JPH0749093B2 - Method for treating gas containing silicon compound - Google Patents
Method for treating gas containing silicon compoundInfo
- Publication number
- JPH0749093B2 JPH0749093B2 JP62046448A JP4644887A JPH0749093B2 JP H0749093 B2 JPH0749093 B2 JP H0749093B2 JP 62046448 A JP62046448 A JP 62046448A JP 4644887 A JP4644887 A JP 4644887A JP H0749093 B2 JPH0749093 B2 JP H0749093B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- silicon compound
- sio
- gas containing
- silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Landscapes
- Treating Waste Gases (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は高純度珪素製造工程等において排出されるガス
に含まれるシラン、クロルシラン、四塩化珪素等の珪素
化合物をアルカリ水溶液で洗浄、除去する排ガスの処理
方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial field of application) The present invention cleans and removes silicon compounds such as silane, chlorosilane, and silicon tetrachloride contained in gas discharged in a high-purity silicon manufacturing process with an alkaline aqueous solution. The present invention relates to a method for treating exhaust gas.
（従来の技術） 高純度珪素製造工程等において排出されるガス（水素ガ
ス）中には、シラン（SiH4）、クロルシラン（SiH4-nCl
n）、四塩化珪素（SiCl4）等の珪素化合物ガスと塩化水
素（HCl）ガスが含まれている。(Prior art) Silane (SiH 4 ) and chlorosilane (SiH 4-n Cl) are contained in the gas (hydrogen gas) discharged in the high-purity silicon manufacturing process.
n), a silicon compound gas such as silicon tetrachloride (SiCl 4 ) and hydrogen chloride (HCl) gas.
しかるに、このような珪素化合物は下記のように水と反
応して二酸化珪素（SiO2）が生成する。However, such a silicon compound reacts with water to form silicon dioxide (SiO 2 ) as described below.
SiH4＋2H2O→SiO2＋4H2 SiH4-nCln＋2H2O→SiO2＋（４−ｎ）H2＋nHCl SiCl4＋2H2O→SiO2＋4HCl 従来よりこのような珪素化合物を含むガスを処理する方
法としては、ガスを苛性ソーダ（NaOH）水溶液で洗浄
（気液接触）し、これらの珪素化合物をSiO2に分解し、
同時にHClを中和する方法が行はれているが、生成したS
iO2な酸性〜弱アルカリ性ではゲル状で析出し装置、機
器等の表面に付着し目詰り、閉塞、圧力損失増大の原因
となるため洗浄液のPHを13〜14に調整しSiO2をNa2SiO3
（メタ珪素ナトリウム）にする必要がある。SiH 4 + 2H 2 O → SiO 2 + 4H 2 SiH 4-n Cln + 2H 2 O → SiO 2 + (4-n) H 2 + nHCl SiCl 4 + 2H 2 O → SiO 2 + 4HCl Conventionally, a gas containing such a silicon compound is treated. As a method to do so, the gas is washed with a caustic soda (NaOH) aqueous solution (gas-liquid contact), these silicon compounds are decomposed into SiO 2 ,
At the same time, there is a method to neutralize HCl.
In the case of iO 2 which is acidic to weakly alkaline, it precipitates in the form of gel and adheres to the surface of equipment and devices, causing clogging, blockage and increased pressure loss.Adjust the pH of the cleaning solution to 13-14 and change SiO 2 to Na 2 SiO 3
(Sodium metasilicon) is required.
SiO2＋2NaOH→Na2SiO3＋H2O 従って、非常に大量の苛性ソーダを必要とするという問
題がある。SiO 2 +2 NaOH → Na 2 SiO 3 + H 2 O Therefore, there is a problem that a very large amount of caustic soda is required.
（発明が解決しようとする問題点） 本発明は、上記のような従来法の問題点を解決し、処理
費が極めて低廉な高純度珪素製造工程等より排出される
珪素化合物を含むガスの処理方法を提供することを目的
とするものである。(Problems to be Solved by the Invention) The present invention solves the problems of the conventional methods as described above, and treats a gas containing a silicon compound discharged from a high-purity silicon manufacturing process or the like at a very low treatment cost. It is intended to provide a method.
