JP2009039605A - Removing method of clo3f - Google Patents

Removing method of clo3f Download PDF

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JP2009039605A
JP2009039605A JP2007204876A JP2007204876A JP2009039605A JP 2009039605 A JP2009039605 A JP 2009039605A JP 2007204876 A JP2007204876 A JP 2007204876A JP 2007204876 A JP2007204876 A JP 2007204876A JP 2009039605 A JP2009039605 A JP 2009039605A
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activated alumina
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JP4952430B2 (en
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Kenji Tanaka
健二 田仲
Isamu Mori
勇 毛利
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Central Glass Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an inexpensive removing method of ClO<SB>3</SB>F which is an impurity in gas. <P>SOLUTION: By reacting active alumina with gas containing ClO<SB>3</SB>F as an impurity, ClO<SB>3</SB>F which is an impurity in gas can be inexpensively removed. Alternatively, by reacting active alumina subjected to dehydration in advance to cause mass reduction by 0.5-15 mass% with gas containing ClO<SB>3</SB>F as an impurity, ClO<SB>3</SB>F which is an impurity in gas can be inexpensively removed. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、ＣｌＯ３Ｆを不純物として含むガス中のＣｌＯ３Ｆを除去する方法に関するものである。 The present invention relates to a method for removing ClO 3 F in a gas containing ClO 3 F as an impurity.

フッ化ペルクロリル（ＣｌＯ３Ｆ）は、一般にアルカリ金属、又はアルカリ土類金属の塩素酸塩とフッ素（Ｆ２）、又はＦ２を含むガスとの反応、あるいはアルカリ金属又はアルカリ土類金属の過塩素酸塩とフッ素化剤［例えば、フルオロ硫酸（ＨＳＯ３Ｆ）など］との反応により生成する。 Perchloryl fluoride (ClO 3 F) is generally a reaction between an alkali metal or alkaline earth metal chlorate and a gas containing fluorine (F 2 ) or F 2 , or an alkali metal or alkaline earth metal reaction. It is formed by a reaction between a chlorate and a fluorinating agent [for example, fluorosulfuric acid (HSO 3 F) etc.

ＣｌＯ３Ｆは、熱的に非常に安定な化合物であり、４７０℃まで加温しないと熱分解しない。また、水に不溶で酸やアルカリで分解できないという特徴がある。さらに、物性がＣｌＯ３Ｆと類似したガス中にＣｌＯ３Ｆが低濃度で含まれる場合には、蒸留による分離や濃縮も難しいため、除去が困難という問題点があった。 ClO 3 F is a thermally very stable compound and does not thermally decompose unless heated to 470 ° C. In addition, it is insoluble in water and cannot be decomposed with acid or alkali. Furthermore, physical properties are ClO 3 F in the gas similar to ClO 3 F when included at a low concentration, since it is also difficult separation and concentration by distillation, removal is disadvantageously difficult.

一般に、ガス中の不純物の除去方法としては、除去したい不純物との熱的安定性の差を利用して不純物を熱分解させ、ガス中の不純物を除去する方法が報告されている（特許文献１）。   In general, as a method for removing impurities in a gas, a method has been reported in which impurities are thermally decomposed by utilizing the difference in thermal stability from the impurities to be removed to remove the impurities in the gas (Patent Document 1). ).

その他、ガス中の不純物の除去方法としては、例えば半導体のクリーニングガスに用いられるＮＦ３の精製にゼオライトなどの精製薬剤を用いた方法が報告されている（非特許文献１）。 In addition, as a method for removing impurities in the gas, for example, a method using a purification agent such as zeolite for purification of NF 3 used for a semiconductor cleaning gas has been reported (Non-patent Document 1).

