction, wherein an adsorption rectification method combining adsorption and rectification is the most widely applied purification technology in China.
The adsorption rectification method is that trichlorosilane containing impurities is respectively introduced into a boron and phosphorus removal adsorption column, a metal removal adsorption column and a carbon removal adsorption column, and then the trichlorosilane adsorbed by the adsorption columns is further subjected to multistage rectification to further remove the impurities. Wherein, the adsorption column needs to change or regenerate the adsorbent after a certain adsorption time in the process of adsorption and impurity removal. Adsorption times vary from weeks to months depending on the adsorbent. According to the adsorption characteristic of the adsorbent, the adsorption performance is gradually attenuated along with the increase of the adsorption time, so that the fluctuation of the adsorption efficiency of the adsorption column can be caused. The adsorption column is used as a fixed bed reactor, regeneration or replacement of an adsorbent can be carried out only after the standby adsorption column is switched, online regeneration cannot be realized, the efficiency is low, and the regeneration process is complex. Moreover, different adsorbents have different adsorption characteristics to different impurities, and special adsorption columns must be respectively arranged for adsorption, so that the cost and complexity of equipment are increased.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art, and provides a method and a system for trichlorosilane adsorption impurity removal, which can optimize a trichlorosilane impurity removal process, realize online continuous regeneration and greatly improve the adsorption impurity removal efficiency.
The technical scheme for solving the technical problems is as follows:
according to one aspect of the invention, a method for adsorbing and removing impurities from trichlorosilane is provided, which comprises the following steps:
introducing the trichlorosilane liquid containing impurities into a liquid-solid fluidized bed, adding an adsorbent, and carrying out adsorption impurity removal on the trichlorosilane liquid;
discharging the adsorbent after adsorbing the impurities to a regeneration reactor for regeneration treatment;
and returning the regenerated adsorbent to the liquid-solid fluidized bed for adsorption and impurity removal again.
Preferably, the regeneration treatment specifically includes:
introducing regeneration gas into the regeneration reactor, and heating and regenerating the adsorbent; or,
and introducing a regeneration liquid into the regeneration reactor to flush or extract and regenerate the adsorbent.
Preferably, the method further comprises:
and discharging the regenerated gas or regenerated liquid after the regeneration treatment to a tail gas or residual liquid treatment device for treatment.
Preferably, when the regenerated adsorbent is returned to the liquid-solid fluidized bed for adsorption impurity removal, the method further comprises:
and supplementing fresh adsorbent into the liquid-solid fluidized bed.
Preferably, the adsorbent is one or more of molecular sieve, activated carbon, resin, aluminum oxide, silica gel, diatomite, montmorillonite, titanium dioxide and bismuth oxybromide.
Preferably, the liquid-solid fluidized bed is one of a low-speed upflow fluidized bed, a low-speed downflow fluidized bed, an upflow liquid-solid circulating fluidized bed, and a downflow liquid-solid circulating fluidized bed.
According to another aspect of the invention, a trichlorosilane adsorption impurity removal system is provided, which comprises a liquid-solid fluidized bed, a discharge pipeline, a regeneration reactor and a return pipeline, wherein:
the liquid-solid fluidized bed is connected with the trichlorosilane buffer tank, and an adsorbent is arranged in the liquid-solid fluidized bed and is used for introducing trichlorosilane liquid containing impurities and carrying out adsorption impurity removal on the trichlorosilane liquid;
the discharge pipeline is connected with the liquid-solid fluidized bed and the regeneration reactor and is used for discharging the adsorbent which adsorbs impurities to the regeneration reactor;
the regeneration reactor is used for regenerating the adsorbent after adsorbing the impurities;
the return pipeline is connected with the regeneration reactor and the liquid-solid fluidized bed and is used for returning the regenerated adsorbent to the liquid-solid fluidized bed for adsorption and impurity removal again.
Preferably, the system further comprises a regeneration auxiliary agent supply device, and the regeneration auxiliary agent supply device is connected with the regeneration reactor and is used for introducing a regeneration auxiliary agent into the regeneration reactor to carry out regeneration treatment on the adsorbent.
Preferably, the system further comprises a tail gas or residual liquid treatment device, wherein the tail gas or residual liquid treatment device is connected with the regeneration reactor and is used for treating the regeneration auxiliary agent after regeneration treatment.
Preferably, the system further comprises a sorbent make-up tank connected to the regeneration reactor for replenishing fresh sorbent.
Preferably, the system further comprises a liquid-solid separator, wherein the liquid-solid separator is connected with the liquid-solid fluidized bed and is used for separating the trichlorosilane liquid after adsorption and impurity removal and the adsorbent after impurity adsorption so as to discharge pure trichlorosilane liquid.
Preferably, the system further comprises a heat exchange device, wherein the heat exchange device is arranged on the return pipeline and is used for adjusting the temperature of the adsorbent and the temperature of the trichlorosilane liquid for conveying the adsorbent.
Preferably, the system further comprises a settling buffer tank provided on the return pipe for enabling continuous return of the adsorbent to the liquid-solid fluidized bed.
