JP2624734B2 - Distillation equipment - Google Patents
Distillation equipmentInfo
- Publication number
- JP2624734B2 JP2624734B2 JP73588A JP73588A JP2624734B2 JP 2624734 B2 JP2624734 B2 JP 2624734B2 JP 73588 A JP73588 A JP 73588A JP 73588 A JP73588 A JP 73588A JP 2624734 B2 JP2624734 B2 JP 2624734B2
- Authority
- JP
- Japan
- Prior art keywords
- solution substance
- closed container
- container
- solution
- substance
- 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 - Fee Related
Links
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
【発明の詳細な説明】 ［発明の目的］ （産業上の利用分野） 本発明は、酸等の溶液状の試薬を精製するための蒸溜
装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Field of Industrial Application) The present invention relates to a distillation apparatus for purifying a reagent in the form of a solution such as an acid.
（従来の技術） 電子工業、原子力工業或いは各種素材工業の進歩に伴
い材料の高純度化の要求が高まっている。また、材料評
価技術においても超微量成分分析技術の向上が望まれて
いる。最近の分析装置の急速な発達により湿式化学分析
において超微量成分の分析が相当可能になってきたが、
分析に使用する試薬から分析目的成分が混入する、いわ
ゆるコンタミネーションの問題により分析のブランク値
が高くなり、必ずしも超微量成分を高精度で分析できな
い場合があった。現在、電子工業用又は有害金属測定用
の高純度試薬が市販されているが、超微量成分分析に用
いるために充分な純度といえず、使用目的に応じて更に
精製する必要があった。(Prior Art) With the progress of the electronics industry, the nuclear industry and the various material industries, there is an increasing demand for higher purity of materials. Also, in the material evaluation technology, the improvement of the ultra trace component analysis technology is desired. The rapid development of recent analyzers has made it possible to analyze ultra-trace components in wet chemical analysis.
Due to the problem of so-called contamination, in which a component to be analyzed is mixed from a reagent used for analysis, a blank value of the analysis is increased, and an ultra-trace component may not always be analyzed with high accuracy. At present, high-purity reagents for use in the electronics industry or for measuring harmful metals are commercially available, but the purity is not sufficient for use in ultra-trace component analysis, and further purification is required depending on the purpose of use.
このようなことから、従来より高純度試薬を調製する
ための蒸溜装置（特開昭60-183002号公報）が知られて
いる。この蒸溜装置は、蒸溜すべき溶液物質が収容され
れた蒸溜槽と、この蒸溜槽の底部に配設されたヒータ
と、前記蒸溜槽の上部に配設された下部が傾斜した形状
の冷却槽と、前記蒸溜槽の上部から底部を貫通して挿入
され、前記冷却槽で凝縮、滴下された蒸溜液を捕集ビン
に導くための導管とを具備した構造になっている。しか
しながら、かかる蒸溜装置では蒸溜槽内に収容した溶液
物質をヒータで加熱沸騰させる際、ミストが発生すると
共に該ミストが冷却槽に付着して溶液物質の蒸気の凝縮
液と共に導管を通して捕集ビンに導入されるため、高純
度の蒸溜液を精製できない問題があった。For this reason, a distillation apparatus (JP-A-60-183002) for preparing a high-purity reagent has been conventionally known. The distillation apparatus includes a distillation tank containing a solution substance to be distilled, a heater disposed at a bottom of the distillation tank, and a cooling tank disposed at an upper part of the distillation tank and having a lower portion inclined. And a conduit which is inserted through the bottom from the top of the distillation tank and guides the distilled liquid condensed and dropped in the cooling tank to a collection bin. However, in such a distillation apparatus, when the solution substance contained in the distillation tank is heated and boiled by the heater, mist is generated and the mist adheres to the cooling tank, and together with the condensate of the vapor of the solution substance, passes through the conduit to the collection bin. Due to the introduction, there was a problem that high-purity distillate could not be purified.
（発明が解決しようとする課題） 本発明は、上記従来の問題点を解決するためになされ
たもので、不純物の混入のない高純度の試薬等を精製し
得る蒸溜装置を提供しようとするものである。(Problems to be Solved by the Invention) The present invention has been made to solve the above-mentioned conventional problems, and aims to provide a distillation apparatus capable of purifying a high-purity reagent or the like without contamination of impurities. It is.
