WO2011024276A1 - クロロシランの精製方法 - Google Patents
クロロシランの精製方法 Download PDFInfo
- Publication number
- WO2011024276A1 WO2011024276A1 PCT/JP2009/064950 JP2009064950W WO2011024276A1 WO 2011024276 A1 WO2011024276 A1 WO 2011024276A1 JP 2009064950 W JP2009064950 W JP 2009064950W WO 2011024276 A1 WO2011024276 A1 WO 2011024276A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- chlorosilane
- exchange resin
- ion exchange
- silica gel
- crude
- Prior art date
Links
Images
Classifications
-
- 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
-
- 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
-
- 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
- C01B33/10784—Purification by adsorption
Definitions
- the present invention relates to a method for purifying chlorosilane.
- Chlorosilanes such as tetrachlorosilane (SiCl 4 ), trichlorosilane (SiHCl 3 ), and dichlorosilane (SiH 2 Cl 2 ) are used as manufacturing raw materials for polycrystalline silicon for semiconductors, monosilane for solar cells, liquid crystals, and the like.
- chlorosilane is produced, for example, by chlorinating metallurgical grade low-purity silicon called “metal silicon” with HCl or the like.
- the thus produced chlorosilane inevitably contains impurity metal elements derived from metallic silicon. Therefore, after the obtained chlorosilane is purified by distillation to remove inevitable impurities as much as possible to obtain high-purity chlorosilane, it is used as a raw material for semiconductor polycrystalline silicon, monosilane and the like.
- boron compound is contained in metal silicon at a ratio of several hundred ppbw to several hundred ppmw, boron becomes a P-type acceptor, which impairs the characteristics of polycrystalline silicon, monosilane and the like. For this reason, it is desired to remove the boron compound as much as possible from the chlorosilane containing the boron compound (hereinafter also referred to as crude chlorosilane), but the boron compound has a boiling point relatively close to that of the chlorosilane, It is difficult to separate by distillation and easily causes contamination of chlorosilane.
- Patent Document 1 a method of adding a silane chloride polymer when distilling crude chlorosilane (see Patent Document 1), a method of passing crude chlorosilane through a silica fixed bed in the gas phase (see Patent Document 1), and crude chlorosilane in a nitrile-supported zeolite. (See Patent Document 3).
- the method of distilling crude chlorosilane is not suitable for separating substances having close boiling points because the distillation operation is a separation method that uses the difference in boiling point between substances.
- the boiling points of dichlorosilane and boron trichloride at atmospheric pressure are about 8 ° C. and about 12 ° C., respectively, which are relatively close.
- Patent Document 1 even when a chlorosilane-based polymer is added during the distillation of the crude chlorosilane, this situation does not change.
- an object of the present invention is to provide a method for purifying crude chlorosilane that can be removed from the crude chlorosilane with a high removal rate and is suitable for industrialization.
- the present inventors have conducted intensive studies to solve the above technical problems. As a result, by bringing the crude chlorosilane containing the boron compound into contact with the ion exchange resin and silica gel, the boron compound contained as an impurity can be removed to a high degree, and the replacement frequency of the boron adsorbent is reduced. The inventors have found that it is possible to carry out purification stably and efficiently, and have completed the present invention.
- the present invention is a method for purifying crude chlorosilane containing a boron compound
- the present invention relates to a method comprising a step of bringing crude chlorosilane into contact with an ion exchange resin and a step of bringing crude chlorosilane into contact with a silica-based adsorbent.
- the present invention relates to a method for purifying crude chlorosilane, wherein a crude chlorosilane containing a boron compound is contacted with an ion exchange resin and then contacted with a silica-based adsorbent.
- chlorosilane in each contact step, chlorosilane is brought into contact with an ion exchange resin and / or silica gel controlled to have a moisture content of 2% or less.
- the ion exchange resin has the general formula (1) —CH 2 NR 1 R 2 (1) (Here, R 1 and R 2 independently represent hydrogen or an alkyl group) It has a functional group shown by.
- the silica-based adsorbent has a particle size range of 40-1000 ⁇ m with 75% or more of the arbitrarily sampled 200 particles having a 50% surface area average particle size of 300 ⁇ m or less.
