JP2001017831A - Treating agent for halogen gas - Google Patents
Treating agent for halogen gasInfo
- Publication number
- JP2001017831A JP2001017831A JP11192786A JP19278699A JP2001017831A JP 2001017831 A JP2001017831 A JP 2001017831A JP 11192786 A JP11192786 A JP 11192786A JP 19278699 A JP19278699 A JP 19278699A JP 2001017831 A JP2001017831 A JP 2001017831A
- Authority
- JP
- Japan
- Prior art keywords
- halogen gas
- treating agent
- inorganic compound
- agent
- reducing agent
- 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.)
- Granted
Links
Landscapes
- Treating Waste Gases (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Drying Of Semiconductors (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は半導体製造時に使用
するハロゲン原子含有ガス等の製造工程時や半導体製造
工程で排出される排ガス中のハロゲンガスを効率的に除
去するに適した処理剤に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a treating agent suitable for efficiently removing halogen gas contained in exhaust gas discharged during a manufacturing process of a halogen atom-containing gas or the like used in semiconductor manufacturing or in a semiconductor manufacturing process.
【0002】[0002]
【従来の技術】従来、ガス中に含まれるハロゲンガスを
除去する手段としては、スクラバ−、スプレー塔、回転
式微細気泡発生装置などを用い、これらのガスを水酸化
ナトリウムなどのアルカリ水溶液と接触させて吸収させ
る湿式法や、塩素等のハロゲンガスを活性炭、ゼオライ
ト、アルミナなどに吸着させたり、カルシウム化合物な
どと接触させて反応除去する乾式法が知られている。2. Description of the Related Art Conventionally, as a means for removing a halogen gas contained in a gas, a scrubber, a spray tower, a rotary fine bubble generator or the like is used, and these gases are brought into contact with an aqueous alkali solution such as sodium hydroxide. There are known a wet method in which a halogen gas such as chlorine is adsorbed on activated carbon, zeolite, alumina, or the like, or a dry method in which a halogen gas such as chlorine is brought into contact with a calcium compound or the like to be reacted and removed.
【0003】[0003]
【発明が解決しようとする課題】しかしながら湿式法
は、一般に後処理に難点がある上装置が複雑で大型にな
るばかりではなく、設備、保守ともに多額の費用を要す
るという欠点がある。一方乾式法も、活性炭、ゼオライ
ト、アルミナのような吸着を利用して排ガス中の塩素等
のハロゲンガスを除去する方法では、吸着と同時に脱離
も起こるので有害成分が下流側にリ−クするという欠点
がある。更に、活性炭の場合には、フッ素などの反応性
のきわめて高いガスを処理する場合には火災の危険性も
ある。However, the wet method generally has disadvantages in post-treatment, and is not only complicated and large-sized, but also requires a large amount of equipment and maintenance. On the other hand, in the dry method, the method of removing halogen gas such as chlorine in exhaust gas by using adsorption such as activated carbon, zeolite and alumina also causes desorption at the same time as adsorption, so harmful components leak downstream. There is a disadvantage that. Further, in the case of activated carbon, there is a danger of fire when treating extremely reactive gas such as fluorine.
【0004】また、カルシウム化合物などを主成分とし
た処理剤の場合は、ハロゲンガスを除去する能力は十分
ではない。従って、半導体製造プロセスから排出される
ようなハロゲンガスに対して除去能力が高いだけでな
く、脱離して下流側にリークするということがない上、
除去の際における火災などの危険性がない除去剤の出現
が望まれていた。[0004] In the case of a treating agent containing a calcium compound or the like as a main component, the ability to remove halogen gas is not sufficient. Therefore, not only is the removal capability of the halogen gas discharged from the semiconductor manufacturing process high, but also it does not desorb and leak downstream.
There has been a demand for the emergence of a remover that does not have a risk of fire or the like during removal.
【0005】そこで本発明者等は、安全で除去効率が良
い上、下流側にリークする恐れのないハロゲンガスの除
去剤について種種検討した結果、硫黄系還元剤を、特定
の固体金属の酸化物、水酸化物、又は炭酸塩と共に使用
する処理剤が、ハロゲンガスに対して脱離を起こすこと
のない、化学反応によってハロゲンを固定化することが
できる上除去能力が高いことを見出し、本発明を完成し
た。従って本発明の目的は、安全で除去効率が高いだけ
でなく、下流側にリークする恐れのない、ハロゲンガス
の除去剤を提供することにある。The inventors of the present invention have conducted various studies on a halogen gas remover which is safe and has high removal efficiency and does not leak to the downstream side. As a result, the sulfur-based reducing agent is converted to a specific solid metal oxide. The present invention has found that a treating agent used together with a hydroxide, a hydroxide, or a carbonate can immobilize halogen by a chemical reaction without causing desorption to a halogen gas and has a high removal ability. Was completed. Accordingly, an object of the present invention is to provide a halogen gas remover that is not only safe and has high removal efficiency but also does not leak downstream.
