JPH0632601A - Purification of hydrogen bromide - Google Patents
Purification of hydrogen bromideInfo
- Publication number
- JPH0632601A JPH0632601A JP4190488A JP19048892A JPH0632601A JP H0632601 A JPH0632601 A JP H0632601A JP 4190488 A JP4190488 A JP 4190488A JP 19048892 A JP19048892 A JP 19048892A JP H0632601 A JPH0632601 A JP H0632601A
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen bromide
- zeolite
- valve
- gas
- crude
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/09—Bromine; Hydrogen bromide
- C01B7/093—Hydrogen bromide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、臭化水素の精製法に関
する。FIELD OF THE INVENTION The present invention relates to a method for purifying hydrogen bromide.
【０００２】[0002]
【従来の技術・問題点】臭化水素は、従来より各種の有
機、無機ブロマイド、及びビタミン、鎮静剤など医薬品
合成の原料として用途が確立されているが、近年、半導
体分野においてもドライエッチング剤としてその特性が
認められ、フロン代替候補にも挙げられるなど、急速に
その用途は広まりつつある。臭化水素は、工業的に水素
と臭素の燃焼反応により製造されているが、粗生成物に
は製造工程から混入、溶解した二酸化炭素、塩化水素、
窒素、酸素が少量含まれている。しかし、これら不純物
の存在はエッチング特性に悪影響を及ぼすため、半導体
用としてはこれらを極力除去した高品質のものが要求さ
れている。従来より粗臭化水素の精製方法として知られ
ているものは、不純物が臭素、水分、硫黄化合物、有機
化合物の場合に限られており、二酸化炭素、塩化水素、
窒素、酸素の除去法は知られていなかった。[Prior Art and Problems] Hydrogen bromide has been conventionally used as a raw material for synthesizing pharmaceuticals such as various organic and inorganic bromides, vitamins and sedatives, but in recent years, it has also been used as a dry etching agent in the semiconductor field. Its characteristics are recognized as, and it is also listed as a CFC substitute candidate, and its applications are rapidly spreading. Hydrogen bromide is industrially produced by the combustion reaction of hydrogen and bromine, but the crude product is mixed from the production process, dissolved carbon dioxide, hydrogen chloride,
It contains a small amount of nitrogen and oxygen. However, since the presence of these impurities adversely affects the etching characteristics, it is required for semiconductors to have high quality by removing them as much as possible. Conventionally known as a method for purifying crude hydrogen bromide, impurities are limited to bromine, water, sulfur compounds, organic compounds, carbon dioxide, hydrogen chloride,
The method of removing nitrogen and oxygen was not known.
【０００３】[0003]
【発明が解決しようとする課題】従って、本発明の目的
は、上記の問題点を解決し、半導体分野に使用できる高
純度臭化水素を得るための簡便な精製法を提供すること
にある。SUMMARY OF THE INVENTION Therefore, an object of the present invention is to solve the above problems and provide a simple purification method for obtaining high-purity hydrogen bromide which can be used in the field of semiconductors.
【０００４】[0004]
【課題を解決するための手段】即ち、本発明に係る臭化
水素の精製法は、粗臭化水素をゼオライトに接触させる
ことを特徴とするものである。That is, the method for purifying hydrogen bromide according to the present invention is characterized in that crude hydrogen bromide is brought into contact with zeolite.
【０００５】以下に、本発明を更に詳しく説明する。本
発明に使用できるゼオライトは、Ａ型、モルデナイト
型、チャバザイト型などが挙げられる。これらはモレキ
ュラーシーブスとして各種市販されており、例えば米国
のユニオンカーバイド社からＡ型として３Ａ、４Ａ、５
Ａ、モルデナイト型としてＡＷ−３００、チャバザイト
型としてＡＷ−５００などが商品化されており、同じく
ノートン社からモルデナイト型としてゼオロン１００、
２００、３００、９００、チャバザイト型としてゼオロ
ン５００が商品化されている。The present invention will be described in more detail below. Zeolites that can be used in the present invention include A type, mordenite type and chabazite type. Various types of these are commercially available as molecular sieves, for example, type A, 3A, 4A, 5 from Union Carbide Corporation of the United States.
A, AW-300 as a mordenite type, AW-500 as a chabazite type have been commercialized, and Zeolone 100 as a mordenite type from Norton,
Zeolon 500 has been commercialized as 200, 300, 900, and chabazite type.