- the silica gel has a specific surface area of BET of 450 m 2 / g or more.
- the particle diameter said here is an equivalent circle diameter which becomes equal to the projected area of the silica gel measured with the microscope.
- a boron compound can be sufficiently removed only by an adsorption operation without requiring a complicated distillation operation.
- purification can be performed at a low cost, which is suitable for industrialization.
- the crude chlorosilane to be purified is a kind of chlorosilane selected from dichlorosilane (SiH 2 Cl 2 ), trichlorosilane (SiHCl 3 ), tetrachlorosilane (SiCl 4 ), or a mixture of two or more chlorosilanes.
- Examples of such crude chlorosilane include crude chlorosilane obtained by chlorinating metallurgical grade silicon.
- a boron compound is inevitably included in a mixture mainly composed of dichlorosilane, trichlorosilane, and tetrachlorosilane. It is.
- the boron compound inevitably contained in the crude chlorosilane is not limited in its form, but the boron contained in the crude chlorosilane obtained by chlorinating metallurgical grade silicon is boron trichloride. It is often contained in the form of various chlorides such as diboron tetrachloride. The amount of the boron compound contained varies, but usually several ppbw to several ppmw of the boron compound remain in the crude chlorosilane.
- a crude chlorosilane containing the boron compound obtained by chlorinating metallurgical grade silicon is brought into contact with two adsorbents, an ion exchange resin and silica gel, to obtain a crude product.
- Boron compounds in chlorosilane are reduced or removed to obtain highly purified chlorosilane.
- the boron concentration in the crude chlorosilane as described above in which a boron compound of several ppbw to several ppmw remains can be reduced to 1 ppbw or less.
- the crude chlorosilane is first contacted with the ion exchange resin or the silica gel, and even if the crude chlorosilane is first contacted with the ion exchange resin and then contacted with the silica gel, You may make it contact with exchange resin.
- the ion exchange resin has a relatively low boron adsorption capacity, but the boron adsorption amount is large, whereas the silica gel is It was found that the boron adsorption capacity is high, but the boron adsorption amount is relatively small. Therefore, in order to maintain high purity purification over a long period of time, it is desirable to contact the crude chlorosilane in the order of ion exchange resin and silica gel.
- any substrate, functional group, etc. may be used as long as the boron compound can be ion exchange removed from the crude chlorosilane.
- R 1 and R 2 represent hydrogen and an alkyl group (preferably having 1 to 3 carbon atoms, particularly preferably 1 carbon atom))
- bonding the functional group represented by these can be used conveniently.
- Such an anion exchange resin also has a styrene unit having a specific surface area of BET of 15 m 2 / g to 20 m 2 / g and a pore volume of 0.5 to 1.0 ml / g by mercury porosimetry. It has been found that a weakly basic anion exchange resin made of a crosslinked copolymer is particularly preferred. Examples of such weakly basic anion exchange resins include “Amberlyst A-21” (registered trademark) manufactured by Rohm and Haas, and “Diaion WA-30” (registered trademark) manufactured by Mitsubishi Chemical. ).
- the silica gel used may be any silica gel as long as it can remove the boron compound from the crude chlorosilane. As a result of intensive studies by the present inventors, 75% or more of the particles are within the particle diameter range of 40 to 1000 ⁇ m. It was found that silica gel having a 50% surface area average particle size of 300 ⁇ m or less and a BET specific surface area of 450 m 2 / g or more is preferable. If the particle size of the silica gel is too large, the contact area with the crude chlorosilane is reduced, and the adsorption efficiency is reduced.
- silica gel examples include “Wakogel C-100” (registered trademark) manufactured by Wako Pure Chemical Industries, Ltd., “Grade 9385” and “Grade 7734” (both are trademarks) manufactured by Merck & Co., Inc.
- the water content of both the ion exchange resin and the silica gel is adjusted to 2% or less. This is because if the water content is 2% or more, the ion exchange resin is thermally deteriorated and the system is clogged with precipitated silica, which makes long-term stable operation difficult.