また、ガス中の不純物として、Ｈ２Ｏ、ＣＯ２、ＮＯ２を除去する方法として活性アルミナを用いた方法が報告されている（特許文献２）が、ＣｌＯ３Ｆを除去する方法として活性アルミナの使用は報告されていない。
特開平１−２６１２１０号公報 特開平５−７８１１７号公報 Ｃｈｅｍ.Ｅｎｇ.８４, １１６, (１９７７) Further, a method using activated alumina as a method for removing H 2 O, CO 2 and NO 2 as impurities in the gas has been reported (Patent Document 2), but activated alumina as a method for removing ClO 3 F. The use of is not reported.
JP-A-1-261210 Japanese Patent Laid-Open No. 5-78117 Chem. Eng. 84, 116, (1977)

上記の熱的安定性の差を利用して不純物を熱分解させる方法において、ＣｌＯ３Ｆは熱的に非常に安定であり、同様に熱的に安定なガス中にＣｌＯ３Ｆが不純物として含まれる場合にはＣｌＯ３Ｆを除去できない。 In the method of thermally decomposing impurities using the above difference in thermal stability, ClO 3 F is thermally very stable, and similarly, ClO 3 F is contained as an impurity in a thermally stable gas. In this case, ClO 3 F cannot be removed.

また、上記のゼオライトなどの精製薬剤を用いる方法においてもＣｌＯ３Ｆを除去できない。 In addition, ClO 3 F cannot be removed even in the above-described method using a purification agent such as zeolite.

すなわち、ＣｌＯ３Ｆの除去方法に関する報告はされていない。 That is, there is no report on a method for removing ClO 3 F.

従って、本発明の課題は、ＣｌＯ３Ｆを除去できる安価な除去方法を提供することである。 Accordingly, an object of the present invention is to provide an inexpensive removal method capable of removing ClO 3 F.

本発明者らは、かかる問題点に鑑み鋭意検討の結果、化学的、熱的に安定なＣｌＯ３Ｆを活性アルミナと反応させ、除去できることを見出した。 As a result of intensive studies in view of such problems, the present inventors have found that chemically and thermally stable ClO 3 F can be removed by reacting with activated alumina.

すなわち、本発明は、ＣｌＯ３Ｆを不純物として含むガスに活性アルミナを反応させることを特徴とするＣｌＯ３Ｆの除去方法を提供するものである。 That is, the present invention provides a method for removing ClO 3 F, characterized by reacting activated alumina with a gas containing ClO 3 F as an impurity.

または、予め０．５〜１５質量％の質量減少を起こすまで脱水処理を施した活性アルミナを使用することを特徴とする上記のＣｌＯ３Ｆの除去方法を提供するものである。 Alternatively, the present invention provides a method for removing ClO 3 F described above, characterized by using activated alumina that has been dehydrated in advance until a mass loss of 0.5 to 15% by mass occurs.

本発明により、ガス中の不純物であるＣｌＯ３Ｆを除去することが可能となる。 According to the present invention, ClO 3 F that is an impurity in a gas can be removed.

以下、本発明の内容を詳細に説明する。   Hereinafter, the contents of the present invention will be described in detail.

使用する活性アルミナは、製法、形状については特に問わないが、比表面積が大きいものを使用する方がＣｌＯ３Ｆの処理量が多くなるため望ましい。また、使用する際には、あらかじめ脱水処理を施すことが望ましい。脱水処理を施さないとＣｌＯ３Ｆの除去量が極端に少なくなる。脱水処理の方法については、特に問わないが、脱水により生じる質量減少が０．５〜１５質量％程度になるまで行ってから使用する方が望ましい。 The activated alumina to be used is not particularly limited in terms of the production method and shape, but it is desirable to use a material having a large specific surface area because the treatment amount of ClO 3 F increases. Moreover, when using, it is desirable to perform a dehydration process beforehand. Without dehydration, the amount of ClO 3 F removed becomes extremely small. The method for the dehydration treatment is not particularly limited, but it is preferable to use the dehydration process after the mass reduction caused by the dehydration is about 0.5 to 15% by mass.

