CN111453736A - Trichlorosilane purification system and method - Google Patents
Trichlorosilane purification system and method Download PDFInfo
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- CN111453736A CN111453736A CN202010344097.3A CN202010344097A CN111453736A CN 111453736 A CN111453736 A CN 111453736A CN 202010344097 A CN202010344097 A CN 202010344097A CN 111453736 A CN111453736 A CN 111453736A
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- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 147
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000000746 purification Methods 0.000 title claims abstract description 40
- 239000000654 additive Substances 0.000 claims abstract description 73
- 230000000996 additive effect Effects 0.000 claims abstract description 72
- 239000000463 material Substances 0.000 claims abstract description 50
- 239000000126 substance Substances 0.000 claims abstract description 36
- 239000012043 crude product Substances 0.000 claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000011777 magnesium Substances 0.000 claims description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 11
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 35
- 229910052799 carbon Inorganic materials 0.000 abstract description 35
- 239000012535 impurity Substances 0.000 abstract description 34
- 239000000047 product Substances 0.000 abstract description 14
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 20
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 16
- 238000009835 boiling Methods 0.000 description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene chloride Substances ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 14
- 229910001629 magnesium chloride Inorganic materials 0.000 description 12
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 11
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- CCERQOYLJJULMD-UHFFFAOYSA-M magnesium;carbanide;chloride Chemical compound [CH3-].[Mg+2].[Cl-] CCERQOYLJJULMD-UHFFFAOYSA-M 0.000 description 8
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 8
- 238000004821 distillation Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920005591 polysilicon Polymers 0.000 description 5
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 2
- 239000005048 methyldichlorosilane Substances 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000066 reactive distillation Methods 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4211—Regulation; Control of columns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4211—Regulation; Control of columns
- B01D3/4216—Head stream
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a trichlorosilane purification system and a method. Wherein, trichlorosilane clean system includes: an additive pretreatment device having a simple metal substance inlet, an organic solvent inlet, and an additive outlet; the trichlorosilane pretreatment device is provided with a trichlorosilane crude product inlet, an additive inlet and a mixed material outlet, and the additive inlet is connected with the additive outlet; the rectifying device is provided with a material inlet and a refined trichlorosilane outlet, and the material inlet is connected with the mixed material outlet. According to the trichlorosilane purification system, the additive pretreatment device, the trichlorosilane pretreatment device and the rectification device are adopted, so that carbon-containing impurities in trichlorosilane can be effectively removed, and a high-purity trichlorosilane product is obtained.
Description
Technical Field
The invention relates to the technical field of polysilicon production, in particular to a trichlorosilane purification system and a trichlorosilane purification method.
Background
The electronic grade polysilicon is an initial raw material of an integrated circuit industrial chain, can be used for manufacturing various semiconductor silicon devices after being drawn into single crystal, wherein the carbon content is used as a basic performance index of the electronic grade polysilicon, and directly influences the performance of various subsequent products. When the carbon content is too high, a large number of defects exist in the monocrystalline silicon piece, and after the monocrystalline silicon piece is prepared into elements such as chips and transistors, a series of problems such as electric leakage and the like are caused, so that the product is scrapped.
At present, polysilicon is mostly produced by adopting an improved Siemens method, Trichlorosilane (TSC) is purified by a multistage rectification system, and then the TSC is introduced into a CVD reactor to produce polysilicon rods. The trichlorosilane source is generally a cold hydrogenation device or a trichlorosilane synthesis device, and a fixed bed or a fluidized bed is used for producing the silicon powder serving as a raw material. However, under such production conditions, CH is inevitably produced3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And organic impurities containing methyl and methylene. Wherein, CH3SiHCl2Boiling point of 41.5 ℃, (CH)3)2SiCl2Boiling point of 35.5 ℃ and CH2Cl2The boiling point is 39.7 ℃, the boiling point is close to that of TCS, the relative volatility is only 1.1-1.5, the trichlorosilane is difficult to completely remove by a rectification process, and the rectified trichlorosilane often contains more than 1ppmw of the organic impurities, so that the production requirement of electronic grade polycrystalline silicon cannot be met.
Patent CN201811311004.6 discloses a device and a method for preparing high-purity trichlorosilane by adsorbing and removing methylchlorosilane impurities, wherein a directional adsorbent is used for removing methylchlorosilane. Patent CN201811381032.5 discloses a device and a method for removing methyldichlorosilane in trichlorosilane by reactive distillation, wherein methylchlorosilane is removed by reactive distillation. Patent CN201811139932.9 discloses a method for purifying trichlorosilane by disproportionation reaction of silicon tetrachloride and methyldichlorosilane to produce methyltrichlorosilane.