- the method of bringing the crude chlorosilane into contact with an adsorbent such as an ion exchange resin or silica gel is, for example, a method in which the crude chlorosilane is passed through a packed tower or vessel filled with the adsorbent, or in a vessel in which the crude chlorosilane is stored.
- an adsorbent such as an ion exchange resin or silica gel
- FIG. 1 is a flow chart showing an example of equipment for carrying out a method for purifying chlorosilane according to an embodiment of the present invention, wherein 1 is a first packed tower (inner diameter: 10.3 mm; packed height). 2400 mm), 2 is a second packed tower (inner diameter: 10.3 mm; packing height: 1200 mm).
- the first packed column 1 is packed with an adsorbent composed of a weakly basic anion exchange resin having a functional group of the above formula (1), for example, made of a crosslinked copolymer having a styrene unit.
- a crude chlorosilane supply pipe 3 is connected to the bottom of the tube.
- the second packed column 2 is made of silica gel in which 75% or more of the particles are in the particle diameter range of 40 to 1000 ⁇ m, the 50% surface area average particle diameter is 300 ⁇ m or less, and the BET specific surface area is 450 m 2 / g or more.
- a connecting pipe 4 extending from the top of the first packed tower 1 is connected to the bottom of the packed tower 2, and a purified chlorosilane extraction pipe 5 is connected to the top of the packed tower 2. Is extended.
- two packed towers are used, one being an ion exchange resin layer and the other being a silica gel layer.
- a partition is provided in one packed tower and the lower part of the tower is ionized.
- the exchange resin packed bed and the upper part of the tower may be configured as a silica gel packed bed.
- other purification equipment may be provided before and after the removal of impurities other than the boron compound.
- silica gel was used as one of the adsorbents, but if a desired quality can be obtained, a silica-based adsorbent other than silica gel, for example, as disclosed in Patent Document 2, Silica powder, fumed silica, amorphous silica, precipitated silica and the like can also be used. This is because an adsorbent composed of a silicon-based compound does not cause deterioration in the quality of high-purity chlorosilane.
- Example 1 Crude trichlorosilane having a boron concentration of 3000 ppbw was converted into an ion exchange resin (“Amberlyst A-21” (registered trademark) manufactured by Rohm and Haas) and silica gel (“Wakogel C-100” manufactured by Wako Pure Chemical Industries, Ltd.).
- ⁇ Comparative Example 2> Crude trichlorosilane having a boron concentration of 3000 ppbw was passed through a packed bed of silica gel (silica gel loading 165 g) at a flow rate of 135 g / hr.
- the filled silica gel is “Wakogel C-100” (registered trademark) manufactured by Wako Pure Chemical Industries, Ltd., and 75% or more of the particles are in the particle diameter range of 100 to 450 ⁇ m.
- % Surface area average particle diameter of 254 ⁇ m, pore diameter of 70 mm, specific surface area of 450 m 2 / g, and water content of 1.5% were used.
- Example 2 2.5 g of ion exchange resin was immersed in 50 g of crude tetrachlorosilane having a boron concentration of 790 ppmw.
- Two types “Amberlyst A-21” (registered trademark) manufactured by Rohm and Haas and “Amberlite IRA-743” (registered trademark) manufactured by Rohm and Haas, were used.
- “Amberlyst A-21” (registered trademark) is the same as that in Example 1, and “Amberlite IRA-743” (registered trademark) is applied to a base material composed of a crosslinked polymer having a styrene unit.
- ICP-AES dielectric coupled plasma emission spectrometer
- the effect of suppressing heat generation during the initial contact between the ion exchange resin and chlorosilane was found by lowering the resin moisture content.
- the resin heat resistance temperature is 100 ° C. or less at the initial contact between the ion exchange resin and chlorosilane, and thermal degradation of the functional group can be suppressed.