［発明の構成］ （課題を解決するための手段） 本発明は、底部付近に溶液物質が収容された密閉容器
と、この密閉容器の側壁に連結された溶液物質の注入部
及び排出部と、前記密閉容器内の溶液物質を加熱するた
めの加熱手段と、前記密閉容器の上部に挿置され、下部
がテーパ状をなす冷却槽と、上端が前記密閉容器内の冷
却槽下部に近接して配置され、かつ下端を該容器底面を
貫通して下方に延出させた捕集導管と、この捕集導管の
下端が挿入される蒸溜液の捕集容器とを具備した蒸溜装
置において、前記密閉容器内の溶液物質に磁界を与える
ための磁界発生手段を配置し、かつ前記溶液物質の液面
上方に位置する前記密閉容器内にフィルタ板を配置し、
更に前記冷却槽下部と溶液物質液面の位置する前記密閉
容器の内面部分及び前記捕集導管の外面部分に遮蔽板を
夫々設けたことを特徴とする蒸溜装置である。[Constitution of the Invention] (Means for Solving the Problems) The present invention relates to a closed container in which a solution substance is accommodated near a bottom, an injection section and a discharge section of the solution substance connected to a side wall of the closed container, A heating means for heating the solution substance in the closed container, a cooling bath inserted in the upper portion of the closed container, and a lower portion having a tapered shape, and an upper end close to a lower portion of the cooling bath in the closed container. A distillation apparatus, comprising: a collection conduit arranged and having a lower end extending downward through the bottom of the container; and a collection container for a distilled liquid into which the lower end of the collection conduit is inserted, A magnetic field generating means for applying a magnetic field to the solution substance in the container is arranged, and a filter plate is arranged in the closed container located above the liquid level of the solution substance,
The distillation apparatus is further characterized in that shielding plates are respectively provided on an inner surface portion of the closed vessel where the lower part of the cooling tank and the surface of the solution substance are located and an outer surface portion of the collecting conduit.
（作用） 本発明によれば、密閉容器内の溶液物質に磁界を与え
るための磁界発生手段を配置することによって、加熱手
段により密閉容器内の溶液物質を加熱、蒸気化する際、
突沸により発生したミスト中にFe、Niなどの強磁性物質
が混入するのを抑制できる。また、溶液物質の液面上方
に位置する密閉容器内にフィルタ板を配置することによ
って、前記突沸によるミストの発生を該フィルタ板によ
り抑制できる。更に、冷却槽下部と溶液物質液面の間に
位置する前記密閉容器の内面部分及び前記捕集導管の外
面部分に遮蔽板を夫々設けることによって、加熱手段に
より密閉容器内の溶液物質を加熱、蒸気化する際、溶液
物質が密閉容器内面や捕集導管外面に沿って上昇するの
を前記各遮蔽板によって防止でき、溶液物質そのものが
導管の上端からその内部に流入するのを防止できる。(Action) According to the present invention, by arranging a magnetic field generating means for applying a magnetic field to the solution substance in the closed container, when the heating means heats and vaporizes the solution substance in the closed container,
Ferromagnetic substances such as Fe and Ni can be prevented from entering the mist generated by bumping. Further, by disposing a filter plate in a closed container located above the liquid surface of the solution substance, generation of mist due to bumping can be suppressed by the filter plate. Furthermore, by providing a shield plate on the inner surface portion of the closed vessel and the outer surface portion of the collection conduit located between the lower portion of the cooling tank and the liquid surface of the solution substance, the heating means heats the solution substance in the closed vessel, When evaporating, the above-mentioned shielding plates can prevent the solution substance from rising along the inner surface of the closed vessel or the outer surface of the collection conduit, and can prevent the solution substance itself from flowing into the inside from the upper end of the conduit.
従って、溶液物質の蒸気を冷却槽で凝縮し、液滴とし
て捕集導管を通して捕集容器に導くことによって、不純
物の混入が極めて少ない高純度の蒸溜液を得ることがで
きる。Accordingly, by condensing the vapor of the solution substance in the cooling tank and guiding the vapor as droplets to the collection container through the collection conduit, a highly pure distilled liquid with very little impurities can be obtained.
（発明の実施例） 以下、本発明の実施例を第１図を参照して詳細に説明
する。Embodiment of the Invention Hereinafter, an embodiment of the present invention will be described in detail with reference to FIG.