However, the lower removal limit of the above method is still high, or an increased production apparatus is required and the cost is high. The existing method for purifying trichlorosilane still needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a trichlorosilane purification system and a trichlorosilane purification method. The trichlorosilane purification system can effectively remove carbon-containing impurities in the trichlorosilane by adopting the additive pretreatment device, the trichlorosilane pretreatment device and the rectification device, so that a high-purity trichlorosilane product is obtained.
In one aspect of the invention, the invention provides a trichlorosilane purification system. According to the embodiment of the invention, the trichlorosilane purification system comprises: an additive pretreatment device having a simple metal substance inlet, an organic solvent inlet, and an additive outlet; the trichlorosilane pretreatment device is provided with a trichlorosilane crude product inlet, an additive inlet and a mixed material outlet, and the additive inlet is connected with the additive outlet; the rectifying device is provided with a material inlet and a refined trichlorosilane outlet, and the material inlet is connected with the mixed material outlet.
According to the trichlorosilane purification system disclosed by the embodiment of the invention, the additive pretreatment device can prepare the additive which is suitable for reacting with carbon-containing impurities in trichlorosilane by using a metal simple substance and an organic solvent; further, the trichlorosilane crude product to be purified and the additive are supplied to a trichlorosilane pretreatment device for reaction, and the metal simple substance in the additive can react with CH in trichlorosilane3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And the carbon-containing impurities react to convert the carbon-containing impurities into substances with relatively high boiling points, so that the substances can be removed from the trichlorosilane by using a rectifying device in the following step. Therefore, the trichlorosilane purification system can effectively remove carbon-containing impurities in trichlorosilane and obtain a high-purity trichlorosilane product by adopting the additive pretreatment device, the trichlorosilane pretreatment device and the rectification device, and compared with the traditional process, the trichlorosilane purification system disclosed by the invention has the advantages that the trichlorosilane product is obtainedThe device investment cost of the hydrogen silicon purification system is lower, and the carbon content of the product is lower.
In addition, the trichlorosilane purification system according to the embodiment of the invention may further have the following additional technical features:
in some embodiments of the invention, the rectification apparatus comprises: the first rectifying tower is provided with a mixed material inlet, a first tower top fraction outlet and a first tower bottom fraction outlet, and the mixed material inlet is connected with the mixed material outlet; a second rectification column having a first overheads fraction inlet, a second overheads fraction outlet, and a second kettle fraction outlet, the first overheads fraction inlet coupled to the first overheads fraction outlet; and the third rectifying tower is provided with a second tower kettle fraction inlet, a third tower top fraction outlet and a third tower kettle fraction outlet, and the second tower kettle fraction inlet is connected with the second tower kettle fraction outlet.
In another aspect of the invention, the invention provides a method for purifying trichlorosilane. According to the embodiment of the invention, the trichlorosilane purification method is implemented by the trichlorosilane purification system of the embodiment, and the trichlorosilane purification method comprises the following steps: (1) supplying the metal simple substance and the organic solvent into an additive pretreatment device for mixing to obtain an additive; (2) feeding the trichlorosilane crude product and the additive into a trichlorosilane pretreatment device for reaction to obtain a mixed material; (3) and feeding the mixed material to a rectifying device for rectifying treatment to obtain the refined trichlorosilane.
According to the method for purifying trichlorosilane, disclosed by the embodiment of the invention, firstly, an additive suitable for reacting with carbon-containing impurities in trichlorosilane is prepared by utilizing a metal simple substance and an organic solvent; further, the trichlorosilane crude product to be purified and the additive are supplied to a trichlorosilane pretreatment device for reaction, and the metal simple substance in the additive can react with CH in trichlorosilane3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2The carbon-containing impurities react to convert into boiling waterThe substances with relatively high points are used for removing the substances from the trichlorosilane by using a rectifying device in the following process. Therefore, the method for purifying trichlorosilane can effectively remove carbon-containing impurities in trichlorosilane to obtain a high-purity trichlorosilane product, and compared with the traditional process, the method for purifying trichlorosilane has the advantages of lower investment cost of a device and lower carbon content of the product.
In addition, the method for purifying trichlorosilane according to the embodiment of the invention may further have the following additional technical features:
in some embodiments of the present invention, the elemental metal is selected from at least one of sodium, potassium, and magnesium.