- ICP-AES dielectric coupled plasma emission spectrometer
- the ion exchange resin was found to adsorb boron for a period of nearly four times that of silica gel.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
また、特許文献3に記載されたようなニトリル担持ゼオライトに粗クロロシランを通過させる方法では、吸着剤の入れ替え等にコストがかかる上、吸着剤からの汚染が考えられるという問題があった。
粗クロロシランをイオン交換樹脂に接触させる工程と
粗クロロシランをシリカ系吸着剤に接触させる工程と
を含んでなる方法に関する。
一実施態様では、各接触工程において、クロロシランは、含水率2%以下に管理したイオン交換樹脂及び/又はシリカゲルに接触させる。一実施態様では、イオン交換樹脂は、一般式(1)
-CH2NR1R2 (1)
(ここで、R1、R2は独立して水素又はアルキル基を表す)
で示される官能基を有する。他の実施態様では、シリカ系吸着剤は、任意に200個サンプリングした粒子の75%以上が40~1000μmの粒子径範囲内にあり、50%表面積平均粒子径が300μm以下である。また、BETでの比表面積が450m2/g以上を有するシリカゲルである。尚、ここで言う粒子径は顕微鏡で測定したシリカゲルの投影面積と等しくなる円相当径である。
ここで、粗クロロシランをイオン交換樹脂及びシリカゲルの何れに最初に接触させるかは任意であり、イオン交換樹脂に最初に接触させた後にシリカゲルに接触させても、シリカゲルに最初に接触させた後にイオン交換樹脂に接触させても構わない。しかしながら、本発明者等は、種々のイオン交換樹脂と種々の特性のシリカゲルを組み合わせて鋭意検討した結果、イオン交換樹脂はボロン吸着能力が比較的低いが、ボロン吸着量は多く、一方、シリカゲルはボロン吸着能力が高いが、ボロン吸着量は比較的少ないことを知見した。よって、高純度の精製を長期に維持するためには、粗クロロシランを、イオン交換樹脂、シリカゲルの順に接触させることが望ましい。
-CH2NR1R2 (1)
(上式中、R1、R2は水素、アルキル基(炭素数は1~3が望ましく、特に炭素数1が望ましい)を表す)
で表される官能基を結合してなる陰イオン交換樹脂を好適に使用できることが分かった。またかかる陰イオン交換樹脂においても、BETでの比表面積が15m2/g~20m2/g、水銀圧入法での細孔容積が0.5~1.0ml/gである、スチレン単位を有する架橋共重合体からなる弱塩基性陰イオン交換樹脂が特に好ましいことが分かった。このような弱塩基性陰イオン交換樹脂としては、例えば、ローム・アンド・ハース社製の「アンバーリストA-21」(登録商標)、三菱化学社製の「ダイヤイオンWA-30」(登録商標)が挙げられる。
かかるシリカゲルとしては、例えば、和光純薬工業株式会社製の「ワコーゲルC-100」(登録商標)、メルク社製「Grade9385」、「Grade7734」(何れも商標)が挙げられる。
かかるクロロシラン精製設備では、粗クロロシランは、最初に弱塩基性陰イオン交換樹脂層を通過した後、シリカゲル層を通過するため、粗クロロシランからのボロン化合物の除去を、高い除去率で簡易に行うことができる。
ボロン濃度3000ppbwの粗トリクロロシランを、イオン交換樹脂(ローム・アンド・ハース社製の「アンバーリストA-21」(登録商標))とシリカゲル(和光純薬工業株式会社製の「ワコーゲルC-100」(登録商標)(粒子の75%以上が100~450μmの粒子径範囲内にあり、50%表面積平均粒子径254μm、細孔径70Å、比表面積450m2/g)の充填層(イオン交換樹脂充填量=72g、シリカゲル充填量=55g)に135g/hrの流量で通過させた。また、イオン交換樹脂の含水率は1.7%、シリカゲルの含水率は1.5%のものを使用した。また充填層の上流側にイオン交換樹脂を、下流側にシリカゲルを充填した。
ボロン濃度3000ppbwの粗トリクロロシランをイオン交換樹脂(ローム・アンド・ハース社製の「アンバーリストA-21」(登録商標))の充填層(イオン交換樹脂充填量=108g)に135g/hrの流量で通過させた。また、イオン交換樹脂の含水率は1.7%のものを使用した。
ボロン濃度3000ppbwの粗トリクロロシランをシリカゲルの充填層(シリカゲル充填量=165g)に135g/hrの流量で通過させた。充填したシリカゲルは、実施例1におけるものと同じく、和光純薬工業株式会社製の「ワコーゲルC-100」(登録商標)で粒子の75%以上が100~450μmの粒子径範囲内にあり、50%表面積平均粒子径254μm、細孔径70Å、比表面積450m2/g、含水率1.5%のものを使用した。
ボロン濃度790ppmwの粗テトラクロロシラン50gにイオン交換樹脂2.5gを浸漬した。ローム・アンド・ハース社製の「アンバーリストA-21」(登録商標)、ローム・アンド・ハース社製の「アンバーライトIRA-743」(登録商標)の2種類を使用した。
「アンバーリストA-21」(登録商標)は実施例1におけるものと同じもので、「アンバーライトIRA-743」(登録商標)はスチレン単位を有する架橋重合体からなる基材等に、一般式(2):
-CH2NCH3CH2[CH(OH)]4CH2OH (2)
で表される官能基を結合してなるイオン交換樹脂である。
-CH2NR1R2 (1)
(ここで、R1、R2は独立して水素、アルキル基を表す)