【０００６】これらは使用する前に３００〜４００℃で
加熱処理を行って活性化することが必要である。ただ
し、加熱処理後、冷却中に大気と接触させないようにす
ることが肝要である。湿気を吸着すると本発明の効果は
著しく損なわれるため、取り扱いは乾燥した不活性ガス
中で行わねばならない。Before using these, it is necessary to perform heat treatment at 300 to 400 ° C. to activate them. However, it is important not to contact with the atmosphere during cooling after the heat treatment. Since the effect of the present invention is significantly impaired when moisture is adsorbed, it must be handled in a dry inert gas.
【０００７】以下、添付図面に基づいて本発明方法を更
に説明する。図１は本発明の実施例で使用する精製テス
トラインのブロック図である。操作はまず粗臭化水素容
器バルブ(2)、ガスクロマトグラフサンプリングバルブ
(6)、排気口バルブ(11)を閉止し、バルブ(10)から真空
に引いてラインの脱気を行う。必要に応じてゼオライト
充填塔(4)は冷却器(5)により所定温度に調節する。ゼオ
ライト充填塔(4)の温度は不純物として二酸化炭素、塩
化水素の除去の場合には常温で充分効果があるが、それ
に加えて更に窒素あるいは酸素の除去を目的とする場合
は、−５０〜０℃の低温下、好ましくは−１５〜−５０
℃に設定するのが効果的である。もちろん、この温度範
囲では二酸化炭素、塩化水素も充分除去できるため、も
とより低温設定すれば良いが、酸素及び窒素の除去を目
的としない場合には特別な温度設定を必要とせず、すな
わち通常は１５〜２５℃の常温を目安にするものの、こ
の範囲に温度を限定する必要はない。The method of the present invention will be further described below with reference to the accompanying drawings. FIG. 1 is a block diagram of a purification test line used in an embodiment of the present invention. First, operate the crude hydrogen bromide container valve (2) and the gas chromatograph sampling valve.
(6) Close the exhaust port valve (11) and draw vacuum from the valve (10) to evacuate the line. If necessary, the zeolite packed column (4) is adjusted to a predetermined temperature by the cooler (5). The temperature of the zeolite packed column (4) is sufficiently effective at room temperature in the case of removing carbon dioxide and hydrogen chloride as impurities, but in addition to that, in the case of further removing nitrogen or oxygen, it is -50 to 0. At a low temperature of ℃, preferably -15 to -50
It is effective to set at ℃. Of course, since carbon dioxide and hydrogen chloride can be sufficiently removed in this temperature range, it is sufficient to set a low temperature, but when the purpose is not to remove oxygen and nitrogen, no special temperature setting is required, that is, normally 15 Although the normal temperature of -25 ° C is a standard, it is not necessary to limit the temperature to this range.
【０００８】ただし、ライン内の臭化水素圧は３０気圧
を越えると精製効果が落ちてくる傾向があるため、圧力
計(3)にて監視する。ゼオライト充填塔(4)の設定温度及
びライン周囲の気温上昇等により内圧が高くならないよ
うに注意しなければならない。However, if the hydrogen bromide pressure in the line exceeds 30 atm, the refining effect tends to deteriorate, so the pressure gauge (3) is used for monitoring. Care must be taken not to increase the internal pressure due to the set temperature of the zeolite packed tower (4) and the temperature rise around the line.
【０００９】脱気後はバルブ(10)を閉止し、粗臭化水素
容器バルブ(2)を開けて粗臭化水素をライン内に満た
し、一旦流量調整用バルブ(8)を閉止する。その後、排
気口バルブ(11)を開けてバルブ(10)より不活性ガスをパ
ージしながら流量調整用バルブ(8)により粗臭化水素を
所定流量にして流す。After deaeration, the valve (10) is closed, the crude hydrogen bromide container valve (2) is opened to fill the line with crude hydrogen bromide, and the flow rate adjusting valve (8) is once closed. Then, the exhaust port valve (11) is opened, and while purging the inert gas through the valve (10), crude hydrogen bromide is flowed at a predetermined flow rate by the flow rate adjusting valve (8).