活性アルミナは管に充填して用いる。ＣｌＯ３Ｆを不純物に含んだガスとの接触の方法については、封入法、流通法いずれでも構わない。また、ＣｌＯ３Ｆを不純物に含んだガスは、活性アルミナによって除去されないガス、例えばＮ２、Ｏ２、Ｈｅ、Ａｒ、Ｎｅ、Ｘｅ等の不活性ガスやＳｉＨ４、ＣＨ４、Ｃ２Ｈ６、Ｃ３Ｈ８などの水素化物ガス、ＳｉＦ４、ＧｅＦ４、ＮＦ３、ＳＦ６、ＣＦ４、Ｃ２Ｆ６、Ｃ３Ｆ８などのフッ化物ガスなどが挙げられる。単体でも構わないが、混合ガスでも構わない。さらに、ＣｌＯ３Ｆ以外の不純物については、活性アルミナと直接反応するもの以外のものであれば、含まれていても構わない。しかし、活性アルミナに吸着されるものは、ＣｌＯ３Ｆの処理能力が低下するので、含まれていない方が好ましい。 Activated alumina is used by filling the tube. As a method of contact with a gas containing ClO 3 F as an impurity, either an encapsulation method or a distribution method may be used. A gas containing ClO 3 F as an impurity is a gas that is not removed by activated alumina, for example, an inert gas such as N 2 , O 2 , He, Ar, Ne, or Xe, SiH 4 , CH 4 , or C 2 H 6. Hydride gas such as C 3 H 8 , fluoride gas such as SiF 4 , GeF 4 , NF 3 , SF 6 , CF 4 , C 2 F 6 , and C 3 F 8 . It may be a single substance or a mixed gas. Further, impurities other than ClO 3 F may be included as long as they are other than those that react directly with activated alumina. However, what is adsorbed on the activated alumina is preferably not contained because the treatment capacity of ClO 3 F is lowered.

活性アルミナとの反応温度については、０〜４７０℃が好ましい。低すぎると新たに冷凍機や保冷設備が必要となり、安価に精製することができなくなる。４７０℃を超えるとＣｌＯ３Ｆが熱分解し始めるのでＣｌＯ３Ｆの除去に活性アルミナを用いる必要性がなくなる。 About reaction temperature with activated alumina, 0-470 degreeC is preferable. If it is too low, a new refrigerator and cold insulation equipment will be required, and it will not be possible to purify at low cost. If it exceeds 470 ° C., ClO 3 F begins to thermally decompose, so that it is not necessary to use activated alumina to remove ClO 3 F.

活性アルミナとの反応圧力についても、特に制限はないが、０．２ＭＰａ以下の圧力が操作しやすいので好ましい。   The reaction pressure with activated alumina is not particularly limited, but a pressure of 0.2 MPa or less is preferable because it is easy to operate.

活性アルミナを充填した管中の滞留時間は、１〜６００秒が好ましい。１秒未満では十分な効果が得られないし、６００秒より長くなると圧力損失が増大し、ガスの流れが悪化する。   The residence time in the tube filled with activated alumina is preferably 1 to 600 seconds. If it is less than 1 second, a sufficient effect cannot be obtained, and if it is longer than 600 seconds, the pressure loss increases and the gas flow deteriorates.

以下、実施例により本発明を詳細に説明する。   Hereinafter, the present invention will be described in detail by way of examples.