【0006】[0006]
【課題を解決するための手段】本発明の上記の目的は、
固体金属の酸化物、水酸化物及び炭酸塩の中から選択さ
れた少なくとも1種の無機化合物及び必要に応じて添加
された成形助剤とからなる基材に、硫黄原子を含有する
還元剤を含有せしめてなることを特徴とするハロゲンガ
ス用処理剤によって達成された。SUMMARY OF THE INVENTION The above objects of the present invention are as follows.
A reducing agent containing a sulfur atom is added to a substrate comprising at least one inorganic compound selected from oxides, hydroxides and carbonates of solid metals and a molding aid added as necessary. The present invention has been attained by a halogen gas treating agent which is characterized by being contained.
【0007】[0007]
【発明の実施の形態】本発明における固体金属の酸化
物、水酸化物、炭酸塩とは、アルカリ土類金属、Fe、
Co、Ni、Zn、Mn、Cu(I)の中から選択され
る少なくとも1種の金属の酸化物、水酸化物、炭酸塩な
どの無機化合物である。本発明のおいてはこれらの無機
化合物に、必要に応じ、更にクレイ等の成形助剤を混合
して成形することが好ましい。このような、前記無機化
合物と成形助剤からなる基材中の前期無機化合物の含有
量は、5〜100重量%であることが好ましく特に20
〜80重量%であることが好ましい。前記成形助剤は本
業界で公知のものの中から適宜選択することができる
が、例えば、ベントナイトやカオリンなどのクレイが使
用できる。BEST MODE FOR CARRYING OUT THE INVENTION The oxides, hydroxides and carbonates of solid metals in the present invention are defined as alkaline earth metals, Fe,
Inorganic compounds such as oxides, hydroxides, and carbonates of at least one metal selected from Co, Ni, Zn, Mn, and Cu (I). In the present invention, it is preferable that a molding aid such as clay is further mixed with these inorganic compounds, if necessary, for molding. The content of the inorganic compound in the base material comprising the inorganic compound and the molding aid is preferably 5 to 100% by weight, and particularly preferably 20 to 100% by weight.
Preferably it is ~ 80% by weight. The molding aid can be appropriately selected from those known in the art. For example, clay such as bentonite and kaolin can be used.
【0008】本発明における硫黄原子を含有する還元剤
の例としては、亜硫酸塩、亜二チオン酸塩、四チオン酸
塩、チオ硫酸塩を挙げることができる。これらの還元剤
は単独で使用することも、2種以上を併用することがで
きる。還元剤の使用量は、成形助剤を除く、前記基材の
中の無機化合物100重量部に対して1から120重量
部、好ましくは10から80重量部である。この還元剤
は、X2+H2O→HX+HXOの反応で発生するHX
Oを還元してX−を生成させることにより、上記反応の
進行を促進させるものである。[0008] Examples of the reducing agent containing a sulfur atom in the present invention include sulfite, dithionite, tetrathionate and thiosulfate. These reducing agents can be used alone or in combination of two or more. The amount of the reducing agent to be used is 1 to 120 parts by weight, preferably 10 to 80 parts by weight, based on 100 parts by weight of the inorganic compound in the base material, excluding the molding aid. This reducing agent is HX generated by the reaction of X 2 + H 2 O → HX + HXO.
By reducing O to generate X − , the progress of the above reaction is promoted.
【0009】本発明の処理剤の形状やサイズはその使用
形態により適宜選択することができるが、一般的には直
径が1〜6mmで長さが3〜20mm程度の円柱状ペレット
が好適に用いられる。しかしながら、当然これに限定さ
れるわけではなく、種々の異形状のペレット、錠剤形
状、顆粒状及び破砕粒状、または噴霧乾燥による微粒子
状などとすることもできる。The shape and size of the treating agent of the present invention can be appropriately selected according to the form of use, but generally, cylindrical pellets having a diameter of 1 to 6 mm and a length of about 3 to 20 mm are preferably used. Can be However, the present invention is not limited to this, and may be variously shaped pellets, tablets, granules and crushed granules, or fine particles formed by spray drying.