で示される官能基を有するイオン交換樹脂はボロン吸着量が大きいことが判明した。
ボロン濃度13~24ppbwの粗トリクロロシランをシリカゲル充填層(シリカゲル充填量=約30g)に135g/hrの流量で通過させた。充填したシリカゲルの含水率は1.4~1.7%で、粒子径の異なるものを3種使用した。
ボロン濃度3000ppbwの粗トリクロロシランを含水率の異なるイオン交換樹脂充填層(イオン交換樹脂充填量=12g;ローム・アンド・ハース社製の「アンバーリストA-21」(登録商標))にフィードし、イオン交換樹脂とクロロシランの初期接触時の発熱を測定した。また、イオン交換樹脂通過前後のクロロシランをサンプリングし、含有ボロン濃度を誘電結合プラズマ発光分析装置(ICP-AES)にて測定し、イオン交換樹脂のボロン吸着量を測定した。結果を表6に示す。
ボロン濃度3000ppbwの粗トリクロロシランを含水率の異なるシリカゲル充填層(シリカゲル充填量=19g;和光純薬工業株式会社製の「ワコーゲルC-100」(登録商標))にフィードした。シリカゲル通過前後のクロロシランをサンプリングし、含有ボロン濃度を誘電結合プラズマ発光分析装置(ICP-AES)にて測定し、シリカゲルのボロン吸着量を測定した。結果を表7に示す。
ボロン濃度3000ppbwの粗トリクロロシランをイオン交換樹脂充填層(イオン交換樹脂充填量=12g;ローム・アンド・ハース社製の「アンバーリストA-21」(登録商標))、及び、シリカゲル充填層(シリカゲル充填量=18g;和光純薬工業株式会社製の「ワコーゲルC-100」(登録商標))にそれぞれ3.24kg/dayの流量で通過させた。充填したイオン交換樹脂の含水率は1.7%、シリカゲルの含水率は1.5%のものを使用した。
2 第二充填塔
3 供給管
4 接続管
5 抜出し管
Claims (5)
- ボロン化合物を含有する粗クロロシランを精製する方法であって、
粗クロロシランをイオン交換樹脂に接触させる工程と
粗クロロシランをシリカ系吸着剤に接触させる工程と
を含んでなる方法。 - ボロン化合物を含有する粗クロロシランをイオン交換樹脂に接触させた後にシリカ系吸着剤に接触させる、請求項1に記載の精製方法。
- 含水率2%以下に管理したイオン交換樹脂及びシリカ系吸着剤にクロロシランを接触させる、請求項1又は2に記載の精製方法。
- イオン交換樹脂が、一般式(1)
-CH2NR1R2 (1)
(ここで、R1、R2は独立して水素又はアルキル基を表す)
で示される官能基を有する、請求項1から3の何れか一項に記載の精製方法。 - シリカ系吸着剤が、粒子の75%以上が40~1000μmの粒子径範囲内、300μm以下の50%表面積平均粒子径、450m2/g以上の比表面積を有するシリカゲルである、請求項1から4の何れか一項に記載の精製方法。
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2009/064950 WO2011024276A1 (ja) | 2009-08-27 | 2009-08-27 | クロロシランの精製方法 |
KR1020127007452A KR101629061B1 (ko) | 2009-08-27 | 2009-08-27 | 클로로실란의 정제 방법 |
CN2009801611866A CN102482106A (zh) | 2009-08-27 | 2009-08-27 | 氯硅烷的提纯方法 |
EP09848724.2A EP2471740A4 (en) | 2009-08-27 | 2009-08-27 | PROCESS FOR THE PURIFICATION OF CHLOROSILANE |
SG2012012191A SG178848A1 (en) | 2009-08-27 | 2009-08-27 | Method for purifying chlorosilane |
US13/391,912 US20120148471A1 (en) | 2009-08-27 | 2009-08-27 | Method for purifying chlorosilane |
JP2011528558A JP5513511B2 (ja) | 2009-08-27 | 2009-08-27 | クロロシランの精製方法 |
TW099128581A TWI485109B (zh) | 2009-08-27 | 2010-08-26 | 氯矽烷的精製方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2009/064950 WO2011024276A1 (ja) | 2009-08-27 | 2009-08-27 | クロロシランの精製方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2011024276A1 true WO2011024276A1 (ja) | 2011-03-03 |
Family
ID=43627403
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2009/064950 WO2011024276A1 (ja) | 2009-08-27 | 2009-08-27 | クロロシランの精製方法 |
Country Status (8)
Country | Link |
---|---|
US (1) | US20120148471A1 (ja) |
EP (1) | EP2471740A4 (ja) |
JP (1) | JP5513511B2 (ja) |