（問題点を解決するための手段） 従来法が珪素化合物を含むガスをNaOH水溶液を使用しPH
＝13〜14で洗浄するに対し、本発明は水酸化カルシウム
［Ca（OH）２］懸濁水を使用し液のPHを9.5〜10.5に保
持しつつ洗浄するものである。(Means for Solving Problems) In the conventional method, a gas containing a silicon compound is used as a pH solution by using an aqueous NaOH solution.
= 13 to 14, the present invention uses calcium hydroxide [Ca (OH) 2 ] suspension water while maintaining the pH of the solution at 9.5 to 10.5.
本発明者等は種々実験研究の結果、高純度珪素製造工程
から排出される珪素化合物を含むガスをCa（OH）２懸濁
水で洗浄（気液接触）すると、まずガス中に含まれる珪
素化合物は水と反応しSiO2が生成すると共にH ClはCa
（OH）２により中和され、このときSiO2はゲル状で析出
するが、洗浄水のPHを9.5〜10.5に保持することにより
析出したSiO2とCa（OH）２が反応し、Ca（HSiO3）２と
なりゲル状SiO2を伴つて極めて沈降しやすいスラリーと
なることを知り本発明を完成したもので、PH9.5以下で
はゲル状物質を残り沈降分離が困難でPH10.5以上ではCa
（OH）２を余分に消費するのみで特別の効果は認められ
ない。As a result of various experimental studies, the present inventors found that when a gas containing a silicon compound discharged from a high-purity silicon manufacturing process was washed with Ca (OH) 2 suspension water (gas-liquid contact), the silicon compound contained in the gas was first obtained. Reacts with water to form SiO 2 and H Cl is Ca
It is neutralized by (OH) 2 , and at this time SiO 2 is precipitated in the form of gel, but by maintaining the pH of the washing water at 9.5 to 10.5, the precipitated SiO 2 reacts with Ca (OH) 2 to form Ca (OH) 2. The present invention has been completed by knowing that HSiO 3 ) 2 becomes a slurry that easily precipitates together with gel-like SiO 2 , and the gel-like substance remains at PH 9.5 or less and sedimentation separation is difficult, and at PH 10.5 or more. Ca
Only extra consumption of (OH) 2 and no special effect.
すなわち、本発明は高純度珪素製造工程等より排出され
るシラン、クロルシラン、四塩化珪素等の珪素化合物の
少なくとも１成分を含むガスと水酸化カルシウム懸濁水
とをPH9.5〜10.5で気液接触させた後、生成したスラリ
ーを沈降、分離すると共に、その母液に水酸化カルシウ
ムを添加してPHを調整し循環再使用する。That is, according to the present invention, a gas containing at least one component of a silicon compound such as silane, chlorosilane, and silicon tetrachloride discharged from a high-purity silicon manufacturing process and calcium hydroxide suspension water are brought into contact with each other at a pH of 9.5 to 10.5. After that, the produced slurry is settled and separated, and calcium hydroxide is added to the mother liquor to adjust the PH and reused by circulation.
以下、本発明を図面に基づいて詳細に説明する。Hereinafter, the present invention will be described in detail with reference to the drawings.
図面は本発明の実施例のフローシートを示すもので、
（１）はジエツトスクラバ、（２）は循環槽、（３）は
沈降分離槽である。The drawings show a flow sheet of an embodiment of the present invention,
(1) is a jet scrubber, (2) is a circulation tank, and (3) is a sedimentation separation tank.