【0010】例えば、一般的な押出円柱状ペレットを製
造する場合には、所定量の水酸化カルシウムとベントナ
イト粉末をニ−ダ−等の混合混練装置で十分に乾式混合
した後に、混合粉末1重量部に対して0.2〜0.5重
量部の、好ましくは0.3〜0.4重量部の水を添加し
て混練する。水を添加する際には混合物が不均一となら
ないように分割投入することが望ましい。For example, when manufacturing a general extruded cylindrical pellet, a predetermined amount of calcium hydroxide and bentonite powder are thoroughly dry-mixed with a kneading device such as a kneader or the like, and then 1 weight of the mixed powder is added. 0.2 to 0.5 part by weight, preferably 0.3 to 0.4 part by weight of water is added to the mixture and kneaded. When adding water, it is desirable to divide the mixture so that the mixture is not uneven.
【0011】得られた混合物を押出成形機あるいはペレ
タイザ−で、所定の形状のダイスを用いて円柱状ペレッ
トに成形する。これを通常の空気雰囲気下の80〜40
0℃、好ましくは100〜300℃の温度で乾燥する。
次いで、亜硫酸ナトリウム等の還元剤を少なくとも1種
溶解した水溶液をペレットに含浸させて、再度、100
℃で乾燥する。The obtained mixture is formed into cylindrical pellets using an extruder or a pelletizer using a die having a predetermined shape. This is carried out under a normal air atmosphere at 80 to 40
Dry at a temperature of 0 ° C, preferably 100-300 ° C.
Next, the pellet is impregnated with an aqueous solution in which at least one reducing agent such as sodium sulfite is dissolved,
Dry at ℃.
【0012】本発明の処理剤の製造方法は、上記の方法
に限定されるわけではなく、例えば、必要に応じて添加
した成形助剤と固体金属酸化物等の乾燥均一混合物に、
硫黄原子含有還元剤の適当な濃度の水溶液を添加混錬し
た後、120℃以下で乾燥し、乾燥物を粉砕して製造す
ることもできる。The method for producing the treating agent of the present invention is not limited to the above-described method. For example, a dry uniform mixture of a molding aid added as necessary and a solid metal oxide may be used.
After adding and kneading an aqueous solution of an appropriate concentration of a sulfur atom-containing reducing agent, the mixture can be dried and dried at a temperature of 120 ° C. or lower, and the dried product can be pulverized to produce a product.
【0013】本発明の処理剤の使用方法は特に限定され
るものではなく、移動床や流動床に使用することもでき
るが通常は固定床に使用する。例えば円筒内に充填し、
これにハロゲンガスを含有する排気ガスを流通させ、排
気ガス中のハロゲンガスを安全且つ効率良く除去するこ
とができる。The method of using the treating agent of the present invention is not particularly limited, and it can be used for a moving bed or a fluidized bed, but is usually used for a fixed bed. For example, filling in a cylinder,
Exhaust gas containing halogen gas is allowed to flow through this, and halogen gas in the exhaust gas can be safely and efficiently removed.
【0014】[0014]
【発明の効果】本発明の処理剤は、低濃度の乾燥ガス中
から安全且つ効率良くハロゲンガスを除去することがで
きるので、大気中に排出する直前の排気ガスの処理に特
に有用である。以下、本発明を実施例によって更に詳述
するが、本発明はこれによって限定されるものではな
い。The treating agent of the present invention can safely and efficiently remove a halogen gas from a dry gas having a low concentration, and is particularly useful for treating exhaust gas immediately before being discharged into the atmosphere. Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited thereto.
【0015】[0015]
【実施例】排ガス中の塩素除去試験 後記する各処理剤10mlを直径15mmの容器に充填
し、塩素ガスを1%含有する乾燥窒素を、20℃の常圧
下にて、35ml/分の流速で流通させ、除去能力が低
下して下流側の塩素が1ppmに達するに至るまでの時
間を測定した。ガス中の塩素濃度をガス検知管(ガステ
ック(株)製)及びガス検知器(ガステック製、GCL
−1A)で測定した。測定終了後に窒素でパ−ジした後
の、処理剤の初期重量に対する重量変化率から吸収した
塩素量を求めると共に、吸収した塩素が脱離するか否か
を確認した。【Example】Removal test of chlorine in exhaust gas Fill 10ml of each treatment agent to be described later into a 15mm diameter container
And dry nitrogen containing 1% chlorine gas at a normal pressure of 20 ° C.