図１に、本発明を用いた実験の概略系統図を示す。ＣｌＯ３Ｆ除去処理の対象となるＣｌＯ３Ｆ含有ガス１は、ＣｌＯ３ＦをＮ２で希釈したガス（実施例１）、ＣｌＯ３ＦをＣＨ４で希釈したガス（実施例２）、もしくはＣｌＯ３ＦをＮＦ３で希釈したガス（実施例３）を使用する。このガスを、開閉弁９、１１、１２、及び１３を開き、開閉弁１０、１４、及び１５を閉じることにより、活性アルミナを充填した充填管５に導入し接触させ、空容器７に捕集する。空容器７に捕集されたガスを、ＣｌＯ３Ｆの検出下限が０．５ｖｏｌｐｐｍのＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析し、ＣｌＯ３Ｆの濃度を測定する。また、活性アルミナを脱水処理する場合、ドライポンプ８により真空引きする時には、開閉弁１２、及び１４を開き、開閉弁９、１０、１１、１３、及び１５を閉じ、さらに加熱時にヒーター６を用い（実施例１、２、及び３）、Ｎ２パージを行う時には、開閉弁１０、１１、１２、及び１５を開き、開閉弁９、１３、及び１４を閉じ、さらに加熱時にヒーター６を用いて（実施例４）行う。 FIG. 1 shows a schematic system diagram of an experiment using the present invention. ClO 3 F removal ClO 3 F-containing gas 1 to be processed is, ClO 3 F was diluted with N 2 gas (Example 1), ClO 3 F was diluted with CH 4 gas (Example 2), or A gas obtained by diluting ClO 3 F with NF 3 (Example 3) is used. This gas is collected in an empty container 7 by opening and closing the on-off valves 9, 11, 12, and 13 and closing the on-off valves 10, 14, and 15, introducing the gas into the filling tube 5 filled with activated alumina. To do. The gas collected in the empty container 7 is analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.) having a detection lower limit of ClO 3 F of 0.5 volppm, and the concentration of ClO 3 F is measured. When dehydrating activated alumina, when opening the vacuum with the dry pump 8, the on-off valves 12 and 14 are opened, the on-off valves 9, 10, 11, 13, and 15 are closed, and the heater 6 is used for heating. (Examples 1, 2, and 3) When performing N 2 purge, the on-off valves 10, 11, 12, and 15 are opened, the on-off valves 9, 13, and 14 are closed, and the heater 6 is used during heating. (Example 4)

実施例１
活性アルミナを充填した充填管５として、長さ４０ｃｍの２５Ａ管に活性アルミナ（住友化学製、ＫＨＯ−２４）を１４１ｇ充填し、ヒーター６で２５０℃に加熱した状態で２時間ドライポンプ８により真空引きを行うことにより脱水処理を実施し、４．０質量％の質量減少を生じた。この脱水処理を施した活性アルミナを充填した充填管５に、室温、大気圧下において、ＣｌＯ３Ｆ除去処理対象のガスとしてＣｌＯ３Ｆを１４１０ｖｏｌｐｐｍ含むＮ２の流量をマスフローコントローラ４にて５０Ｎｍｌ/ｍｉｎ（充填管滞留時間２３６秒相当）に制御し、活性アルミナを充填した充填管５に流通させ、活性アルミナを充填した充填管５通過後のガスを空容器７に捕集した。 Example 1
As a filling tube 5 filled with activated alumina, 141 g of activated alumina (KHO-24, manufactured by Sumitomo Chemical Co., Ltd.) is filled in a 40 cm long 25A tube, and is heated by a heater 6 to 250 ° C. and vacuumed by a dry pump 8 for 2 hours. The dehydration process was carried out by pulling, resulting in a mass loss of 4.0% by mass. A flow rate of N 2 containing 1410 volppm of ClO 3 F as a gas to be removed with ClO 3 F at a room temperature and atmospheric pressure in a filling tube 5 filled with this dehydrated activated alumina is 50 Nml / It was controlled to min (corresponding to a filling tube residence time of 236 seconds) and circulated through the filling tube 5 filled with activated alumina, and the gas after passing through the filling tube 5 filled with activated alumina was collected in the empty container 7.

その後、捕集したガス中のＣｌＯ３Ｆ濃度をＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析した。その結果、ＣｌＯ３Ｆ濃度は検出下限の０．５ｖｏｌｐｐｍ未満であり、ＣｌＯ３Ｆを除去できることが確認できた。 Thereafter, the ClO 3 F concentration in the collected gas was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.). As a result, the ClO 3 F concentration was less than the lower limit of detection of 0.5 vol ppm, and it was confirmed that ClO 3 F could be removed.