KR (1) | KR101629061B1 (ja) |
CN (1) | CN102482106A (ja) |
SG (1) | SG178848A1 (ja) |
TW (1) | TWI485109B (ja) |
WO (1) | WO2011024276A1 (ja) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2013163614A1 (en) * | 2012-04-27 | 2013-10-31 | Centrotherm Photovoltaics Usa, Inc. | Advanced off-gas recovery process and system |
WO2014167757A1 (ja) | 2013-04-11 | 2014-10-16 | 信越化学工業株式会社 | シラン化合物またはクロロシラン化合物の精製方法、多結晶シリコンの製造方法、および、弱塩基性イオン交換樹脂の再生処理方法 |
EP2778133A4 (en) * | 2011-11-11 | 2015-07-15 | Lg Chemical Ltd | DEVICE FOR FINISHING TRIHALOSILANE |
JP7477620B2 (ja) | 2020-11-05 | 2024-05-01 | ワッカー ケミー アクチエンゲゼルシャフト | クロロシラン混合物から不純物を除去する方法 |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2013067283A2 (en) * | 2011-11-02 | 2013-05-10 | Gtat Corporation | Purification of trichlorosilane |
CN102701216B (zh) * | 2012-06-19 | 2015-06-03 | 中国恩菲工程技术有限公司 | 一种二氯二氢硅除杂方法 |
CN102701217A (zh) * | 2012-06-19 | 2012-10-03 | 中国恩菲工程技术有限公司 | 一种二氯二氢硅除杂设备 |
CN103241742B (zh) * | 2013-05-13 | 2015-02-18 | 杨恺 | 高纯度SiCl4提纯方法 |
DE102017125221A1 (de) * | 2017-10-27 | 2019-05-02 | Nexwafe Gmbh | Verfahren und Vorrichtung zur Entfernung von Verunreinigungen aus Chlorsilanen |
CN108017060B (zh) * | 2018-02-09 | 2019-06-28 | 浙江博瑞电子科技有限公司 | 一种六氯乙硅烷的纯化方法 |
WO2021104618A1 (de) * | 2019-11-27 | 2021-06-03 | Wacker Chemie Ag | Verfahren zur entfernung einer verunreinigung aus einem chlorsilangemisch |
CN113402640A (zh) * | 2021-06-10 | 2021-09-17 | 青海亚洲硅业半导体有限公司 | 用于氯硅烷除杂的吸附树脂及其制备方法 |
CN113479892B (zh) * | 2021-07-30 | 2023-09-26 | 天津大学 | 三氯氢硅除碳反应-选择性吸附耦合装置及方法 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5983925A (ja) | 1982-09-29 | 1984-05-15 | ダウ・コ−ニング・コ−ポレ−シヨン | クロロシランの精製方法 |
JPS61167693A (ja) * | 1985-01-22 | 1986-07-29 | Showa Denko Kk | ジクロロシランの精製方法 |
JPS61197415A (ja) | 1985-02-27 | 1986-09-01 | Showa Denko Kk | ジクロロシランの精製法 |
JPH02153815A (ja) * | 1988-12-06 | 1990-06-13 | Mitsubishi Metal Corp | クロロポリシランの精製方法 |
JPH02196014A (ja) * | 1989-01-25 | 1990-08-02 | Denki Kagaku Kogyo Kk | 高純度ジクロロシランの製造方法 |
JP2007001791A (ja) | 2005-06-21 | 2007-01-11 | Mitsubishi Materials Polycrystalline Silicon Corp | 三塩化シランの精製方法 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3414603A (en) * | 1965-03-16 | 1968-12-03 | Tyco Laboratories Inc | Method of purifying organochlorosilanes |
US3968199A (en) * | 1974-02-25 | 1976-07-06 | Union Carbide Corporation | Process for making silane |