図中の１は、底部付近に蒸溜精製するための溶液物質
２が収容された密閉容器である。ここに用いる溶液物質
としては、例えば塩酸、硝酸、硫酸、弗化水素酸等を挙
げることができる。この密閉容器１の底面には、前記溶
液物質２を加熱するためのヒータ３が配設されており、
かつ該ヒータ３の底面には例えば永久磁石からなる磁界
発生部材４が配設されている。こうしたヒータ３、磁界
発生部材４を底面に順次配設した密閉容器１は、支持台
５上に設置されている。前記密閉容器１の下部側壁に
は、溶液物質の注入部６が連結され、かつ該注入部６と
対向する該密閉容器１の下部側壁には上下に折れ曲がっ
た溶液物質の排出部７が連結されている。Reference numeral 1 in the figure denotes a closed container containing a solution substance 2 for distillation purification near the bottom. Examples of the solution substance used here include hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid and the like. A heater 3 for heating the solution substance 2 is provided on a bottom surface of the closed container 1.
A magnetic field generating member 4 made of, for example, a permanent magnet is provided on the bottom surface of the heater 3. The sealed container 1 in which the heater 3 and the magnetic field generating member 4 are sequentially arranged on the bottom surface is installed on a support 5. A solution material injection part 6 is connected to a lower side wall of the closed container 1, and a vertically bent solution material discharge part 7 is connected to the lower side wall of the closed container 1 opposed to the injection part 6. ing.
また、前記密閉容器１の上部には、冷却槽８が挿置さ
れている。この冷却槽８は、下部がテーパ状をなすと共
に上下封じられた外筒体９と、この外筒体９の上部から
挿置された内筒体10と、前記外筒体９の上部側壁に開口
された冷却水入口11と、前記内筒体10の上端に形成され
た冷却水出口12とから構成されている。こうした冷却槽
８において、冷却水入口11から冷却水を導入することに
より冷却水は外筒体９と内筒体10の間の環状空間を通っ
て下方に移動して外筒体９を冷却し、この後内筒体10内
に流入して冷却水出口12から排出される。前記密閉容器
１内には、捕集導管13がその上端を前記冷却槽８のテー
パ状下部に近接して配置され、かつ該捕集導管13の下端
は該密閉容器１の底面、ヒータ３、磁界発生部材４及び
支持台５を貫通して下方に延出されている。前記冷却槽
８のテーパ状下部に近接する捕集導管13の上端には、漏
斗形状の捕集部14が形成されている。前記捕集導管13の
下端は、捕集容器15の口部に挿入されている。この捕集
容器15は、冷却容器17内に配置され、かつ該冷却容器17
内には冷却水18が満たされている。前記冷却容器17の下
部側壁には、冷却水導入部19が設けられ、かつ同容器17
の上部側壁には冷却水のオーバーフロ部20が設けられて
いる。Further, a cooling bath 8 is inserted above the closed container 1. The cooling tank 8 has a tapered lower portion, an upper and lower sealed outer cylinder 9, an inner cylinder 10 inserted from above the outer cylinder 9, and an upper side wall of the outer cylinder 9. A cooling water inlet 11 is opened, and a cooling water outlet 12 is formed at an upper end of the inner cylindrical body 10. In such a cooling tank 8, by introducing cooling water from the cooling water inlet 11, the cooling water moves downward through the annular space between the outer cylinder 9 and the inner cylinder 10 to cool the outer cylinder 9. Thereafter, the cooling water flows into the inner cylindrical body 10 and is discharged from the cooling water outlet 12. In the closed vessel 1, a collecting conduit 13 is disposed with its upper end close to the tapered lower portion of the cooling bath 8, and the lower end of the collecting conduit 13 is provided on the bottom of the closed container 1, the heater 3, It extends downward through the magnetic field generating member 4 and the support base 5. At the upper end of the collecting conduit 13 near the tapered lower part of the cooling tank 8, a collecting part 14 having a funnel shape is formed. The lower end of the collection conduit 13 is inserted into the mouth of the collection container 15. This collection container 15 is disposed in the cooling container 17 and
The inside is filled with cooling water 18. A cooling water introduction section 19 is provided on a lower side wall of the cooling vessel 17, and
Is provided with an overflow section 20 for cooling water.