実施例２
ＣｌＯ３Ｆ除去処理対象のガスとして、ＣｌＯ３Ｆを２２８０ｖｏｌｐｐｍ含むＣＨ４を使用する以外は、実施例１と同条件で行った。実施例１と同様に活性アルミナを充填した充填管５を通過後、空容器７に捕集したガス中のＣｌＯ３Ｆ濃度をＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析した。その結果、ＣｌＯ３Ｆ濃度は検出下限の０．５ｖｏｌｐｐｍ未満であり、ＣＨ４中のＣｌＯ３Ｆを除去できることが確認できた。 Example 2
The same conditions as in Example 1 were used except that CH 4 containing 2280 vol ppm of ClO 3 F was used as the gas to be subjected to the ClO 3 F removal treatment. Similarly to Example 1, after passing through the filling tube 5 filled with activated alumina, the ClO 3 F concentration in the gas collected in the empty container 7 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.). As a result, the ClO 3 F concentration was less than the lower detection limit of 0.5 vol ppm, and it was confirmed that ClO 3 F in CH 4 could be removed.

実施例３
ＣｌＯ３Ｆ除去処理対象のガスとして、ＣｌＯ３Ｆを２０５０ｖｏｌｐｐｍ含むＮＦ３使用する以外は、実施例１と同条件で行った。実施例１と同様に活性アルミナを充填した充填管５を通過後、空容器７に捕集したガス中のＣｌＯ３Ｆ濃度をＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析した。その結果、ＣｌＯ３Ｆ濃度は検出下限の０．５ｖｏｌｐｐｍ未満であり、ＮＦ３中のＣｌＯ３Ｆを除去できることが確認できた。 Example 3
As ClO 3 F removal treatment object gas, except that NF 3 used including 2050volppm the ClO 3 F, were carried out under the same conditions as in Example 1. Similarly to Example 1, after passing through the filling tube 5 filled with activated alumina, the ClO 3 F concentration in the gas collected in the empty container 7 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.). As a result, the ClO 3 F concentration was less than the detection lower limit of 0.5 vol ppm, and it was confirmed that ClO 3 F in NF 3 could be removed.

実施例４
活性アルミナの脱水処理として、ヒーター６で１８０℃に加熱した状態で４時間のＮ２パージ（流量１０００Ｎｍｌ/ｍｉｎ）を行い、２．７質量％の質量減少を生じた以外は、実施例１と同条件で行った。実施例１と同様に活性アルミナを充填した充填管５を通過後、空容器７に捕集したガス中のＣｌＯ３Ｆ濃度をＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析した。その結果、ＣｌＯ３Ｆ濃度は検出下限の０．５ｖｏｌｐｐｍ未満であり、Ｎ２パージによる活性アルミナの脱水処理においてもＣｌＯ３Ｆを除去できることが確認できた。 Example 4
As the dehydration treatment of activated alumina, Example 2 was performed except that a N 2 purge (flow rate: 1000 Nml / min) was performed for 4 hours in a state heated to 180 ° C. by the heater 6 and a mass loss of 2.7 mass% was generated. The same conditions were used. Similarly to Example 1, after passing through the filling tube 5 filled with activated alumina, the ClO 3 F concentration in the gas collected in the empty container 7 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.). As a result, the ClO 3 F concentration was less than the lower limit of detection of 0.5 vol ppm, and it was confirmed that ClO 3 F could be removed even in the dehydration treatment of activated alumina by N 2 purge.

実施例５
活性アルミナの脱水処理を行わない以外は、実施例１と同条件で行った。実施例１と同様に活性アルミナを充填した充填管５を通過後、空容器７に捕集したガス中のＣｌＯ３Ｆ濃度をＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析した。その結果、ＣｌＯ３Ｆ濃度は１３０ｖｏｌｐｐｍであり、ＣｌＯ３Ｆを除去できることが確認できた。 Example 5
The same conditions as in Example 1 were followed except that the activated alumina was not dehydrated. Similarly to Example 1, after passing through the filling tube 5 filled with activated alumina, the ClO 3 F concentration in the gas collected in the empty container 7 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.). As a result, the ClO 3 F concentration was 130 vol ppm, and it was confirmed that ClO 3 F could be removed.