珪素化合物を含む被処理ガスはガス導入管（４）を経て
ジエツトスクラバ（１）に導入され、ここで管（５）を
経て導入される、後記する循環液と気液接触し、ガス中
の珪素化合物はSiO2、Ca（HSiO3）２に変化し循環槽
（２）に送られ、次いで生成したスラリーを含む循環槽
内液はポンプ（６）を介し、管（７）を経て沈降分離槽
（３）に導かれ、ここで沈降、分離したスラリーは管
（８）を経てポンプ（９）により系外に取り出され、そ
の上澄み液は管（10）を経て循環槽（２）へ還流され
る。The gas to be treated containing a silicon compound is introduced into the jet scrubber (1) via the gas introduction pipe (4), and is introduced into the jet scrubber (1) through the pipe (5) to be in contact with a circulating liquid described later to make contact with the circulating liquid, and the silicon in the gas The compound changes into SiO 2 and Ca (HSiO 3 ) 2 and is sent to the circulation tank (2). Then, the liquid in the circulation tank containing the produced slurry passes through the pump (6), the pipe (7) and the sedimentation separation tank. The slurry, which is guided to (3), where it is settled and separated, is taken out of the system by the pump (9) through the pipe (8), and the supernatant liquid is refluxed to the circulation tank (2) through the pipe (10). It
一方、循環液と気液接触し珪素化合物、およびH Clガス
を除去されたガスは管（11）を経て系外に取り出され
る。On the other hand, the gas which is in gas-liquid contact with the circulating liquid to remove the silicon compound and H 2 Cl 2 gas is taken out of the system through the pipe (11).
（12）はPH検出器で循環槽内液のPHを検出し連動するバ
ルブ（13）を作動し管（14）よりCa（OH）２スラリーを
循環槽に注入し、槽内液のPHは9.5〜10.5に調整され、
その槽内液は循環液としてポンプ（15）により管（５）
を経て、前記したようにジエツトスクラバ（１）に導入
され、ガス導入管（４）を経て導入される被処理ガスと
気液接触する。以上の連続操作によつて処理が進行す
る。（16）は補給水供給管を示す。(12) is a PH detector that detects the pH of the liquid in the circulation tank and activates the interlocking valve (13) to inject Ca (OH) 2 slurry from the pipe (14) into the circulation tank. Adjusted to 9.5 to 10.5,
The liquid in the tank is used as a circulating liquid by a pipe (5) by a pump (15).
As described above, the gas is introduced into the jet scrubber (1) and comes into gas-liquid contact with the gas to be treated introduced through the gas introduction pipe (4). The process proceeds by the above continuous operation. (16) shows a makeup water supply pipe.
なお、上記実施例において気液接触装置としてジエツト
スクラバを使用したが、もれ棚等の他の型式の気液接触
装置を使用してもよい。Although the jet scrubber is used as the gas-liquid contactor in the above embodiment, another type of gas-liquid contactor such as a leak rack may be used.
（発明の効果） 以上の説明で明らかなように、従来法によれば装置、機
器等の目詰まり、閉塞等の障害を防止するためには、Na
OHを使用し循環液のPHを13〜14に保持し、生成したゲル
状のSiO2をNa2SiO3にする必要があり、そのため高価なN
aOHを多量必要とするが、本発明によれば安価なCa（O
H）２を使用し循環液のPHを9.5〜10.5に保持することに
より、ゲル状のSiO2は生成したCa（HSiO3）２との共存
により極めて沈降し易いスラリーとなつて容易に沈降、
分離できるため、装置、機器等に付着し、目詰まり、閉
塞等をおこすことなく安定な運転をすることが可能で、
Ca（OH）２の消費量はSiO2lモルに対して1/2モル以下で
充分で、且つ、Ca（OH）２の購入単価はNaOHに比較しは
るかに安価であるから、従来法に比較し本発明方法によ
ればその処理費は極めて低廉である。(Effects of the Invention) As is clear from the above description, according to the conventional method, in order to prevent obstacles such as clogging and blockage of devices and equipment, Na
It is necessary to keep the pH of the circulating fluid at 13 to 14 by using OH, and to convert the formed gel-like SiO 2 into Na 2 SiO 3 , which is why expensive N
Although a large amount of aOH is required, the inexpensive Ca (O
H) 2 is used to maintain the pH of the circulating fluid at 9.5 to 10.5, so that gel-like SiO 2 easily precipitates as a slurry that is extremely prone to coexist due to the coexistence of Ca (HSiO 3 ) 2 formed,
Since it can be separated, it can be attached to equipment, equipment, etc., and stable operation can be performed without causing clogging, blockage, etc.