Flow at a flow rate of 35 ml / min.
Down to the point where chlorine on the downstream side reaches 1 ppm
The interval was measured. The chlorine concentration in the gas is measured by a gas detector
GCL) and gas detector (GCL, GCL)
-1A). After purging with nitrogen after completion of measurement
Was absorbed from the rate of change in weight with respect to the initial weight of the treating agent.
Determine the amount of chlorine and determine if the absorbed chlorine is desorbed
It was confirmed.
【0016】実施例1.市販の消石灰300g、ベント
ナイト50g及びイオン交換水150gを混練機でよく
混合した後、得られたウェットケ−キを1.6mmφの
ペレット状に押出成形し、乾燥機中で、270℃で8時
間乾燥を行って基材のペレットを調製した。次いで、得
られたペレットに30重量%の亜硫酸ナトリウム水溶液
を含浸させ、乾燥機中で、100℃で8時間乾燥を行っ
て本発明の処理剤を調製した。Embodiment 1 FIG. After thoroughly mixing 300 g of commercially available slaked lime, 50 g of bentonite and 150 g of ion-exchanged water with a kneader, the obtained wet cake is extruded into pellets of 1.6 mmφ and dried in a dryer at 270 ° C. for 8 hours. Was performed to prepare pellets of the substrate. Next, the obtained pellets were impregnated with a 30% by weight aqueous solution of sodium sulfite, and dried in a dryer at 100 ° C. for 8 hours to prepare a treating agent of the present invention.
【0017】実施例2.消石灰の代りに市販のアルミナ
300gを用いた他は実施例1と全く同様にして、本発
明の処理剤を調製した。 実施例3.消石灰の代りに市販の酸化亜鉛300gを用
いた他は実施例1と全く同様にして、本発明の処理剤を
調製した。 実施例4.亜硫酸ナトリウムの代りに亜二チオン酸ナト
リウムを用いた他は実施例1と全く同様にして、本発明
の処理剤を調製した。 実施例5.亜硫酸ナトリウムの代りにチオ硫酸ナトリウ
ムを用いた他は実施例1と全く同様にして、本発明の処
理剤を調製した。 比較例1.市販のモレキュラ−シ−ブ13X(2から3m
mの球状)を処理剤として用いた。 比較例2.市販の活性炭(2から3mmの顆粒)を処理
剤として用いた。 比較例3.亜硫酸水溶液を含浸させなかった他は実施例
1と全く同様にして作製した基材ペレットを処理剤とし
て用いた。Embodiment 2 FIG. A treating agent of the present invention was prepared in exactly the same manner as in Example 1 except that 300 g of commercially available alumina was used instead of slaked lime. Embodiment 3 FIG. A treating agent of the present invention was prepared in exactly the same manner as in Example 1 except that 300 g of commercially available zinc oxide was used instead of slaked lime. Embodiment 4. FIG. A treating agent of the present invention was prepared in exactly the same manner as in Example 1 except that sodium dithionite was used instead of sodium sulfite. Embodiment 5 FIG. A treating agent of the present invention was prepared in exactly the same manner as in Example 1 except that sodium thiosulfate was used instead of sodium sulfite. Comparative Example 1 Commercial molecular sieve 13X (2 to 3 m
m spherical) was used as a treating agent. Comparative Example 2. Commercially available activated carbon (2-3 mm granules) was used as a treatment. Comparative Example 3 A substrate pellet prepared in exactly the same manner as in Example 1 except that the aqueous solution of sulfurous acid was not impregnated was used as a treating agent.
【0018】各処理剤を用いて排ガス中の塩素処理能力
試験を行った結果は表1に示した通りである。Table 1 shows the results of a test of the ability to treat chlorine in exhaust gas using each treating agent.
【表1】 表1の結果から明らかな如く、本発明の処理剤が、安全
且つ確実に塩素を除去することができること、及び、処
理剤としての寿命が長いことが実証された。[Table 1] As is clear from the results in Table 1, it has been proved that the treatment agent of the present invention can safely and reliably remove chlorine and has a long life as a treatment agent.