US4676967A (en) * | 1978-08-23 | 1987-06-30 | Union Carbide Corporation | High purity silane and silicon production |
US4713230A (en) * | 1982-09-29 | 1987-12-15 | Dow Corning Corporation | Purification of chlorosilanes |
US4900520A (en) * | 1988-10-31 | 1990-02-13 | Gaf Chemicals Corporation | Process for removal of soluble platinum group metal catalysts from liquid product mixtures |
DE102007050199A1 (de) * | 2007-10-20 | 2009-04-23 | Evonik Degussa Gmbh | Entfernung von Fremdmetallen aus anorganischen Silanen |
CN101428804A (zh) * | 2008-12-03 | 2009-05-13 | 孙永敏 | 用树脂去除氯硅烷类物料中硼磷离子的方法 |
-
2009
- 2009-08-27 JP JP2011528558A patent/JP5513511B2/ja active Active
- 2009-08-27 EP EP09848724.2A patent/EP2471740A4/en not_active Withdrawn
- 2009-08-27 SG SG2012012191A patent/SG178848A1/en unknown
- 2009-08-27 KR KR1020127007452A patent/KR101629061B1/ko active IP Right Grant
- 2009-08-27 US US13/391,912 patent/US20120148471A1/en not_active Abandoned
- 2009-08-27 WO PCT/JP2009/064950 patent/WO2011024276A1/ja active Application Filing
- 2009-08-27 CN CN2009801611866A patent/CN102482106A/zh active Pending
-
2010
- 2010-08-26 TW TW099128581A patent/TWI485109B/zh active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5983925A (ja) | 1982-09-29 | 1984-05-15 | ダウ・コ−ニング・コ−ポレ−シヨン | クロロシランの精製方法 |
JPS61167693A (ja) * | 1985-01-22 | 1986-07-29 | Showa Denko Kk | ジクロロシランの精製方法 |
JPS61197415A (ja) | 1985-02-27 | 1986-09-01 | Showa Denko Kk | ジクロロシランの精製法 |
JPH02153815A (ja) * | 1988-12-06 | 1990-06-13 | Mitsubishi Metal Corp | クロロポリシランの精製方法 |
JPH02196014A (ja) * | 1989-01-25 | 1990-08-02 | Denki Kagaku Kogyo Kk | 高純度ジクロロシランの製造方法 |
JP2007001791A (ja) | 2005-06-21 | 2007-01-11 | Mitsubishi Materials Polycrystalline Silicon Corp | 三塩化シランの精製方法 |
Non-Patent Citations (1)
Title |
---|
See also references of EP2471740A4 * |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2778133A4 (en) * | 2011-11-11 | 2015-07-15 | Lg Chemical Ltd | DEVICE FOR FINISHING TRIHALOSILANE |
WO2013163614A1 (en) * | 2012-04-27 | 2013-10-31 | Centrotherm Photovoltaics Usa, Inc. | Advanced off-gas recovery process and system |
CN104411636A (zh) * | 2012-04-27 | 2015-03-11 | 森特瑟姆光伏美国有限公司 | 改进的尾气回收方法和系统 |
WO2014167757A1 (ja) | 2013-04-11 | 2014-10-16 | 信越化学工業株式会社 | シラン化合物またはクロロシラン化合物の精製方法、多結晶シリコンの製造方法、および、弱塩基性イオン交換樹脂の再生処理方法 |
JP2014205589A (ja) * | 2013-04-11 | 2014-10-30 | 信越化学工業株式会社 | シラン化合物またはクロロシラン化合物の精製方法、多結晶シリコンの製造方法、および、弱塩基性イオン交換樹脂の再生処理方法 |