更に、前記密閉容器１内の溶液物質２が収容された部
分及び該溶液物質２の液面上方には、フィルタ板21a、2
1bが夫々設けられている。これらフィルタ板21a、21b
は、多数の穴が穿設された円板状をなすと共に中央に前
記捕集導管13が貫通する穴を開口した形状になってい
る。なお、穴はいかなる形状でもよく、かつ穴の大きさ
は５mm2前後にすることが望ましい。また、前記各フィ
ルタ21a、21bは夫々１枚で形成しても、複数枚所定の間
隔をあけて積層して形成してもよい。前記冷却層８下部
と溶液物質２液面の間に位置する前記密閉容器１の内面
部分には、互いに平行して下方に傾斜した複数枚の第１
の遮蔽板22が夫々設けられている。また、前記冷却槽８
下部と溶液物質２液面の間に位置する前記捕集導管13の
外面部分には複数枚の第２の遮蔽板23が下方に傾斜する
ように夫々設けられている。前記密閉容器１の側壁に
は、吸排気管24が連結されており、かつ該吸排気管24に
はバルブ25が介装されている。なお、前記溶液物質２が
硝酸、塩酸、硫酸からなる場合には、該溶液物質２、そ
の蒸発物質及び蒸溜液が接触する密閉容器１、フィルタ
板21a、21b、捕集導管13、捕集容器15及び遮蔽板22、23
は高純度石英により形成し、一方、溶液物質２が弗化水
素酸からなる場合には、該溶液物質２、その蒸発物質及
び蒸溜液が接触する密閉容器１、フィルタ板21a、21b、
捕集導管13、捕集容器15及び遮蔽板22、23は弗素樹脂
（例えばポリテトロフルオロエチレン）により形成し
た。Further, a filter plate 21a, 2a is provided above the portion of the closed container 1 in which the solution substance 2 is stored and above the liquid level of the solution substance 2.
1b is provided respectively. These filter plates 21a, 21b
Has a shape of a disc having a large number of holes formed therein, and has a shape in which a hole through which the collection conduit 13 penetrates is opened at the center. The hole may have any shape, and the size of the hole is desirably about 5 mm 2 . Each of the filters 21a and 21b may be formed of a single sheet, or may be formed by laminating a plurality of filters at predetermined intervals. The inner surface portion of the closed vessel 1 located between the lower part of the cooling layer 8 and the liquid surface of the solution substance 2 includes a plurality of first sheets inclined downward in parallel with each other.
Are provided. Further, the cooling tank 8
A plurality of second shielding plates 23 are provided on the outer surface of the collection conduit 13 located between the lower part and the liquid surface of the solution substance 2 so as to be inclined downward. An intake / exhaust pipe 24 is connected to a side wall of the closed vessel 1, and a valve 25 is interposed in the intake / exhaust pipe 24. When the solution substance 2 is composed of nitric acid, hydrochloric acid, or sulfuric acid, the solution substance 2, the hermetically sealed container 1, the filter plates 21a and 21b, the collection conduit 13, the collection container, 15 and shielding plates 22, 23
Is formed of high-purity quartz. On the other hand, when the solution substance 2 is made of hydrofluoric acid, the closed vessel 1, the filter plates 21a, 21b,
The collection conduit 13, the collection container 15, and the shielding plates 22 and 23 were formed of a fluorine resin (for example, polytetrafluoroethylene).
次に、前述した第１図図示の蒸溜装置の作用を説明す
る。Next, the operation of the distillation apparatus shown in FIG. 1 will be described.