Preferably, the system further comprises a gas-liquid separator, and the gas-liquid separator is respectively connected with the trichlorosilane buffer tank, the liquid-solid fluidized bed and the regeneration reactor and is used for discharging gas in the system.
Preferably, the number of the regeneration reactors in the system is two, and the two regeneration reactors are arranged in parallel and sequentially run in turn.
Has the beneficial effects that:
the method and the system for adsorbing and removing impurities from trichlorosilane can optimize the trichlorosilane impurity removing process, realize continuous discharge, regeneration and feeding of saturated adsorbent and greatly improve the efficiency of adsorbing and removing impurities. Moreover, by arranging the settling buffer tank, the adsorbent can be continuously returned to the liquid-solid fluidized bed, so that the system can run more stably; through the arrangement of the gas-liquid separator, possible gas in the system can be discharged, and accumulation of the gas in the system is avoided; by arranging more than one set of regeneration reactors, a plurality of sets of regeneration reactors can alternately run the regeneration treatment process, the instability of the adsorption process caused by the separation between the regeneration reactors and the liquid-solid fluidized bed in the regeneration treatment process is prevented, the continuous discharge, regeneration and feeding of the system adsorbent are ensured, and the circulation is realized.
Drawings
FIG. 1 is a block diagram of a trichlorosilane adsorption impurity removal system in an embodiment of the present invention;
FIG. 2 is a schematic diagram of a first structure of a trichlorosilane adsorption impurity removal system according to an embodiment of the present disclosure;
FIG. 3 is a schematic structural diagram of a trichlorosilane adsorption impurity removal system in an embodiment of the present invention when two sets of regeneration reactors are adopted;
FIG. 4 is a schematic diagram of a second structure of a trichlorosilane adsorption impurity removal system according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of a third structure of a trichlorosilane adsorption impurity removal system in an embodiment of the present invention;
FIG. 6 is a schematic view of a structure of a liquid-solid fluidized bed in an example of the present invention;
FIG. 7 is a schematic diagram of a fourth structure of a trichlorosilane adsorption impurity removal system in an embodiment of the present invention;
fig. 8 is a schematic structural diagram of a fifth structure of a trichlorosilane adsorption impurity removal system in an embodiment of the present invention.
In the figure: 1. a trichlorosilane buffer tank; 2. a delivery pump; 3. liquid-solid fluidized bed 31-first riser adsorption reactor; 32. a first downcomer adsorption reactor; 33. a second riser adsorption reactor; 34. a second downcomer adsorption reactor; 4. a liquid-solid separator; 5. a regeneration aid supply device; 6. an adsorbent replenishment tank; 7. a regeneration reactor; 8. a tail gas or raffinate treatment unit; 9. a liquid inlet branch pipe; 10. evacuating the line; 11. a discharge line; 12. a return line; 121. a first tube section; 122. a second tube section; 13. a regeneration aid feed line; 14. a replenishing pipeline; 15. a tail gas or raffinate line; 16. a settling buffer tank; 17. a gas-liquid separator; 18-a second liquid inlet branch pipe; 19. a first exhaust line; 20. a second exhaust line; 21. and a third exhaust line.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "on" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience and simplicity of description, and do not indicate or imply that the indicated device or element must be provided with a specific orientation, configured and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected," "disposed," "mounted," "fixed," and the like are to be construed broadly, e.g., as being fixedly or removably connected, or integrally connected; either directly or indirectly through intervening media, or through the interconnection of two elements. The specific meaning of the above terms in the present invention can be understood in specific cases for those skilled in the art.
Example 1
As shown in fig. 1, this embodiment discloses a method for removing impurities by adsorption of trichlorosilane, which includes:
introducing the trichlorosilane liquid containing impurities into a liquid-solid fluidized bed 3 (also called a liquid-solid fluidized bed adsorption reactor), adding an adsorbent, adsorbing the impurities by the adsorbent, and removing impurities by adsorbing the trichlorosilane liquid;
discharging the adsorbent after adsorbing impurities from the liquid-solid fluidized bed 3 to a regeneration reactor 7 (also called an adsorbent regeneration reactor) for regeneration treatment;
and returning the regenerated adsorbent to the liquid-solid fluidized bed 3 for adsorption and impurity removal again.