In some embodiments of the invention, the organic solvent is selected from at least one of tetrahydrofuran, 2-methyltetrahydrofuran.
In some embodiments of the invention, in the additive, the mass fraction of the metal simple substance is 1-3%.
In some embodiments of the invention, in the step (2), the flow rate of the additive is 0.005-0.015% of the flow rate of the trichlorosilane crude product.
In some embodiments of the invention, step (3) further comprises: (3-1) feeding the mixed material into a first rectifying tower for first rectifying treatment to obtain a first tower top fraction and a first tower bottom fraction; (3-2) supplying the first overhead fraction to a second rectifying tower for second rectifying treatment to obtain a second overhead fraction and a second tower bottom fraction; and (3-3) supplying the second tower bottom fraction to a third rectifying tower for third rectifying treatment to obtain a third tower top fraction (refined trichlorosilane) and a third tower bottom fraction.
In some embodiments of the invention, in the first rectification treatment, the operation pressure at the top of the tower is 0.2-0.5 MPaG, the operation temperature at the top of the tower is 70-96 ℃, the operation pressure at the bottom of the tower is 0.22-0.52 MPaG, the operation temperature at the bottom of the tower is 72-98 ℃, and the reflux ratio is 10-20.
In some embodiments of the invention, in the second rectification treatment, the operation pressure at the top of the tower is 0.25-0.55 MPaG, the operation temperature at the top of the tower is 74-98 ℃, the operation pressure at the bottom of the tower is 0.27-0.57 MPaG, the operation temperature at the bottom of the tower is 76.8-100.8 ℃, and the reflux ratio is 8-15.
In some embodiments of the present invention, in the third distillation treatment, the operation pressure at the top of the column is 0.3 to 0.6MPaG, the operation temperature at the top of the column is 79.2 to 103.2 ℃, the operation pressure at the bottom of the column is 0.32 to 0.63MPaG, and the operation temperature at the bottom of the column is 81.6 to 105.6 ℃.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic structural diagram of a trichlorosilane purification system according to one embodiment of the invention;
FIG. 2 is a schematic structural diagram of a trichlorosilane purification system according to yet another embodiment of the invention;
FIG. 3 is a schematic flow diagram of a trichlorosilane purification method according to one embodiment of the invention;
fig. 4 is a schematic flow chart of a trichlorosilane purification method according to still another embodiment of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Furthermore, the terms "first", "second", "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," or "third" may explicitly or implicitly include at least one of the feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In one aspect of the invention, the invention provides a trichlorosilane purification system. Referring to fig. 1, according to an embodiment of the present invention, the trichlorosilane purification system includes: additive pretreatment device 100, trichlorosilane pretreatment device 200 and rectification device 300. The additive pretreatment device 100 is provided with a simple metal substance inlet 101, an organic solvent inlet 102 and an additive outlet 103; the trichlorosilane pretreatment device 200 is provided with a trichlorosilane crude product inlet 201, an additive inlet 202 and a mixed material outlet 203, wherein the additive inlet 202 is connected with the additive outlet 103; the rectifying device 300 is provided with a material inlet 301 and a refined trichlorosilane outlet 302, wherein the material inlet 301 is connected with the mixed material outlet 203.
The trichlorosilane purification system according to an embodiment of the invention is further described in detail with reference to fig. 1 and 2.
According to the embodiment of the present invention, the additive pretreatment device 100 has an elemental metal inlet 101, an organic solvent inlet 102, and an additive outlet 103. The additive pretreatment device 100 is suitable for mixing a metal simple substance and an organic solvent to obtain an additive.
According to embodiments of the present inventionThe metal element may be at least one selected from sodium, potassium and magnesium, and preferably magnesium. The metal simple substance can react with CH in the trichlorosilane crude product3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And the carbon-containing impurities react to convert the carbon-containing impurities into substances with relatively high boiling points, so that the substances can be removed from the trichlorosilane by using a rectifying device in the following step.
According to some embodiments of the present invention, the organic solvent may be at least one selected from tetrahydrofuran and 2-methyltetrahydrofuran, and preferably 2-methyltetrahydrofuran. Therefore, CH in the metal simple substance and the trichlorosilane crude product can be further improved3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And the reaction efficiency of the carbon-containing impurities is equal, so that the removal rate of the carbon-containing impurities is further improved. The boiling point of 2-methyltetrahydrofuran is higher relative to tetrahydrofuran and is easier to remove by subsequent rectification.