まず、注入部６から密閉容器１内に溶液物質２を注入
し、排出部７から排出して該容器１内に一定量の溶液物
質２を貯蔵する。つづいて、磁界発生部材４から溶液物
質２に所定の磁気力を与え、かつ冷却槽９の冷却水入口
11から冷却水を供給して冷却水出口12から排出して該冷
却槽８の外筒体９を冷却し、更にヒータ３により密閉容
器１内の溶液物質２をその沸点以上に加熱する。こうし
たヒータ３による加熱によって、密閉容器１内の溶液物
質２が沸騰、蒸気化される。この場合、溶液物質２の表
面でミストの発生が起こるが、該溶液物質２中及びその
上方にフィルタ板21a、21bが夫々配置されているため、
ミストが溶液物質の蒸気26と共に密閉容器１の上部に上
昇するのを抑制される。また、前記磁界発生部材４から
の磁気力の作用によりミスト中にFe、Co、Ni等の強磁性
不純物が混入されるのを防止される。更に、溶液物質２
を加熱、蒸気化する際して該溶液物質２が密閉容器１内
面や捕集導管13外面に沿って上昇する、いわゆるクリー
ピングを密閉容器１内面及び捕集導管13外面に夫々設け
られた遮蔽板22、23によって阻止され、溶液物質２その
ものが捕集導管13上端の捕集部14からその内部に流入す
るのを防止される。First, the solution substance 2 is injected into the closed container 1 from the injection part 6 and discharged from the discharge part 7 to store a certain amount of the solution substance 2 in the container 1. Subsequently, a predetermined magnetic force is applied to the solution substance 2 from the magnetic field generating member 4 and the cooling water inlet of the cooling tank 9 is provided.
Cooling water is supplied from 11 and discharged from the cooling water outlet 12 to cool the outer cylinder 9 of the cooling bath 8, and the heater 3 heats the solution substance 2 in the closed vessel 1 to a temperature higher than its boiling point. By the heating by the heater 3, the solution substance 2 in the closed container 1 is boiled and vaporized. In this case, mist is generated on the surface of the solution substance 2, but since the filter plates 21a and 21b are respectively disposed in and above the solution substance 2,
The mist is prevented from rising to the upper part of the closed container 1 together with the vapor 26 of the solution substance. Further, the action of the magnetic force from the magnetic field generating member 4 prevents ferrite impurities such as Fe, Co, and Ni from being mixed into the mist. In addition, solution substance 2
When the solution is heated and vaporized, the solution substance 2 rises along the inner surface of the closed container 1 and the outer surface of the collecting conduit 13, so-called creeping is performed by shielding the inner surface of the closed container 1 and the outer surface of the collecting conduit 13 respectively. The solution substance 2 itself is blocked by the plates 22 and 23, and is prevented from flowing into the inside of the collecting substance 13 from the collecting part 14 at the upper end of the collecting pipe 13.
上記ヒータ３の加熱により蒸気化され、ミスト等の混
入が抑制された溶液物質の蒸気26は、密閉容器１内を上
昇し、その上部に配置された冷却槽８の外表面に接触し
て凝縮する。こうして冷却槽８で凝縮された溶液物質の
蒸溜液滴27は、該冷却槽８のテーパ部に沿って下部集
り、落下する。落下した蒸溜液滴は、冷却槽８の下部に
近接して配置された捕集部14をから捕集導管13内に導入
される。捕集導管13を伝わって落下する蒸溜液滴は、該
導管13の下端から予め冷却容器17内で冷却水18により冷
却された捕集容器15に落下して蒸溜液28として捕集され
る。The vapor 26 of the solution substance, which is vaporized by the heating of the heater 3 and in which the mist or the like is suppressed from entering, rises in the closed vessel 1 and contacts the outer surface of the cooling tank 8 disposed thereon to condense. I do. The distilled liquid droplets 27 of the solution substance condensed in the cooling bath 8 gather at the lower portion along the tapered portion of the cooling bath 8 and fall. The dropped distillation droplets are introduced into the collection conduit 13 through the collection unit 14 arranged close to the lower part of the cooling bath 8. Distilled droplets that fall along the collecting conduit 13 fall from the lower end of the conduit 13 into the collecting container 15 previously cooled by the cooling water 18 in the cooling container 17 and are collected as distilled liquid 28.
従って、本発明によれば密閉容器１内でヒータ３によ
り溶液物質２を蒸気化する際、密閉容器１内を上昇する
溶液物質の蒸気26中へのミストの混入を抑制できると共
に、該ミスト中への強磁性金属の混入を防止し、かつク
リーピングによる溶液物質２そのものが捕集導管13内に
流入されるのを防止できるため、冷却槽８での凝縮、捕
集導管13を通しての蒸溜液滴の落下、蒸溜液滴の捕集容
器15への捕集によって極めて高純度の蒸溜液を得ること
ができる。Therefore, according to the present invention, when the solution substance 2 is vaporized by the heater 3 in the closed container 1, the mist can be prevented from being mixed into the vapor 26 of the solution substance rising in the closed container 1, and To prevent the ferromagnetic metal from being mixed into the liquid and to prevent the solution substance 2 itself from flowing into the collection conduit 13 due to creeping. An extremely high purity distilled liquid can be obtained by dropping the droplets and collecting the distilled liquid droplets in the collecting container 15.