Specifically, as shown in fig. 2, 4, 5, 7, and 8, the trichlorosilane liquid containing impurities is introduced from the inlet of the liquid-solid fluidized bed 3, and the impurities in the trichlorosilane liquid are adsorbed in the liquid-solid fluidized bed 3 by the adsorbent, so that the impurities are removed. Discharging the purified trichlorosilane liquid after impurity removal from an outlet of the liquid-solid fluidized bed 3. The discharge line 11 is connected to discharge a part of the adsorbent adsorbing impurities (e.g., adsorbent saturated with adsorption) into the regeneration reactor 7, and when the adsorbent in the regeneration reactor 7 reaches a certain capacity, the discharge line 11 is disconnected to regenerate the adsorbent in the regeneration reactor 7. The regeneration treatment specifically includes: introducing a regeneration auxiliary agent into the regeneration reactor 7, wherein the regeneration auxiliary agent can be regenerated gas or regenerated liquid, and specifically, the regeneration treatment can be that the regeneration gas is introduced into the regeneration reactor 7 to heat and regenerate the adsorbent; alternatively, the regeneration treatment may be to introduce a regeneration liquid into the regeneration reactor 7 to flush or extract the adsorbent for regeneration. After regeneration is completed, introduction of regeneration gas or regeneration liquid is stopped, regeneration gas tail gas or regeneration liquid residual liquid is discharged to a tail gas or residual liquid treatment device 8 through a tail gas or residual liquid pipeline 15 for subsequent treatment, then the tail gas or residual liquid pipeline 15 is disconnected, trichlorosilane liquid (preferably trichlorosilane liquid containing impurities and without impurity adsorption is adopted, hereinafter referred to as trichlorosilane liquid), a return pipeline 12 is connected, regenerated adsorbent is conveyed back to the liquid-solid fluidized bed 3 through the trichlorosilane liquid, and adsorption impurity removal and adsorbent regeneration circulation are achieved.
Compared with the prior art, the method has the advantages that the liquid-solid fluidized bed 3 is used for replacing a traditional fixed bed adsorption column to serve as an adsorption reactor, the trichlorosilane impurity removal process can be optimized, continuous discharge, regeneration and feeding of the saturated adsorbent are achieved, and the adsorption impurity removal efficiency is greatly improved.
In this embodiment, the regeneration gas is preferably hot nitrogen, and the regeneration liquid is preferably one or a mixture of more of sulfolane, tripropylamine, and hydrocarbon compounds.
In some embodiments, when returning the regenerated adsorbent to the liquid-solid fluidized bed 3 for adsorption impurity removal again, the method further includes: the liquid-solid fluidized bed 3 is replenished with fresh adsorbent.
Specifically, after the regeneration of the adsorbent is completed, the fresh adsorbent is replenished into the regeneration reactor 7 before the trichlorosilane liquid is introduced into the regeneration reactor 7, so that the fresh adsorbent is replenished into the liquid-solid fluidized bed. The amount of the supplementary adsorbent is specifically selected according to actual requirements, and this embodiment is not repeated.
In this embodiment, the adsorbent may be any one of a molecular sieve adsorbent, activated carbon, resin, aluminum oxide, silica gel, diatomaceous earth, montmorillonite, titanium dioxide, and bismuth oxybromide, and because different adsorbents have different adsorption capacities for different impurities, the adsorbents may also be blended according to different impurity concentrations and demands for the adsorbents, that is, the adsorbents may also be a combination of multiple kinds of the adsorbents, for example, a combination of resin and activated carbon. The specific amount or ratio of the adsorbent is specifically selected according to the actual conditions such as the kind and the adsorption capacity of the adsorbent, which is not described in detail in this embodiment.
In this embodiment, the liquid-solid fluidized bed 3 may be one of a low-speed upflow fluidized bed, a low-speed downflow fluidized bed, an upflow liquid-solid circulating fluidized bed, and a downflow liquid-solid circulating fluidized bed, depending on the difference in the density and adsorption capacity of the adsorbent. For example, when the density of the adsorbent (such as molecular sieve adsorbent) is greater than that of the trichlorosilane liquid, as shown in fig. 2, a low-speed upflow fluidized bed is preferably used; when the density of the adsorbent is less than that of the trichlorosilane liquid, as shown in fig. 5, a low-speed descending fluidized bed is preferably adopted; when the requirement on the adsorption stability is high and the density of the adsorbent is greater than that of the trichlorosilane liquid, as shown in fig. 7, an upflow liquid-solid circulating fluidized bed is preferably adopted; when the requirement of adsorption stability is high and the density of the adsorbent is less than that of the trichlorosilane liquid, a descending liquid-solid circulating fluidized bed is preferably adopted as shown in figure 8.
In some embodiments, considering that the operating temperature of the regeneration reactor 7 is different from the operating temperature of the liquid-solid fluidized bed, the method of this embodiment further comprises: and (3) carrying out heat exchange treatment on the regenerated adsorbent to adjust the temperature of the adsorbent and the trichlorosilane liquid for conveying the adsorbent to be as close to the operating temperature of the liquid-solid fluidized bed 3 as possible.
The method for adsorbing and removing the impurities from the trichlorosilane can optimize the trichlorosilane impurity removal process, realize continuous discharge, regeneration and feeding of the saturated adsorbent and greatly improve the efficiency of adsorption and impurity removal.