The consumption amount of Ca (OH) 2 is sufficient to be 1/2 mol or less with respect to SiO 2 l mol, and the purchase unit price of Ca (OH) 2 is much lower than that of NaOH. In comparison, according to the method of the present invention, the processing cost is extremely low.
（実施例） 図面に示すフローシートにしたがって、下記条件で行つ
た。(Example) The process was carried out under the following conditions according to the flow sheet shown in the drawing.
（１）被処理ガスの成分 SiCl4 0.021mol/m3 SiHCl3 0.001 〃 SiH2Cl2 0.013 〃 HCl 0.37 〃 （その他 H2ガス） （２）ガス量 30 Nm3/Hr （３）循環液量 4.20 m3/Hr （４）循環液のPH 10.0 上記条件で、約111時間連続運転した結果、Ca（OH）２
の消費量はガス100m3当たり2.1Kgで、装置、機器類には
付着物なく、安定な運転が可能で、出口ガス中の各珪素
化合物の含有量はTraceであつた。(1) Components of gas to be treated SiCl 4 0.021mol / m 3 SiHCl 3 0.001 〃 SiH 2 Cl 2 0.013 〃 HCl 0.37 〃 (other H 2 gas) (2) Gas volume 30 Nm 3 / Hr (3) Circulating fluid volume 4.20 m 3 / Hr (4) PH 10.0 of circulating fluid Under the above conditions, as a result of continuous operation for about 111 hours, Ca (OH) 2
The consumption was 2.1 kg per 100 m 3 of gas, there was no deposit on equipment and devices, stable operation was possible, and the content of each silicon compound in the outlet gas was Trace.
尚、比較試験として上記ガスを従来法で処理した場合、
NaOHの消費量はガス100m3当たり2.5Kgであつた。Incidentally, when the above gas was treated by a conventional method as a comparative test,
The consumption of NaOH was 2.5 kg per 100 m 3 of gas.
従つて、本発明方法によれば従来法に比較し処理費は著
しく低廉である。Therefore, according to the method of the present invention, the processing cost is remarkably low as compared with the conventional method.
図面は本発明を説明するための実施例のフローシート図
である。 １……ジエツトスクラバ、２……循環槽、３……沈降分
離槽、４……ガス導入管、11……ガス取出管、12……PH
検出器The drawings are flow sheet diagrams of embodiments for explaining the present invention. 1 ... Jet scrubber, 2 ... Circulation tank, 3 ... Sedimentation / separation tank, 4 ... Gas introduction pipe, 11 ... Gas extraction pipe, 12 ... PH
Detector
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｂ０１Ｄ 53/77 Ｂ０１Ｄ 53/34 ＺＡＢ (72)発明者 田尻 忠昭 兵庫県神戸市中央区熊内町８丁目４番８号 (56)参考文献 特開 昭60−125229（ＪＰ，Ａ) 特開 昭57−94323（ＪＰ，Ａ)─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification number Internal reference number FI Technical display location B01D 53/77 B01D 53/34 ZAB (72) Inventor Tadaaki Tajiri Kumauchi-machi, Chuo-ku, Kobe-shi, Hyogo 8-4-8 (56) Reference JP-A-60-125229 (JP, A) JP-A-57-94323 (JP, A)
Claims (1)
素化合物の少なくとも１成分を含むガスと、水酸化カル
シウム懸濁水とをPH9.5〜10.5で気液接触させた後、生
成したスラリーを沈降、分離すると共に、その母液に水
酸化カルシウムを添加してPHを調整し循環再使用するこ
とを特徴とする珪素化合物を含むガスの処理方法。1. A gas containing at least one component of a silicon compound such as silane, chlorosilane, and silicon tetrachloride and calcium hydroxide suspension water are brought into gas-liquid contact with PH 9.5 to 10.5, and then the resulting slurry is settled. A method for treating a gas containing a silicon compound, which comprises separating and separating, adding calcium hydroxide to the mother liquor, adjusting the PH, and recirculating and reusing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62046448A JPH0749093B2 (en) | 1987-02-28 | 1987-02-28 | Method for treating gas containing silicon compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62046448A JPH0749093B2 (en) | 1987-02-28 | 1987-02-28 | Method for treating gas containing silicon compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63214321A JPS63214321A (en) | 1988-09-07 |
| JPH0749093B2 true JPH0749093B2 (en) | 1995-05-31 |
Family
ID=12747436