According to some embodiments of the present invention, in the above additive, the mass fraction of the metal element may be 1 to 3%, for example, 1%, 1.5%, 2%, 2.5%, 3%. Therefore, the removal rate of carbon-containing impurities in the trichlorosilane can be further improved.
According to the embodiment of the invention, the trichlorosilane pretreatment device 200 is provided with a trichlorosilane crude product inlet 201, an additive inlet 202 and a mixed material outlet 203, wherein the additive inlet 202 is connected with the additive outlet 103. The trichlorosilane pretreatment device 200 is suitable for mixing and reacting trichlorosilane crude products and additives to obtain mixed materials.
According to the embodiment of the invention, the metal simple substance in the additive can be mixed with CH in the trichlorosilane crude product3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2When the carbon-containing impurities react, the carbon-containing impurities are converted into substances with relatively high boiling points, so that the substances can be separated from the trichlorosilane by using a rectifying device in the following stepAnd (4) removing. Taking an additive adopting metal Mg as an example, the reaction of the trichlorosilane crude product with the additive comprises the following steps:
Mg+CH3Cl→CH3MgCl；
Mg+CH2Cl2→CH2MgCl2；
CH3SiHCl2+CH3MgCl→(CH3)2SiHCl+MgCl2；
CH3MgCl+(CH3)2SiHCl→(CH3)3SiH+MgCl2；
CH3MgCl+(CH3)2SiCl2→(CH3)3SiCl+MgCl2；
CH2MgCl2+(CH3)2SiHCl→(CH3)3SiCl+MgCl2。
according to the embodiment of the invention, in the above step, the flow rate of the additive may be 0.005-0.015% of the flow rate of the trichlorosilane crude product, and is preferably 0.01%. Therefore, the stable reaction between the additive and the trichlorosilane crude product can be further ensured, and the removal rate of carbon-containing impurities in the trichlorosilane can be further improved.
According to the embodiment of the invention, the rectifying device 300 is provided with a material inlet 301 and a refined trichlorosilane outlet 302, wherein the material inlet 301 is connected with the mixed material outlet 203. The rectifying device 300 is suitable for rectifying the mixed material obtained by the reaction of the trichlorosilane crude product and the additive to obtain the refined trichlorosilane. After the trichlorosilane reacts with the additive, most of the carbon-containing impurities are converted into substances with relatively high boiling points, and the substances can be removed from the trichlorosilane through rectification treatment. The content of carbon-containing impurities in the refined trichlorosilane obtained by rectification is less than 20 ppbw.
Referring to fig. 2, according to an embodiment of the present invention, a rectification apparatus 300 includes: a first rectifying column 310, a second rectifying column 320, and a second rectifying column 330.
According to an embodiment of the present invention, the first rectification column 310 has a mixed material inlet 311, a first overhead fraction outlet 312 and a first kettle fraction outlet 313, the mixed material inlet 311 being connected to the mixed material outlet 203; the second rectification column 320 has a first overheads fraction inlet 321, a second overheads fraction outlet 322, and a second bottoms fraction outlet 323, the first overheads fraction inlet 321 connected to the first overheads fraction outlet 312; the third rectification column 330 has a second bottom fraction inlet 331, a third overhead fraction outlet 332 and a third bottom fraction outlet 333, the second bottom fraction inlet 331 being connected to the second bottom fraction outlet 323. Therefore, the mixed material obtained by the reaction of the trichlorosilane crude product and the additive is subjected to three-stage rectification treatment through the first to third rectification towers, so that the removal rate of carbon-containing impurities in the trichlorosilane crude product can be further improved
According to an embodiment of the present invention, the operating parameters in the first rectification column include: the operation pressure at the top of the column is 0.2 to 0.5MPaG (e.g., 0.2MPaG, 0.3MPaG, 0.4MPaG, 0.5MPaG, etc.), the operation temperature at the top of the column is 70 to 96 ℃ (e.g., 70 ℃, 74 ℃, 76 ℃, 80 ℃, 88 ℃, 94 ℃, 96 ℃, etc.), the operation pressure at the bottom of the column is 0.22 to 0.52MPaG (e.g., 0.22MPaG, 0.32MPaG, 0.42MPaG, 0.52MPaG, etc.), the operation temperature at the bottom of the column is 72 to 98 ℃ (e.g., 72 ℃, 74 ℃, 76 ℃, 80 ℃, 82 ℃, 88 ℃, 90 ℃, 94 ℃, 98 ℃, etc.), and the reflux ratio is 10 to 20. Preferably, the operation pressure at the top of the tower is 0.3-0.4 MPaG, the operation temperature at the top of the tower is 80-88 ℃, the operation pressure at the bottom of the tower is 0.32-0.42 MPaG, and the operation temperature at the bottom of the tower is 82-90 ℃. Under the above operation parameters, the cut-off amount of the heavy components in the materials is 3-10% of the feeding amount, and the heavy components separated from the tower bottom can be transferred to other processes for use.