───────────────────────────────────────────────────── フロントページの続き Fターム(参考) 4D002 AA17 AA18 AC10 BA03 BA06 CA07 DA04 DA05 DA11 DA12 DA13 DA16 DA21 DA46 DA47 DA70 EA02 GA01 GA02 GB01 GB02 GB03 GB08 GB11 GB12 GB20 4G066 AA15B AA16B AA18B AA20C AA26B AA27B AA45D AA47D AA64C AE19C CA31 DA02 FA27 FA37 5F004 AA16 BC02 BC08 DA00 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4D002 AA17 AA18 AC10 BA03 BA06 CA07 DA04 DA05 DA11 DA12 DA13 DA16 DA21 DA46 DA47 DA70 EA02 GA01 GA02 GB01 GB02 GB03 GB08 GB11 GB12 GB20 4G066 AA15B AA16B AA18B AA20C AA26AAAAAAE CA31 DA02 FA27 FA37 5F004 AA16 BC02 BC08 DA00
Claims (5)
の中から選択された少なくとも1種の無機化合物及び必
要に応じて添加された成形助剤とからなる基材に、硫黄
原子を含有する還元剤を含有せしめてなることを特徴と
するハロゲンガス用処理剤。A substrate comprising at least one inorganic compound selected from oxides, hydroxides and carbonates of a solid metal, and a molding aid optionally added, is provided with a sulfur atom. A treating agent for halogen gas, characterized by containing a reducing agent.
リ土類金属、Fe、Co、Ni、Zn、Mn、Cu
(I)の中から選択された少なくとも1種の金属であ
る、請求項1に記載されたハロゲンガス用処理剤。2. The method according to claim 1, wherein the metal element constituting the base material is an alkaline earth metal, Fe, Co, Ni, Zn, Mn, Cu
The halogen gas treating agent according to claim 1, which is at least one metal selected from (I).
塩、四チオン酸塩、及びチオ硫酸塩の中から選択された
少なくとも1種類である、請求項1又は2に記載された
ハロゲンガス用処理剤。3. The halogen according to claim 1, wherein the reducing agent is at least one selected from a sulfite, a dithionate, a tetrathionate, and a thiosulfate. Gas treatment agent.
酸化物、炭酸塩の総含有量が、該基材の5〜100重量
%である、請求項1〜3の何れかに記載されたハロゲン
ガス用処理剤。4. The method according to claim 1, wherein the total content of solid metal oxides, hydroxides, and carbonates in the substrate is 5 to 100% by weight of the substrate. Treatment agent for halogen gas.
化合物100重量部に対して1〜120重量部である、
請求項1〜4の何れかに記載されたハロゲンガス用処理
剤。5. The content of the reducing agent in the treating agent is 1 to 120 parts by weight based on 100 parts by weight of the inorganic compound.
The halogen gas treating agent according to claim 1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19278699A JP4913271B2 (en) | 1999-07-07 | 1999-07-07 | Halogen gas treatment agent |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19278699A JP4913271B2 (en) | 1999-07-07 | 1999-07-07 | Halogen gas treatment agent |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2001017831A true JP2001017831A (en) | 2001-01-23 |
JP4913271B2 JP4913271B2 (en) | 2012-04-11 |
Family
ID=16296984
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---|---|---|---|
JP19278699A Expired - Lifetime JP4913271B2 (en) | 1999-07-07 | 1999-07-07 | Halogen gas treatment agent |
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Cited By (11)
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WO2007135823A1 (en) | 2006-05-19 | 2007-11-29 | Asahi Glass Company, Limited | Method of removing halogen gas and remover for halogen gas |
JP2010064040A (en) * | 2008-09-12 | 2010-03-25 | Asahi Glass Co Ltd | Halogen gas removing agent and method for removing halogen gas |
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JP2015112545A (en) * | 2013-12-12 | 2015-06-22 | 宇部興産株式会社 | Gas treatment device and gas treatment cartridge |
JP2015112546A (en) * | 2013-12-12 | 2015-06-22 | 宇部興産株式会社 | Gas treatment device and gas treatment cartridge |
JP2015112547A (en) * | 2013-12-12 | 2015-06-22 | 宇部興産株式会社 | Gas treatment device and gas treatment cartridge |
JP2018126679A (en) * | 2017-02-07 | 2018-08-16 | クラリアント触媒株式会社 | Remover of halogen gas, manufacturing method therefor, halogen gas removal method using the same and system for removing halogen gas |
JP2019122906A (en) * | 2018-01-15 | 2019-07-25 | 宇部興産株式会社 | Gas processing device |
JP2020018953A (en) * | 2018-07-30 | 2020-02-06 | クラリアント触媒株式会社 | Halogen gas remover and manufacturing method therefor, and method for monitoring consumption state of remover |
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