【００１０】不活性ガスのパージは大気の逆流を防ぐ意
味で重要な操作であり、窒素、アルゴンあるいはヘリウ
ムなどを精製操作中は常時流しておくのが良い。なお、
図１は精製テストラインで、ガスクロマトグラフサンプ
リングバルブ(6)で精製された臭化水素を分析・評価す
ることを目的としているため、排気口バルブ(11)から排
出されるガスが不活性ガスと臭化水素の混合物となって
も特に問題はない。Purging with an inert gas is an important operation in the sense of preventing backflow of the atmosphere, and it is preferable that nitrogen, argon, helium, or the like be always flowed during the refining operation. In addition,
Figure 1 is a purification test line, which aims to analyze and evaluate hydrogen bromide purified by the gas chromatograph sampling valve (6), so the gas discharged from the exhaust port valve (11) is an inert gas. There is no particular problem even if it becomes a mixture of hydrogen bromide.
【００１１】臭化水素の流量は不純物の吸着速度、精製
物の生産性を考慮して本発明の場合、空間速度(ＳＶ)を
８００〜１０００時間-1にするのが適当であり、また、
８００〜８８０時間-1がより好適である。In the case of the present invention, it is appropriate that the flow rate of hydrogen bromide is such that the space velocity (SV) is 800 to 1000 hours -1 in consideration of the adsorption rate of impurities and the productivity of purified products.
800 to 880 hours- 1 is more preferable.
【００１２】上述の操作により、ゼオライト処理した臭
化水素中の二酸化炭素、塩化水素、酸素及び窒素の濃度
をそれぞれ１ｐｐｍ以下にすることが可能となる。分析
チェックは二酸化炭素、酸素及び窒素の場合、ガスクロ
マトグラフサンプリングバルブ(6)よりガスクロマトグ
ラフ(7)に必要量分取して行い、塩化水素は排気口バル
ブ(11)よりサンプリングしてイオンクロマトグラフを用
いて行った。これら分析を精製中適時行うことにより、
不純物の破過点を求めることができる。By the above operation, it becomes possible to reduce the concentration of carbon dioxide, hydrogen chloride, oxygen and nitrogen in the hydrobromide treated with zeolite to 1 ppm or less, respectively. In the case of carbon dioxide, oxygen and nitrogen, the analysis check is carried out by collecting the required amount in the gas chromatograph (7) from the gas chromatograph sampling valve (6), and the hydrogen chloride is sampled from the exhaust port valve (11) to the ion chromatograph. Was performed using. By performing these analyzes in a timely manner during purification,
The breakthrough point of impurities can be obtained.
【００１３】破過した後のゼオライトの再生法は、一般
に良く知られている圧力スイングサイクルの方法が適用
できる。即ち、ライン内の臭化水素圧をパージした後、
１００ｍｍＨｇ以下の減圧処理を施せば、効率よく吸着
不純物を脱着することができる。この方法だと、再生の
ための加熱と再生後の冷却が不必要であるためゼオライ
トの吸着能力保持の寿命も長くなり、また、非常に短い
サイクルで再生を完了することが可能となる。As a method for regenerating zeolite after breakthrough, a generally well-known pressure swing cycle method can be applied. That is, after purging the hydrogen bromide pressure in the line,
Adsorbed impurities can be desorbed efficiently by applying a reduced pressure treatment of 100 mmHg or less. According to this method, since heating for regeneration and cooling after regeneration are unnecessary, the life of retaining the adsorption capacity of zeolite is extended, and regeneration can be completed in a very short cycle.
【００１４】[0014]
実施例１ 充分乾燥した市販品「モレキュラーシーブス３Ａ」１ｋ
ｇを冷却装置付内径５０ｍｍのステンレスカラムに充填
した。この充填塔に二酸化炭素１８０ｐｐｍ、塩化水素
４６０ｐｐｍ、酸素１４０ｐｐｍ、窒素５５０ｐｐｍを
含む粗臭化水素を充填塔の温度を−２６℃に設定し、Ｓ
Ｖ８２０時間-1で流した。以後、不純物濃度を経時的に
測定した。なお、ライン内のガス圧は１６気圧であっ
た。その結果、二酸化炭素、塩化水素、酸素及び窒素濃
度が１ｐｐｍ以上となるまでの臭化水素の精製量は、そ
れぞれ３２０ｋｇ、２９０ｋｇ、２１０ｋｇ及び１９５
ｋｇであった。Example 1 Fully dried commercial product "Molecular Sieves 3A" 1k
g was packed in a stainless steel column with an inner diameter of 50 mm equipped with a cooling device. Crude hydrogen bromide containing 180 ppm of carbon dioxide, 460 ppm of hydrogen chloride, 140 ppm of oxygen, and 550 ppm of nitrogen was set in the packed tower at a temperature of -26 ° C.