According to an embodiment of the present invention, the operating parameters in the second rectification column include: the operation pressure at the top of the column is 0.25 to 0.55MPaG (e.g., 0.25MPaG, 0.35MPaG, 0.45MPaG, 0.55MPaG, etc.), the operation temperature at the top of the column is 74 to 98 ℃ (e.g., 74 ℃, 76 ℃, 80 ℃, 82 ℃, 88 ℃, 90 ℃, 94 ℃, 98 ℃, etc.), the operation pressure at the bottom of the column is 0.27 to 0.57MPaG (e.g., 0.27MPaG, 0.37MPaG, 0.47MPaG, 0.57MPaG, etc.), the operation temperature at the bottom of the column is 76.8 to 100.8 ℃ (e.g., 76.8 ℃, 80.8 ℃, 82.8 ℃, 88.8 ℃, 90.8 ℃, 94.8 ℃, 100.8 ℃) and the reflux ratio is 8 to 15. Preferably, the operation pressure at the top of the tower is 0.35-0.45 MPaG, the operation temperature at the top of the tower is 84-92 ℃, the operation pressure at the bottom of the tower is 0.38-0.58 MPaG, and the operation temperature at the bottom of the tower is 86-94 ℃. Under the operation parameters, the cut-off amount of the light components in the materials is 3-6% of the feeding amount, and the light components separated from the tower top can be transferred to other processes for use.
According to an embodiment of the present invention, the operating parameters in the third distillation column include: the operation pressure at the top of the column is 0.3 to 0.6MPaG (e.g., 0.3MPaG, 0.4MPaG, 0.5MPaG, 0.6MPaG, etc.), the operation temperature at the top of the column is 79.2 to 103.2 ℃ (e.g., 79.2 ℃, 80.2 ℃, 82.2 ℃, 88.2 ℃, 90.2 ℃, 94.2 ℃, 98.2 ℃, 100.2 ℃, 103.2 ℃, etc.), the operation pressure at the bottom of the column is 0.32 to 0.63MPaG (e.g., 0.33MPaG, 0.43MPaG, 0.53MPaG, 0.63MPaG, etc.), and the operation temperature at the bottom of the column is 81.6 to 105.6 ℃ (e.g., 81.6 ℃, 82.6 ℃, 88.6 ℃, 90.6 ℃, 94.6 ℃, 98.6 ℃, 100.6 ℃, 103.6 ℃, 105.6 ℃, etc.). Preferably, the operation pressure at the top of the tower is 0.45-0.5 MPaG, the operation temperature at the top of the tower is 92-96 ℃, the operation pressure at the bottom of the tower is 0.48-0.53 MPaG, and the operation temperature at the bottom of the tower is 94-98 ℃. Under the operation parameters, the cut-off amount of heavy components in the materials is 1-3% of the feeding amount, the heavy components separated at the bottom of the tower can be used in other processes, and the high-purity trichlorosilane separated at the top of the tower can enter a subsequent reduction process to produce polycrystalline silicon products.
In another aspect of the invention, the invention provides a method for purifying trichlorosilane. According to the embodiment of the invention, the trichlorosilane purification method is implemented by the trichlorosilane purification system of the embodiment. Referring to fig. 3 and 4, the method for purifying trichlorosilane comprises the following steps:
s100: preparation of the additive
In the step, the metal simple substance and the organic solvent are supplied to an additive pretreatment device to be mixed, so that the additive is obtained.
According to an embodiment of the present invention, the metal element may be at least one selected from sodium, potassium, and magnesium, and preferably magnesium. The metal simple substance can react with CH in the trichlorosilane crude product3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And the carbon-containing impurities react to convert the carbon-containing impurities into substances with relatively high boiling points, so that the substances can be removed from the trichlorosilane by using a rectifying device in the following step.