Example 2
As shown in fig. 1, the present embodiment discloses a system for removing impurities by trichlorosilane adsorption, which includes a liquid-solid fluidized bed 3, a discharge pipeline 11, a regeneration reactor 7, and a return pipeline 12, wherein:
the liquid-solid fluidized bed 3 is connected with the trichlorosilane buffer tank 1, the trichlorosilane buffer tank 1 is used for containing trichlorosilane liquid containing impurities, an adsorbent is arranged in the liquid-liquid solidification bed 3, and the liquid-solid fluidized bed 3 is used for introducing the trichlorosilane liquid containing the impurities discharged from the trichlorosilane buffer tank 1 and carrying out adsorption impurity removal on the trichlorosilane liquid by utilizing the adsorbent to obtain pure trichlorosilane liquid;
the discharge pipeline 11 is connected with the liquid-solid fluidized bed 3 and the regeneration reactor 7 and is used for discharging the adsorbent which adsorbs impurities to the regeneration reactor 7;
the regeneration reactor 7 is used for regenerating the adsorbent after adsorbing impurities;
the return pipeline 12 is connected with the regeneration reactor 7 and the liquid-solid fluidized bed 3 and is used for returning the regenerated adsorbent to the liquid-solid fluidized bed 3 for adsorption and impurity removal again.
Specifically, as shown in fig. 2, the liquid-solid fluidized bed 3 may be a low-speed upward-flow fluidized bed, and the adsorbent is an adsorbent having a density greater than that of the trichlorosilane liquid, for example, a molecular sieve adsorbent. The liquid-solid fluidized bed 3 is connected with the trichlorosilane buffer tank 1 through a liquid inlet pipeline, and a delivery pump 2 is arranged on the liquid inlet pipeline. And a discharge control valve is arranged on the discharge pipeline 11, and after adsorption is finished, the discharge control valve is opened to discharge the adsorbent adsorbing impurities to the regeneration reactor 7. The return line 12 is provided with a return control valve, and after the regeneration treatment is completed, the return control valve is opened to return the regenerated adsorbent to the liquid-solid fluidized bed 3. Through setting up discharge control valve, return control valve, can be when needing to carry out regeneration treatment process to the adsorbent, through closing discharge control valve and return control valve, make and cut off between regeneration reactor 7 and the liquid-solid fluidized bed 3 to the impurity that the regeneration process released causes the pollution to the adsorption process. An emptying pipeline 10 is arranged at the bottom of the regeneration reactor, an emptying control valve is arranged on the emptying pipeline 10, and the emptying pipeline 10 is used for discharging liquid (trichlorosilane liquid) in the regeneration reactor 7 before regeneration treatment.
In some embodiments, the number of the regeneration reactors (i.e., adsorbent regeneration reactors) in this embodiment is preferably one or more, for example, two, as shown in fig. 3, in consideration of the fact that the regeneration reactor 7 is isolated from the liquid-solid fluidized bed 3 during the regeneration process, which may cause instability of the adsorption process to some extent. The two sets of regeneration reactors 7 operate the regeneration treatment process in turn, when one set of regeneration reactor 7 operates the regeneration treatment process, the regeneration reactor 7 in the regeneration treatment process is separated from the liquid-solid fluidized bed 3, and simultaneously, the other set of regeneration reactor 7 is kept communicated with the liquid-solid fluidized bed 3 and continuously returns to the adsorbent after the regeneration treatment, so as to ensure that the liquid-solid fluidized bed continuously maintains a stable operation state.
In this embodiment, as shown in fig. 2, the regeneration reactor 7 is further connected to the trichlorosilane buffer tank 1, specifically, the regeneration reactor 7 is provided with a liquid inlet branch pipe 9, the liquid inlet branch pipe 9 is connected to a liquid inlet pipeline, the liquid inlet branch pipe 9 is provided with a branch pipe control valve, the branch pipe control valve is used for controlling the on/off of the liquid inlet branch pipe, the liquid inlet branch pipe 9 is used for introducing a trichlorosilane liquid containing impurities (hereinafter collectively referred to as a trichlorosilane liquid) into the regeneration reactor 7 after regeneration is completed, so as to transport the regenerated adsorbent back to the liquid-solid fluidized bed 3 by using the trichlorosilane liquid.
In some embodiments, as shown in fig. 2, the system of this embodiment further includes a regeneration aid supply device 5, and the regeneration aid supply device 5 is connected to the regeneration reactor 7 through a regeneration aid feeding line 13 for feeding a regeneration aid to the regeneration reactor to perform a regeneration treatment on the adsorbent.
Specifically, a regeneration aid feeding control valve is arranged on the regeneration aid feeding pipeline 13 to control the on-off of the regeneration aid feeding pipeline. The regeneration auxiliary agent may specifically be a regeneration gas, and in this case, the regeneration auxiliary agent supply device 5 is configured to introduce the regeneration gas into the regeneration reactor, so as to heat and regenerate the adsorbent by using the regeneration gas; the regeneration aid may also be a regeneration liquid, and in this case, the regeneration aid supply device 5 is used for introducing the regeneration liquid into the regeneration reactor 7 to flush or extract and regenerate the adsorbent by the regeneration liquid.
In some embodiments, as shown in fig. 2, the system of this embodiment further includes a tail gas or raffinate treatment device 8, the tail gas or raffinate treatment device 8 is connected to the regeneration reactor 7 through a tail gas or raffinate pipeline 15, and is configured to treat the regeneration assistant after the regeneration treatment, i.e., treat the regeneration gas after the regeneration treatment (i.e., tail gas of the regeneration gas) or the regeneration liquid after the regeneration treatment (i.e., raffinate of the regeneration liquid), and the tail gas or raffinate pipeline 15 is provided with a tail gas or raffinate control valve to control on/off of the tail gas or raffinate pipeline.