比較例１
活性アルミナの代わりにモレキュラーシーブス４Ａ（和光純薬製）を用いる以外は実施例１と同条件で行った。実施例１と同様に脱水処理を施したモレキュラーシーブス４Ａを充填した充填管５を通過後、空容器７に捕集したガス中のＣｌＯ3Ｆ濃度をＦＴ−ＩＲ（大塚電子社製 ＩＧ−１０００）で分析した。その結果、ＣｌＯ3Ｆ濃度は充填管通過前と変化無く、モレキュラーシーブス４ＡではＣｌＯ3Ｆを除去できないことが確認できた。 Comparative Example 1
It carried out on the same conditions as Example 1 except using molecular sieve 4A (made by Wako Purechemical) instead of activated alumina. The ClO 3 F concentration in the gas collected in the empty container 7 after passing through the filling tube 5 filled with the molecular sieves 4A subjected to dehydration treatment in the same manner as in Example 1 was changed to FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.). ). As a result, the ClO 3 F concentration did not change before passing through the filling tube, and it was confirmed that the molecular sieves 4A could not remove ClO 3 F.

上記の測定結果を表１に記載した。   The measurement results are shown in Table 1.

Figure 2009039605
Figure 2009039605

本発明は、例えば塩化物ガス、フッ化物ガスを使用する半導体工場や化学工場などの排出ガスの除害手段として、また、フロンガスや半導体製造用ガスの精製手段として利用可能である。   The present invention can be used, for example, as a means for removing exhaust gas from semiconductor factories and chemical factories using chloride gas and fluoride gas, and as a means for purifying chlorofluorocarbon gas and semiconductor manufacturing gas.

本発明を用いた実験の概略系統図である。It is a general | schematic systematic diagram of the experiment using this invention.

符号の説明Explanation of symbols

１：ＣｌＯ３Ｆを含むガス（Ｎ２、ＣＨ４、またはＮＦ３希釈）
２：Ｎ２ボンベ
３：減圧弁
４：マスフローコントローラ
５：充填管
６：ヒーター
７：空容器
８：ドライポンプ
９〜１５：開閉弁
1: Gas containing ClO 3 F (N 2 , CH 4 , or NF 3 dilution)
2: N 2 cylinder 3: Pressure reducing valve 4: Mass flow controller 5: Filling pipe 6: Heater 7: Empty container 8: Dry pump 9-15: Open / close valve

Claims (2)

ＣｌＯ３Ｆを不純物として含むガスに活性アルミナを反応させることを特徴とするＣｌＯ３Ｆの除去方法。 A method for removing ClO 3 F, comprising reacting activated alumina with a gas containing ClO 3 F as an impurity. 予め０．５〜１５質量％の質量減少を起こすまで脱水処理を施した活性アルミナを使用することを特徴とする請求項1に記載のＣｌＯ３Ｆの除去方法。
2. The method for removing ClO 3 F according to claim 1, wherein activated alumina which has been subjected to dehydration treatment in advance until mass reduction of 0.5 to 15% by mass is caused in advance.
JP2007204876A 2007-08-07 2007-08-07 Removal method of ClO3F Expired - Fee Related JP4952430B2 (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04122420A (en) * 1989-12-07 1992-04-22 Man Technol Gmbh Method and device for removing fluorine and/or inorganic fluoride
JP2000086236A (en) * 1998-09-17 2000-03-28 Mizusawa Ind Chem Ltd Acidic activated alumina and its production
JP2000319433A (en) * 1999-05-07 2000-11-21 Mitsubishi Chemicals Corp Apparatus for surface treatment using fluorine gas
JP2007508383A (en) * 2003-10-17 2007-04-05 ライオンデル ケミカル テクノロジー、 エル．ピー． Purification of tertiary butyl alcohol

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04122420A (en) * 1989-12-07 1992-04-22 Man Technol Gmbh Method and device for removing fluorine and/or inorganic fluoride
JP2000086236A (en) * 1998-09-17 2000-03-28 Mizusawa Ind Chem Ltd Acidic activated alumina and its production
JP2000319433A (en) * 1999-05-07 2000-11-21 Mitsubishi Chemicals Corp Apparatus for surface treatment using fluorine gas
JP2007508383A (en) * 2003-10-17 2007-04-05 ライオンデル ケミカル テクノロジー、 エル．ピー． Purification of tertiary butyl alcohol

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