Flushed at V820 h- 1 . After that, the impurity concentration was measured with time. The gas pressure in the line was 16 atm. As a result, the purified amounts of hydrogen bromide until the concentration of carbon dioxide, hydrogen chloride, oxygen and nitrogen becomes 1 ppm or more are 320 kg, 290 kg, 210 kg and 195, respectively.
It was kg.
【００１５】実施例２ ゼオライトに市販品「ゼオロン５００」を用いた以外は
実施例１と同様の操作を行ったところ、二酸化炭素、塩
化水素、酸素及び窒素濃度が１ｐｐｍ以上となるまでの
臭化水素の精製量は、それぞれ２８５ｋｇ、２８０ｋ
ｇ、１９０ｋｇ及び１６５ｋｇであった。Example 2 The same operation as in Example 1 was carried out except that the commercially available product "Zeolone 500" was used as the zeolite, and the bromination until the carbon dioxide, hydrogen chloride, oxygen and nitrogen concentrations reached 1 ppm or more. The amount of hydrogen purified is 285 kg and 280 k, respectively.
g, 190 kg and 165 kg.
【００１６】実施例３ ゼオライトに市販品「ＡＷ−３００」を用い、充填塔の
温度を２２℃に設定し、ライン内のガス圧が２３気圧で
実施例１と同様の操作を行ったところ、二酸化炭素、塩
化水素、酸素及び窒素濃度が１ｐｐｍ以上となるまでの
臭化水素の精製量は、それぞれ２９５ｋｇ、２８０ｋ
ｇ、１８ｋｇ及び１１ｋｇであった。Example 3 When a commercially available product "AW-300" was used as zeolite, the temperature of the packed column was set to 22 ° C., and the gas pressure in the line was 23 atm, the same operation as in Example 1 was carried out. The purification amount of hydrogen bromide until the concentration of carbon dioxide, hydrogen chloride, oxygen and nitrogen becomes 1 ppm or more is 295 kg and 280 k, respectively.
g, 18 kg and 11 kg.
【００１７】実施例４ ゼオライトに市販品「モレキュラーシーブス３Ａ」を用
い、充填塔の温度を４２℃、ライン内のガス圧を３４気
圧に設定して実施例１と同様の操作を行ったところ、二
酸化炭素、塩化水素、酸素及び窒素濃度が１ｐｐｍ以上
となるまでの臭化水素の精製量は、それぞれ１８５ｋ
ｇ、１７４ｋｇ、５.５ｋｇ及び４ｋｇであった。Example 4 The same operation as in Example 1 was carried out using a commercially available "Molecular Sieves 3A" as the zeolite, setting the temperature of the packed column at 42 ° C and the gas pressure in the line at 34 atm. Purification amount of hydrogen bromide until the concentration of carbon dioxide, hydrogen chloride, oxygen and nitrogen becomes 1ppm or more, respectively, is 185k
g, 174 kg, 5.5 kg and 4 kg.
【００１８】実施例５ 実施例１において、粗臭化水素を３２０ｋｇ処理して破
過した後、粗臭化水素容器バルブを閉止してライン内の
残留ガスを排気口バルブより抜き取り、常圧に戻した後
更に６０ｍｍＨｇの減圧処理を１時間施し、ゼオライト
を再生した。その後、実施例１と同様の操作を行ったと
ころ、二酸化炭素、塩化水素、酸素及び窒素濃度が１ｐ
ｐｍ以上となるまでの臭化水素の精製量は、それぞれ３
１５ｋｇ、２７５ｋｇ、２１０ｋｇ及び１９０ｋｇであ
った。Example 5 In Example 1, after 320 kg of crude hydrogen bromide was treated and broke through, the crude hydrogen bromide container valve was closed and residual gas in the line was extracted from the exhaust port valve to normal pressure. After returning, the pressure reduction treatment of 60 mmHg was further performed for 1 hour to regenerate the zeolite. After that, when the same operation as in Example 1 was performed, the carbon dioxide, hydrogen chloride, oxygen and nitrogen concentrations were 1 p
Purification amount of hydrogen bromide until it becomes pm or more is 3
It was 15 kg, 275 kg, 210 kg and 190 kg.