According to some embodiments of the present invention, the organic solvent may be at least one selected from tetrahydrofuran and 2-methyltetrahydrofuran, and preferably 2-methyltetrahydrofuran. Therefore, CH in the metal simple substance and the trichlorosilane crude product can be further improved3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And the reaction efficiency of the carbon-containing impurities is equal, so that the removal rate of the carbon-containing impurities is further improved. The boiling point of 2-methyltetrahydrofuran is higher relative to tetrahydrofuran and is easier to remove by subsequent rectification.
According to some embodiments of the present invention, in the above additive, the mass fraction of the metal element may be 1 to 3%, for example, 1%, 1.5%, 2%, 2.5%, 3%. Therefore, the removal rate of carbon-containing impurities in the trichlorosilane can be further improved.
S200: reacting the trichlorosilane crude product with an additive
In the step, the trichlorosilane crude product and the additive are supplied to a trichlorosilane pretreatment device for reaction, and a mixed material is obtained. According to the embodiment of the invention, the metal simple substance in the additive can be mixed with CH in the trichlorosilane crude product3SiHCl2、(CH3)2SiCl2、(CH3)2SiHCl、CH3Cl、CH2Cl2And the carbon-containing impurities react to convert the carbon-containing impurities into substances with relatively high boiling points, so that the substances can be removed from the trichlorosilane by using a rectifying device in the following step. Taking an additive adopting metal Mg as an example, the reaction of the trichlorosilane crude product with the additive comprises the following steps:
Mg+CH3Cl→CH3MgCl；
Mg+CH2Cl2→CH2MgCl2；
CH3SiHCl2+CH3MgCl→(CH3)2SiHCl+MgCl2；
CH3MgCl+(CH3)2SiHCl→(CH3)3SiH+MgCl2；
CH3MgCl+(CH3)2SiCl2→(CH3)3SiCl+MgCl2；
CH2MgCl2+(CH3)2SiHCl→(CH3)3SiCl+MgCl2。
according to the embodiment of the invention, in the above step, the flow rate of the additive may be 0.005-0.015% of the flow rate of the trichlorosilane crude product, and is preferably 0.01%. Therefore, the stable reaction between the additive and the trichlorosilane crude product can be further ensured, and the removal rate of carbon-containing impurities in the trichlorosilane can be further improved.
S300: rectification treatment
In the step, the mixed material is supplied to a rectification device for rectification treatment, so as to obtain refined trichlorosilane. After the trichlorosilane reacts with the additive, most of the carbon-containing impurities are converted into substances with relatively high boiling points, and the substances can be removed from the trichlorosilane through rectification treatment. The content of carbon-containing impurities in the refined trichlorosilane obtained by rectification is less than 20 ppbw.
Referring to fig. 4, the S300 further includes:
s310: first rectification treatment
In the step, the mixed material is supplied to a first rectifying tower to be subjected to first rectifying treatment, so that a first tower top fraction and a first tower bottom fraction are obtained.
According to an embodiment of the present invention, in the first rectification treatment, the operation pressure at the top of the column is 0.2 to 0.5MPaG (e.g., 0.2MPaG, 0.3MPaG, 0.4MPaG, 0.5MPaG, etc.), the operation temperature at the top of the column is 70 to 96 ℃ (e.g., 70 ℃, 74 ℃, 76 ℃, 80 ℃, 88 ℃, 94 ℃, 96 ℃, etc.), the operation pressure at the bottom of the column is 0.22 to 0.52MPaG (e.g., 0.22MPaG, 0.32MPaG, 0.42MPaG, 0.52MPaG, etc.), the operation temperature at the bottom of the column is 72 to 98 ℃ (e.g., 72 ℃, 74 ℃, 76 ℃, 80 ℃, 82 ℃, 88 ℃, 90 ℃, 94 ℃, 98 ℃, etc.), and the reflux ratio is 10 to 20. Preferably, the operation pressure at the top of the tower is 0.3-0.4 MPaG, the operation temperature at the top of the tower is 80-88 ℃, the operation pressure at the bottom of the tower is 0.32-0.42 MPaG, and the operation temperature at the bottom of the tower is 82-90 ℃. Under the above operation parameters, the cut-off amount of the heavy components in the materials is 3-10% of the feeding amount, and the heavy components separated from the tower bottom can be transferred to other processes for use.
S320: second rectification treatment
In this step, the first overhead fraction is supplied to a second rectifying tower to be subjected to a second rectifying treatment, thereby obtaining a second overhead fraction and a second tower bottoms fraction.