Specifically, the regeneration auxiliary feeding pipeline 13 may be arranged at the upper part of the regeneration reactor 7, and the tail gas or residual liquid pipeline 15 is arranged at the lower part of the regeneration reactor 7, i.e. the regeneration auxiliary enters from the upper end, and the regeneration tail gas or the regeneration liquid residual liquid is discharged from the lower end; the regeneration auxiliary agent feeding pipeline 13 can also be arranged at the lower part of the regeneration reactor, and the tail gas or residual liquid pipeline 15 is arranged at the upper part of the regeneration reactor, namely, the regeneration auxiliary agent enters from the lower end, and the regeneration tail gas or the regeneration liquid residual liquid is discharged from the upper end.
In some embodiments, as shown in fig. 2, the system of the present embodiment further includes an adsorbent replenishing tank 6, the adsorbent replenishing tank 6 is connected to the regeneration reactor 7 through a replenishing pipeline 14, more specifically, the adsorbent replenishing tank 6 is preferably connected to an upper portion of the regeneration reactor 7 through a replenishing pipeline, a replenishing control valve is disposed on the replenishing pipeline 14, the replenishing control valve is used for controlling on/off of the replenishing pipeline, the replenishing pipeline 14 is used for replenishing fresh adsorbent, and in addition, during a system start-up phase, the replenishing pipeline can be used for introducing adsorbent into the regeneration reactor 7 through the adsorbent replenishing tank 6 to add adsorbent into the liquid-solid fluidized bed 3.
In some embodiments, the system of this embodiment further includes a liquid-solid separator 4, where the liquid-solid separator 4 is connected to the liquid-solid fluidized bed 3, and is configured to separate the purified trichlorosilane liquid after impurity removal from the adsorbent (especially, adsorbent saturated in adsorption) after impurity adsorption, so as to discharge the purified trichlorosilane liquid obtained after impurity adsorption removal.
In this embodiment, the liquid-solid separator 4 may be a centrifugal liquid-solid separator using inertial separation, a settling tank separator using settling separation, or a ceramic filter element filter or a stainless steel filter element filter using filtering separation.
In some embodiments, the system of this embodiment further includes a heat exchange device (not shown in the drawings), which is disposed on the return line 12 and is used to adjust the temperature of the adsorbent and the trichlorosilane liquid for conveying the adsorbent to be as close as possible to the operating temperature of the liquid-solid fluidized bed 3.
The following details are given for example of the operation process of the trichlorosilane adsorption impurity removal system in this embodiment, and specifically are as follows:
closing the branch pipe control valve, the discharge control valve, the return control valve, the supplement control valve, the emptying control valve, the regeneration auxiliary agent feeding control valve and the tail gas or residual liquid control valve, starting the delivery pump 2, introducing the trichlorosilane liquid containing impurities from an inlet of the liquid-solid fluidized bed 3, adsorbing and removing impurities of the impurities in the trichlorosilane liquid in the liquid-solid fluidized bed 3 through a molecular sieve adsorbent in the liquid-solid fluidized bed 3, discharging the purified trichlorosilane liquid after removing the impurities from an outlet of the liquid-solid fluidized bed 3 to a liquid-solid separator 4, and discharging the purified trichlorosilane liquid out of the system after liquid-solid separation;
after the adsorption is stable, opening a branch pipe control valve, connecting a liquid inlet branch pipe 9, simultaneously, opening a discharge control valve, connecting a discharge pipeline 11, discharging a part of adsorbent (such as adsorbent saturated in adsorption) adsorbing impurities into a regeneration reactor 7 along with trichlorosilane liquid, opening a branch pipe control valve and a return control valve so as to discharge the adsorbent from a liquid-solid fluidized bed 3 to the regeneration reactor 7, closing the discharge control valve, the branch pipe control valve and the return control valve when the adsorbent in the regeneration reactor 7 reaches a certain capacity, opening an emptying control valve to discharge the trichlorosilane liquid, opening a regeneration auxiliary agent feeding control valve and a tail gas or residual liquid control valve after the trichlorosilane liquid is discharged, introducing hot nitrogen (i.e. regeneration gas) or sulfolane (i.e. regeneration liquid) into the regeneration reactor 7, carrying out regeneration treatment on the adsorbent in the regeneration reactor 7, and discharging the tail gas or residual liquid of the regeneration gas or residual liquid into a tail gas or residual liquid treatment device 8 through a tail gas or regeneration pipeline 15 to carry out subsequent treatment;
after the regeneration is completed, for example, when the regeneration reactor is operated for a certain period of time (e.g. 2 hours) or the concentration of impurities in the regeneration gas tail gas or the regeneration liquid residual liquid discharged from the regeneration reactor 7 is lower than a certain value (e.g. the total carbon content of impurities is less than or equal to 0.1 μ g/g, and/or the boron content of impurities is less than or equal to 1ng/g, and/or the phosphorus content of impurities is less than or equal to 2ng/g, and/or the total metal content is less than or equal to 30 ng/g), the regeneration auxiliary agent feeding control valve is closed, the introduction of the regeneration gas or the regeneration liquid is stopped, and after the regeneration gas tail gas or the regeneration liquid residual liquid is discharged, the tail gas or residual liquid control valve is closed, and the tail gas or residual liquid pipeline 15 is disconnected;
and then, opening a branch pipe control valve, introducing trichlorosilane liquid into the regeneration reactor 7, opening a return control valve after the regeneration reactor 7 is full, communicating a return pipeline 12, and conveying the regenerated adsorbent back to the liquid-solid fluidized bed 3 by using the trichlorosilane liquid, thereby realizing adsorption impurity removal and adsorbent regeneration circulation.