US9669400B2 (en) | 2013-04-11 | 2017-06-06 | Shin-Etsu Chemical Co., Ltd. | Method for purifying silane compound or chlorosilane compound, method for producing polycrystalline silicon, and method for regenerating weakly basic ion-exchange resin |
EP3296261A1 (en) | 2013-04-11 | 2018-03-21 | Shin-Etsu Chemical Co., Ltd. | Method for regenerating weakly basic ion-exchange resin |
JP7477620B2 (ja) | 2020-11-05 | 2024-05-01 | ワッカー ケミー アクチエンゲゼルシャフト | クロロシラン混合物から不純物を除去する方法 |
Also Published As
Publication number | Publication date |
---|---|
KR20120090990A (ko) | 2012-08-17 |
TW201119942A (en) | 2011-06-16 |
US20120148471A1 (en) | 2012-06-14 |
JPWO2011024276A1 (ja) | 2013-01-24 |
EP2471740A1 (en) | 2012-07-04 |
TWI485109B (zh) | 2015-05-21 |
KR101629061B1 (ko) | 2016-06-09 |
SG178848A1 (en) | 2012-04-27 |
EP2471740A4 (en) | 2014-07-30 |
CN102482106A (zh) | 2012-05-30 |
JP5513511B2 (ja) | 2014-06-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5513511B2 (ja) | クロロシランの精製方法 | |
JP5122700B1 (ja) | モノシランの精製方法 | |
JP5738289B2 (ja) | ハロゲンシランを不均化するため及び異種金属を除去するための方法及びアミノ官能性樹脂の使用 | |
JP3892794B2 (ja) | クロロシラン及びその精製方法 | |
JP5879283B2 (ja) | トリクロロシランの製造方法 | |
KR101307074B1 (ko) | 육염화 이규소의 정제 방법 및 고순도 육염화 이규소 | |
WO2018131500A1 (ja) | 多結晶シリコンの製造方法 | |
TWI568673B (zh) | 三氯矽烷之純化 | |
KR101134230B1 (ko) | 염화실란 정제 방법 및 시스템, 그리고 금속계 불순물 정제용 흡착제 | |
US5723644A (en) | Phosphorous removal from chlorosilane | |
CA1207127A (en) | Purification of chlorosilanes | |
JPH1036377A (ja) | 高純度アルコキシシランの製造方法 | |
TWI773121B (zh) | 獲得六氯二矽烷的方法 | |
JP2006117559A (ja) | トリメチルシランの精製方法 | |
JPWO2020153342A1 (ja) | 精製クロロシラン類の製造方法 | |
KR20120106290A (ko) | 삼염화실란의 정제 방법 | |
KR20160143973A (ko) | 음이온 교환수지를 이용한 클로로실란의 정제방법 | |
TW201339167A (zh) | 三甲基矽烷之純化方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 200980161186.6 Country of ref document: CN |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 09848724 Country of ref document: EP Kind code of ref document: A1 |
|
WWE | Wipo information: entry into national phase |
Ref document number: 13391912 Country of ref document: US Ref document number: 2011528558 Country of ref document: JP |
|
REEP | Request for entry into the european phase |
Ref document number: 2009848724 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2009848724 Country of ref document: EP |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
ENP | Entry into the national phase |
Ref document number: 20127007452 Country of ref document: KR Kind code of ref document: A |