According to an embodiment of the present invention, in the second rectification treatment, the column top operating pressure is 0.25 to 0.55MPaG (e.g., 0.25MPaG, 0.35MPaG, 0.45MPaG, 0.55MPaG, etc.), the column top operating temperature is 74 to 98 ℃ (e.g., 74 ℃, 76 ℃, 80 ℃, 82 ℃, 88 ℃, 90 ℃, 94 ℃, 98 ℃, etc.), the column bottom operating pressure is 0.27 to 0.57MPaG (e.g., 0.27MPaG, 0.37MPaG, 0.47MPaG, 0.57MPaG, etc.), the column bottom operating temperature is 76.8 to 100.8 ℃ (e.g., 76.8 ℃, 80.8 ℃, 82.8 ℃, 88.8 ℃, 90.8 ℃, 94.8 ℃, 100.8 ℃, etc.), and the reflux ratio is 8 to 15. Preferably, the operation pressure at the top of the tower is 0.35-0.45 MPaG, the operation temperature at the top of the tower is 84-92 ℃, the operation pressure at the bottom of the tower is 0.38-0.58 MPaG, and the operation temperature at the bottom of the tower is 86-94 ℃. Under the operation parameters, the cut-off amount of the light components in the materials is 3-6% of the feeding amount, and the light components separated from the tower top can be transferred to other processes for use.
S330: third rectification treatment
In this step, the second column bottom fraction is supplied to a third rectifying column to be subjected to a third rectifying treatment, so that a third column top fraction (refined trichlorosilane) and a third column bottom fraction are obtained.
According to an embodiment of the present invention, in the third rectification treatment, the column top operating pressure is 0.3 to 0.6MPaG (e.g., 0.3MPaG, 0.4MPaG, 0.5MPaG, 0.6MPaG, etc.), the column top operating temperature is 79.2 to 103.2 ℃ (e.g., 79.2 ℃, 80.2 ℃, 82.2 ℃, 88.2 ℃, 90.2 ℃, 94.2 ℃, 98.2 ℃, 100.2 ℃, 103.2 ℃, etc.), the column bottom operating pressure is 0.32 to 0.63MPaG (e.g., 0.33MPaG, 0.43MPaG, 0.53MPaG, 0.63MPaG, etc.), and the column bottom operating temperature is 81.6 to 105.6 ℃ (e.g., 81.6 ℃, 82.6 ℃, 88.6 ℃, 90.6 ℃, 94.6 ℃, 98.6 ℃, 100.6 ℃, 103.6 ℃, 105.6 ℃, etc.). Preferably, the operation pressure at the top of the tower is 0.45-0.5 MPaG, the operation temperature at the top of the tower is 92-96 ℃, the operation pressure at the bottom of the tower is 0.48-0.53 MPaG, and the operation temperature at the bottom of the tower is 94-98 ℃. Under the operation parameters, the cut-off amount of heavy components in the materials is 1-3% of the feeding amount, the heavy components separated at the bottom of the tower can be used in other processes, and the high-purity trichlorosilane separated at the top of the tower can enter a subsequent reduction process to produce polycrystalline silicon products.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
(1) Adding 1-3% of metal Mg in mass percent into 2-methyltetrahydrofuran, and uniformly stirring to obtain the additive.
(2) And adding the additive and the trichlorosilane crude product into a trichlorosilane pretreatment device for reaction, wherein the flow rate of the additive is 0.01 percent of that of the trichlorosilane crude product, and obtaining a mixed material after the reaction is finished.
(3) The mixture was fed to a first rectifying column to conduct a first rectifying treatment, the top pressure of the first rectifying column was set to 0.3MPaG, the top operating temperature was set to 80 ℃, the bottom operating pressure was set to 0.32MPaG, the bottom temperature was set to 82 ℃, the reflux ratio was 15, and the bottom cut was 7% of the feed amount.
(4) The overhead fraction separated in the first distillation column was fed to a second distillation column, and the second distillation column was subjected to a second distillation treatment, wherein the overhead pressure of the second distillation column was set to 0.4MPaG, the overhead operating temperature was set to 88 ℃, the column bottom operating pressure was set to 0.43MPaG, the column bottom temperature was set to 90 ℃, the reflux ratio was 11, and the overhead cut amount was 5% of the feed amount.