The system for adsorbing and removing impurities from trichlorosilane can optimize the trichlorosilane impurity removal process, realize continuous discharge, regeneration and feeding of saturated adsorbent, and greatly improve the adsorption and impurity removal efficiency.
Example 3
The embodiment discloses a trichlorosilane adsorption impurity removal system, which is different from the system of embodiment 2 in that:
as shown in fig. 4, the system of this embodiment further includes a settling buffer tank 16, and the settling buffer tank 16 is disposed on the return line 12, and is used for enabling the adsorbent to continuously return to the liquid-solid fluidized bed, so that the system operates more stably.
Specifically, the return line includes a first pipe section 121 and a second pipe section 122, the inlet of the settling buffer tank 16 is connected to the regeneration reactor 7 through the first pipe section 121, and the outlet of the settling buffer tank 16 is connected to the liquid-solid fluidized bed 3 through the second pipe section 122. The regenerated adsorbent is introduced into the settling buffer tank 16, and then continuously introduced into the liquid-solid fluidized bed 3 through the settling buffer tank 16.
Example 4
The embodiment discloses a trichlorosilane adsorption impurity removal system, which is different from the system of embodiment 2 in that:
as shown in fig. 5, the liquid-solid fluidized bed 3 of the system of this embodiment adopts a low-speed downflow fluidized bed, at this time, an inlet of the liquid-solid fluidized bed 3 is disposed at the upper portion of the liquid-solid fluidized bed 3, the trichlorosilane buffer tank 1 is connected with the upper portion of the liquid-solid fluidized bed 3 through a liquid inlet pipeline, an outlet of the liquid-solid fluidized bed 3 is disposed at the lower portion or the bottom of the liquid-solid fluidized bed, that is, trichlorosilane liquid containing impurities is introduced from the upper portion of the liquid-solid fluidized bed, and purified trichlorosilane after the impurities are discharged from the lower portion or the bottom of the liquid-solid fluidized bed 3. The adsorbent is an adsorbent with density less than that of the trichlorosilane liquid, for example, an activated carbon adsorbent or a resin adsorbent is used.
In some embodiments, the system of the present embodiment further includes a gas-liquid separator 17, and the gas-liquid separator 17 is connected to the trichlorosilane buffer tank 1, the liquid-solid fluidized bed 3, and the regeneration reactor 7, respectively, and is used for discharging gas that may exist in the system.
Specifically, the height of the gas-liquid separator 17 should be higher than the heights of the liquid-solid fluidized bed 3 and the regeneration reactor 7. The liquid inlet pipeline is provided with a first exhaust pipeline 19, the trichlorosilane buffer tank 1 is connected with the gas-liquid separator 17 through the first exhaust pipeline 19 on the liquid inlet pipeline, the top of the liquid-solid fluidized bed 3 is connected with the gas-liquid separator 17 through a second exhaust pipeline 20, and the lower part or the bottom (outlet) of the liquid-solid fluidized bed 3 is connected with the bottom of the gas-liquid separator 17 through a third exhaust pipeline 21.
By providing the first exhaust line 19, the second exhaust line 20, and the third exhaust line 21, it is possible to exhaust gas that may be present in the system (particularly, the liquid-solid fluidized bed 3), and to avoid accumulation of gas in the system.
Example 5
The embodiment discloses a system for adsorbing and removing impurities from trichlorosilane, which is different from the system for adsorbing and removing impurities from trichlorosilane described in any one of embodiments 2 to 4 in that:
as shown in fig. 6, the liquid-solid fluidized bed 3 of the system of the present embodiment may be a single-stage liquid-solid fluidized bed (i.e., (a)), or may be a two-stage or higher-stage liquid-solid fluidized bed, for example, a three-stage liquid-solid fluidized bed (i.e., (b)).