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62046448A Expired - Lifetime JPH0749093B2 (en) | 1987-02-28 | 1987-02-28 | Method for treating gas containing silicon compound |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0749093B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0714452B2 (en) * | 1988-12-08 | 1995-02-22 | 電気化学工業株式会社 | How to treat gas |
| JP4850350B2 (en) * | 2001-05-28 | 2012-01-11 | 株式会社東設 | Toxic gas removal method and apparatus |
| KR100795693B1 (en) | 2005-07-15 | 2008-01-17 | 주식회사 소디프신소재 | Method for Purifying Monosilane |
| DE102010002812A1 (en) * | 2010-03-12 | 2011-09-15 | Wacker Chemie Ag | Process for the disposal of hexachlorodisilane-containing vapors |
| CN103100295B (en) * | 2011-11-11 | 2015-08-12 | 浙江昱辉阳光能源有限公司 | A kind of processing method of sour gas and system thereof |
| DE102013206228A1 (en) | 2013-04-09 | 2014-10-09 | Wacker Chemie Ag | Apparatus and method for the treatment of chlorosilanes containing liquids |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5794323A (en) * | 1980-12-03 | 1982-06-11 | Stanley Electric Co Ltd | Treating method for waste gas of cvd apparatus |
| JPS58128146A (en) * | 1982-01-27 | 1983-07-30 | Nippon Sanso Kk | Absorbing agent |
-
1987
- 1987-02-28 JP JP62046448A patent/JPH0749093B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63214321A (en) | 1988-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4147756A (en) | Combustion gas scrubbing system | |
| CN101700466B (en) | Process for treating residual liquid and tail gas in production of polysilicon by improved Siemens method | |
| US4765805A (en) | Method and apparatus for removing dust and gas pollutants from waste gases, particularly waste gases produced in the manufacture of optical waveguide preforms | |
| US4336232A (en) | Production of purified brine | |
| KR20010093838A (en) | Apparatus and method for point-of-use treatment of effluent gas streams | |
| JPH0749093B2 (en) | Method for treating gas containing silicon compound | |
| KR20030001414A (en) | Method for treating exhaust gas containing fluorine-containing compound | |
| US4490343A (en) | Method for the separation of chlorosilanes from a gaseous mixture containing hydrogen chloride and hydrogen | |
| AU2007221951B2 (en) | Water treatment | |
| US4448682A (en) | Production of purified brine | |
| KR101773276B1 (en) | Apparatus and process for treating liquids containing chlorosilanes | |
| CN214635350U (en) | Device for treating hydrogen fluoride gas | |
| US6054104A (en) | Method and apparatus for germanium reclamation from chemical vapor deposition | |
| AU637686B2 (en) | Process of purifying exhaust gas | |
| JPH05253576A (en) | Treatment of fluorine-containing water | |
| JP5896929B2 (en) | Waste gas treatment system and waste gas treatment method for chlorosilanes | |
| CN218307186U (en) | Washing system | |
| JPH0938463A (en) | Semiconductor manufacturing exhaust gas treatment method | |
| JPS5978942A (en) | Treatment of waste gas in system for manufacturing base material for optical fiber | |
| JPH0677669B2 (en) | Exhaust gas treatment method and apparatus | |
| KR101884156B1 (en) | Removing Method of SiO2 in Semiconductor Process | |
| EP1205564A2 (en) | Method of recovering a copper and/or a manganese component from a particulate gas cleaning agent | |
| CN208244407U (en) | Regenerating active carbon gas preprocessing system device | |
| WO2024075500A1 (en) | Method for separating and regenerating anion exchange resin and cation exchange resin in ion exchange resin mixture | |
| CN109336159A (en) | Acetylene-formaldehyde process produces waste acid treatment technique caused by 1,4- butanediol |