(5) And (3) supplying the bottom fraction separated in the second rectifying tower to a third rectifying tower for third rectifying treatment, wherein the top pressure of the third rectifying tower is set to be 0.45MPaG, the top operating temperature is set to be 92 ℃, the bottom operating pressure is set to be 0.48MPaG, the bottom temperature is set to be 94 ℃, the reflux ratio is 9, and the bottom cut amount is 2% of the feeding amount. And separating the high-purity trichlorosilane product from the tower top, wherein the content of carbon-containing impurities is less than 20 ppbw.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A trichlorosilane purification system is characterized by comprising:
an additive pretreatment device having a simple metal substance inlet, an organic solvent inlet, and an additive outlet;
the trichlorosilane pretreatment device is provided with a trichlorosilane crude product inlet, an additive inlet and a mixed material outlet, and the additive inlet is connected with the additive outlet;
the rectifying device is provided with a material inlet and a refined trichlorosilane outlet, and the material inlet is connected with the mixed material outlet.
2. The trichlorosilane purification system according to claim 1, wherein the rectification device comprises:
the first rectifying tower is provided with a mixed material inlet, a first tower top fraction outlet and a first tower bottom fraction outlet, and the mixed material inlet is connected with the mixed material outlet;
a second rectification column having a first overheads fraction inlet, a second overheads fraction outlet, and a second kettle fraction outlet, the first overheads fraction inlet coupled to the first overheads fraction outlet;
and the third rectifying tower is provided with a second tower kettle fraction inlet, a third tower top fraction outlet and a third tower kettle fraction outlet, and the second tower kettle fraction inlet is connected with the second tower kettle fraction outlet.
3. A trichlorosilane purification method is characterized in that the trichlorosilane purification method is implemented by using the trichlorosilane purification system of claim 1 or 2, and the trichlorosilane purification method comprises the following steps:
(1) supplying the metal simple substance and the organic solvent into an additive pretreatment device for mixing to obtain an additive;
(2) feeding the trichlorosilane crude product and the additive into a trichlorosilane pretreatment device for reaction to obtain a mixed material;
(3) and feeding the mixed material to a rectifying device for rectifying treatment to obtain the refined trichlorosilane.
4. The trichlorosilane purification method according to claim 3, wherein the elemental metal is selected from at least one of sodium, potassium and magnesium;
optionally, the organic solvent is selected from at least one of tetrahydrofuran, 2-methyltetrahydrofuran.
5. The trichlorosilane purification method according to claim 3, wherein the mass fraction of the metal simple substance in the additive is 1-3%.
6. The trichlorosilane purification method according to claim 3, wherein in the step (2), the flow rate of the additive is 0.005-0.015% of the flow rate of the trichlorosilane crude product.
7. The trichlorosilane purification method according to claim 3, wherein the step (3) further comprises:
(3-1) feeding the mixed material into a first rectifying tower for first rectifying treatment to obtain a first tower top fraction and a first tower bottom fraction;
(3-2) supplying the first overhead fraction to a second rectifying tower for second rectifying treatment to obtain a second overhead fraction and a second tower bottom fraction;
(3-3) supplying the second tower bottom fraction to a third rectifying tower for third rectifying treatment to obtain a third tower top fraction and a third tower bottom fraction.
8. The method for purifying trichlorosilane according to claim 7, wherein in the first rectification treatment, the operation pressure at the top of the tower is 0.2-0.5 MPaG, the operation temperature at the top of the tower is 70-96 ℃, the operation pressure at the bottom of the tower is 0.22-0.52 MPaG, the operation temperature at the bottom of the tower is 72-98 ℃, and the reflux ratio is 10-20.
9. The trichlorosilane purification method according to claim 7, wherein in the second rectification treatment, the operation pressure at the top of the tower is 0.25-0.55 MPaG, the operation temperature at the top of the tower is 74-98 ℃, the operation pressure at the bottom of the tower is 0.27-0.57 MPaG, the operation temperature at the bottom of the tower is 76.8-100.8 ℃, and the reflux ratio is 8-15.
10. The trichlorosilane purification method according to claim 7, wherein in the third rectification treatment, the operation pressure at the top of the tower is 0.3-0.6 MPaG, the operation temperature at the top of the tower is 79.2-103.2 ℃, the operation pressure at the bottom of the tower is 0.32-0.63 MPaG, and the operation temperature at the bottom of the tower is 81.6-105.6 ℃.
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Address after: 221004 No.66, Yangshan Road, Xuzhou Economic and Technological Development Zone, Jiangsu Province Applicant after: Jiangsu Xinhua Semiconductor Technology Co.,Ltd. Address before: 221004 No.66, Yangshan Road, Xuzhou Economic and Technological Development Zone, Jiangsu Province Applicant before: JIANGSU XINHUA SEMICONDUCTOR MATERIALS TECHNOLOGY CO.,LTD. |
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