Example 6
The embodiment discloses a trichlorosilane adsorption impurity removal system, which is different from the system of embodiment 2 in that:
as shown in FIG. 7, the liquid-solid fluidized bed 3 of the system of this embodiment employs an upflow liquid-solid circulating fluidized bed which includes a first upflow adsorption reactor 31 and a first downflow adsorption reactor 32. The trichlorosilane buffer tank 1 is connected with the bottom of the first ascending pipe adsorption reactor 31 through a liquid inlet pipeline, namely trichlorosilane liquid containing impurities is introduced from the bottom of the first ascending pipe adsorption reactor 31. The liquid-solid separator 4 is connected with the top of the first ascending pipe adsorption reactor 31, and the purified trichlorosilane liquid after impurity removal is discharged after being separated by the liquid-solid separator 4. The upper part of the first downcomer adsorption reactor 32 is connected to the liquid-solid separator, and the adsorbent separated by the liquid-solid separator 4 is discharged to the first downcomer adsorption reactor 32. The lower part or the bottom of the first downcomer adsorption reactor 32 is connected to the lower part or the bottom of the first riser adsorption reactor 31, and is used to return the adsorbent discharged to the first downcomer adsorption reactor 32 to the riser adsorption reactor 31, and the adsorbent circulates through the first riser adsorption reactor 31 and the first downcomer adsorption reactor 32, and is adsorbed together to realize a cycle.
The first downcomer adsorption reactor 31 (preferably the lower or bottom) is also connected to the upper or top part of the regeneration reactor 7 via a discharge line 11, a return line 12, respectively. The discharge line 11 and the return line 12 in this embodiment may be combined, that is, the same line is used for the discharge line and the return line (as shown in fig. 7), which may simplify the system structure to some extent.
In some embodiments, a second liquid inlet branch pipe 18 is further disposed at the lower part or bottom of the first downcomer adsorption reactor 32, and the second liquid inlet branch pipe 18 is connected to the liquid inlet pipeline, that is, trichlorosilane liquid containing impurities can be introduced from the bottom or lower part of the first downcomer adsorption reactor 32.
Compared with the system of the embodiment 2, the downcomer adsorption reactor 32 of the system of the embodiment stores a large amount of adsorbent, the adsorption state is not affected by the discharge and return processes of the adsorbent in the regeneration reactor 7, and the adsorption state is more stable.
Example 7
The embodiment discloses a trichlorosilane adsorption impurity removal system, which is different from the system in embodiment 6 in that:
as shown in FIG. 8, the liquid-solid fluidized bed 3 of the system of this embodiment employs a downflow liquid-solid circulating fluidized bed which includes a second riser adsorption reactor 33 and a second downcomer adsorption reactor 34. The trichlorosilane buffer tank 1 is connected with the top of the second downcomer adsorption reactor 34 through a liquid inlet pipeline, namely trichlorosilane liquid containing impurities is introduced from the top of the second downcomer adsorption reactor 34. The liquid-solid separator 4 is connected with the bottom of the second downcomer adsorption reactor 34, and the purified trichlorosilane liquid after impurity removal is discharged after being separated by the liquid-solid separator 4. The lower part or the bottom of the second rising pipe adsorption reactor 33 is connected with the liquid-solid separator 4, and the adsorbent separated by the liquid-solid separator 4 is discharged to the second rising pipe adsorption reactor 33. The upper part or the top of the second rising pipe adsorption reactor 33 is connected to the upper part or the top of the second downcomer adsorption reactor 34, and is used for returning the adsorbent discharged to the second rising pipe adsorption reactor 33 to the second downcomer adsorption reactor 34, and the adsorbent circulates through the second downcomer adsorption reactor 34 and the second rising pipe adsorption reactor 33, and is adsorbed together to realize circulation.
And the upper part or the top of the second ascending pipe adsorption reactor 33 is also connected with a liquid inlet pipeline through a second liquid inlet branch pipe 18, that is, trichlorosilane liquid containing impurities can be introduced from the upper part or the top of the second ascending pipe adsorption reactor 33.
In addition, the system of the embodiment further comprises a gas-liquid separator 17, and the gas-liquid separator 17 is connected with the trichlorosilane buffer tank 1, the second downcomer adsorption reactor 34 and the second riser adsorption reactor 33 in the liquid-solid fluidized bed 3, and the regeneration reactor 7 respectively, and is used for discharging gas possibly existing in the system before the regeneration treatment is carried out.
Specifically, the height of the gas-liquid separator 4 should be higher than the height of the second downcomer adsorption reactor 34 and the regeneration reactor 7 in the liquid-solid fluidized bed. The trichlorosilane buffer tank 1 is connected with the gas-liquid separator 17 through a first exhaust pipeline 19 on a liquid inlet pipeline, the top of a second downcomer adsorption reactor 34 is connected with the gas-liquid separator 17 through a second exhaust pipeline 20, and the lower parts or the bottoms (outlets) of the second downcomer adsorption reactor 34, the second riser adsorption reactor 33 and the regeneration reactor 7 are connected with the bottom of the gas-liquid separator 17 through a third exhaust pipeline 21.