【００１９】[0019]
【発明の効果】本発明方法により、臭化水素中に含まれ
る二酸化炭素、塩化水素、酸素及び窒素を、簡便な方法
で１ｐｐｍ以下の濃度にまで除去することができ、ＬＳ
Ｉ製造に利用し得る高純度臭化水素を得ることが可能で
ある。According to the method of the present invention, carbon dioxide, hydrogen chloride, oxygen and nitrogen contained in hydrogen bromide can be removed to a concentration of 1 ppm or less by a simple method.
It is possible to obtain high-purity hydrogen bromide that can be used for I production.
【図１】本発明の実施例で使用する精製テストラインの
ブロック図である。FIG. 1 is a block diagram of a purification test line used in an embodiment of the present invention.
１ 粗臭化水素容器 ２ 粗臭化水素容器バルブ ３ 圧力計 ４ ゼオライト充填塔 ５ 冷却器 ６ ガスクロマトグラフサンプリングバルブ ７ ガスクロマトグラフ ８ 流量調節用バルブ ９ 流量計 10 真空用及び不活性ガス導入用バルブ 11 排気口バルブ 1 Crude Hydrogen Bromide Container 2 Crude Hydrogen Bromide Container Valve 3 Pressure Gauge 4 Zeolite Packing Tower 5 Cooler 6 Gas Chromatograph Sampling Valve 7 Gas Chromatograph 8 Flow Control Valve 9 Flow Meter 10 Vacuum and Inert Gas Introduction Valve 11 Exhaust valve
Claims (1)
せることを特徴とする臭化水素の精製法。1. A method for purifying hydrogen bromide, which comprises contacting crude hydrogen bromide with zeolite in a gas phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4190488A JPH0632601A (en) | 1992-07-17 | 1992-07-17 | Purification of hydrogen bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4190488A JPH0632601A (en) | 1992-07-17 | 1992-07-17 | Purification of hydrogen bromide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0632601A true JPH0632601A (en) | 1994-02-08 |
Family
ID=16258931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4190488A Pending JPH0632601A (en) | 1992-07-17 | 1992-07-17 | Purification of hydrogen bromide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0632601A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996008442A1 (en) * | 1994-09-14 | 1996-03-21 | Teisan Kabushiki Kaisha | Method and apparatus for preparing high purity hydrogen bromide |
| EP0714849A1 (en) | 1994-11-28 | 1996-06-05 | Mitsui Toatsu Chemicals, Incorporated | Production process for refined hydrogen iodide |
| FR2772368A1 (en) * | 1997-12-12 | 1999-06-18 | Atochem Elf Sa | PROCESS FOR PRODUCING PURE HYDROGEN BROMIDE AND DEVICE FOR IMPLEMENTING THE SAME |
| EP1236680A2 (en) * | 2001-02-28 | 2002-09-04 | Degussa AG | Process for adsorptive separation of hydrogen halides |
-
1992
- 1992-07-17 JP JP4190488A patent/JPH0632601A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996008442A1 (en) * | 1994-09-14 | 1996-03-21 | Teisan Kabushiki Kaisha | Method and apparatus for preparing high purity hydrogen bromide |
| EP0714849A1 (en) | 1994-11-28 | 1996-06-05 | Mitsui Toatsu Chemicals, Incorporated | Production process for refined hydrogen iodide |
| US5693306A (en) * | 1994-11-28 | 1997-12-02 | Mitsui Toatsu Chemicals, Inc. | Production process for refined hydrogen iodide |
| FR2772368A1 (en) * | 1997-12-12 | 1999-06-18 | Atochem Elf Sa | PROCESS FOR PRODUCING PURE HYDROGEN BROMIDE AND DEVICE FOR IMPLEMENTING THE SAME |
| US6355222B2 (en) * | 1997-12-12 | 2002-03-12 | Elf Atochem S.A. | Manufacture of hydrogen bromide gas |
| EP1236680A2 (en) * | 2001-02-28 | 2002-09-04 | Degussa AG | Process for adsorptive separation of hydrogen halides |
| EP1236680A3 (en) * | 2001-02-28 | 2003-05-28 | Degussa AG | Process for adsorptive separation of hydrogen halides |
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