By providing the first exhaust line 19, the second exhaust line 20, and the third exhaust line 21, it is possible to exhaust gases that may be present in the system (particularly, the second downcomer adsorption reactor 33 and the second downcomer adsorption reactor 34), and it is possible to avoid the stability of the system operation from being affected by accumulation of gases in the system.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (15)
1. A method for adsorbing and removing impurities from trichlorosilane comprises the following steps:
introducing trichlorosilane liquid containing impurities into a liquid-solid fluidized bed, adding an adsorbent, and carrying out adsorption impurity removal on the trichlorosilane liquid;
discharging the adsorbent after adsorbing the impurities to a regeneration reactor for regeneration treatment;
and returning the regenerated adsorbent to the liquid-solid fluidized bed for adsorption and impurity removal again.
2. The trichlorosilane adsorption impurity removal method according to claim 1, wherein the regeneration treatment specifically comprises:
introducing regeneration gas into the regeneration reactor, and heating and regenerating the adsorbent; or,
and introducing a regeneration liquid into the regeneration reactor to flush or extract and regenerate the adsorbent.
3. The trichlorosilane adsorption impurity removal method according to claim 2, further comprising:
and discharging the regenerated gas or regenerated liquid after the regeneration treatment to a tail gas or residual liquid treatment device for treatment.
4. The method for removing impurities by adsorption from trichlorosilane as claimed in claim 1, wherein when the regenerated adsorbent is returned to the liquid-solid fluidized bed for removing impurities by adsorption, the method further comprises:
and supplementing fresh adsorbent into the liquid-solid fluidized bed.
5. The trichlorosilane adsorption impurity removal method according to any one of claims 1 to 4, wherein the adsorbent is one or more of molecular sieve, activated carbon, resin, aluminum oxide, silica gel, diatomite, montmorillonite, titanium dioxide and bismuth oxybromide.
6. The trichlorosilane adsorption impurity removal method according to any one of claims 1 to 4, wherein the liquid-solid fluidized bed is one of a low-speed upflow fluidized bed, a low-speed downflow fluidized bed, an upflow liquid-solid circulating fluidized bed and a downflow liquid-solid circulating fluidized bed.
7. A trichlorosilane adsorption impurity removal system is characterized by comprising a liquid-solid fluidized bed (3), a discharge pipeline (11), a regeneration reactor (7) and a return pipeline (12),
the liquid-solid fluidized bed is connected with the trichlorosilane buffer tank, and an adsorbent is arranged in the liquid-solid fluidized bed and is used for introducing trichlorosilane liquid containing impurities and carrying out adsorption impurity removal on the trichlorosilane liquid;
the discharge pipeline is connected with the liquid-solid fluidized bed and the regeneration reactor and is used for discharging the adsorbent which adsorbs impurities to the regeneration reactor;
the regeneration reactor is used for regenerating the adsorbent after adsorbing the impurities;
the return pipeline is connected with the regeneration reactor and the liquid-solid fluidized bed and is used for returning the regenerated adsorbent to the liquid-solid fluidized bed for adsorption and impurity removal again.
8. The trichlorosilane adsorption impurity removal system according to claim 7, further comprising a regeneration auxiliary agent supply device (5),
the regeneration auxiliary agent supply device is connected with the regeneration reactor and is used for introducing a regeneration auxiliary agent into the regeneration reactor to carry out regeneration treatment on the adsorbent.
9. The trichlorosilane adsorption impurity removal system according to claim 8, further comprising a tail gas or raffinate treatment device (8),
and the tail gas or residual liquid treatment device is connected with the regeneration reactor and is used for treating the regeneration auxiliary agent after regeneration treatment.
10. The trichlorosilane adsorption impurity removal system according to claim 9, further comprising an adsorbent replenishment tank (6),
and the adsorbent replenishing tank is connected with the regeneration reactor and is used for replenishing fresh adsorbent.
11. The trichlorosilane adsorption impurity removal system according to claim 10, further comprising a liquid-solid separator (4),
the liquid-solid separator is connected with the liquid-solid fluidized bed and is used for separating the trichlorosilane liquid after adsorption and impurity removal and the adsorbent after impurity adsorption so as to discharge pure trichlorosilane liquid.
12. The trichlorosilane adsorption impurity removal system according to claim 11, further comprising a heat exchange device,
the heat exchange device is arranged on the return pipeline and used for adjusting the temperature of the adsorbent and the trichlorosilane liquid for conveying the adsorbent.
13. The trichlorosilane adsorption impurity removal system according to any one of claims 7 to 12, further comprising a settling buffer tank (16),
the settling buffer tank is arranged on the return pipe and is used for enabling the adsorbent to continuously return to the liquid-solid fluidized bed.
14. The trichlorosilane adsorption impurity removal system according to any one of claims 7 to 12, further comprising a gas-liquid separator (17),
the gas-liquid separator is respectively connected with the trichlorosilane buffer tank, the liquid-solid fluidized bed and the regeneration reactor and is used for discharging gas in the system.
15. The trichlorosilane adsorption impurity removal system according to claims 7 to 12, wherein the number of the regeneration reactors (7) is two, and the two regeneration reactors are arranged in parallel and sequentially run in turn.
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| CN116328746A (en) * | 2023-04-10 | 2023-06-27 | 新特能源股份有限公司 | Terpyridine-silica gel composite material and preparation method thereof |
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