事実、本実施例の蒸溜装置を用い、次のような実験を
行なうことによって高純度の硝酸等の蒸溜液を得ること
が確認された。In fact, it was confirmed that a high-purity distillate such as nitric acid was obtained by performing the following experiment using the distillation apparatus of this example.
実験例１ 上述した蒸溜装置における磁界発生部材４としてポリ
テトラフルオロエチレンでコートされた永久磁石（直径
25cm×厚さ0.5cm、8 KG auss）、フィルタ板21a、21bと
して直径24mm×厚さ0.3cmで直径0.2cmの穴が約5000個穿
設されたポリテトラフルオロエチレン製板を用い、かつ
溶液物質２、その蒸発物質及び蒸溜液が接触する密閉容
器１、捕集導管13、捕集容器15及び遮蔽板22、23を高純
度石英で形成した。こうした蒸溜装置の密閉容器１内に
溶液物質としの硝酸10000mlを注入口６から供給した。
この時の密閉容器１の空間体積は、約15000cm3であっ
た。つづいて、ヒータ３によって密閉容器１内の硝酸を
119℃に加熱、蒸溜して捕集容器15内に硝酸の蒸溜液を
捕集した。EXPERIMENTAL EXAMPLE 1 A permanent magnet (diameter) coated with polytetrafluoroethylene was used as the magnetic field generating member 4 in the above-described distillation apparatus.
25cm x 0.5cm, 8KG auss), a polytetrafluoroethylene plate with 24mm diameter x 0.3cm thickness and about 5,000 holes with a diameter of 0.2cm perforated as filter plates 21a and 21b, and a solution The substance 2, the hermetically sealed container 1, the collecting conduit 13, the collecting container 15, and the shielding plates 22, 23, which are in contact with the evaporated substance and the distillate, were formed of high-purity quartz. 10000 ml of nitric acid as a solution substance was supplied from the inlet 6 into the closed vessel 1 of such a distillation apparatus.
At this time, the space volume of the sealed container 1 was about 15000 cm 3 . Subsequently, the nitric acid in the closed container 1 is removed by the heater 3.
The mixture was heated to 119 ° C. and distilled, and a distillate of nitric acid was collected in the collection container 15.
比較例１ 磁界発生部材及びフィルタを用いない以外、前記実験
例１と同様な方法により硝酸の蒸溜を行なった。Comparative Example 1 Distillation of nitric acid was performed in the same manner as in Experimental Example 1 except that the magnetic field generating member and the filter were not used.
しかして、本実験例１及び比較例１により得られた硝
酸蒸溜液中のNa、Ｋ、Fe及びCrを以下に示す条件のフレ
ームレス原子吸光装置により分析した。Thus, Na, K, Fe and Cr in the distillate of nitric acid obtained in Experimental Example 1 and Comparative Example 1 were analyzed by a flameless atomic absorption spectrometer under the following conditions.
蒸溜液の乾燥;120℃で30秒間。 Drying of the distillate; 30 seconds at 120 ° C.
灰化;Naは600℃、Ｋは700℃、Fe及びCrは1000℃で夫
々30秒間。Ashing; Na at 600 ° C, K at 700 ° C, Fe and Cr at 1000 ° C for 30 seconds each.
原子化;Naは2500℃、Ｋは2700℃、Fe及びCrは2800℃
で夫々８秒間。Atomization: 2500 ℃ for Na, 2700 ℃ for K, 2800 ℃ for Fe and Cr
For 8 seconds each.
キャリアガス；アルゴンを300ml/min（但し、原子化
の時は通流しない）。Carrier gas: 300 ml / min of argon (however, it does not flow during atomization).
測定波長;Naは589.0nm、Ｋは766.5nm、Feは248.3nm、
Crは359.4nm。Measurement wavelength; Na is 589.0 nm, K is 766.5 nm, Fe is 248.3 nm,
Cr is 359.4 nm.
妨害吸収補正用光源;Na、Ｋの時はハロゲンタングス
テンランプ、Fe、Crの時は重水素ランプを使用。Light source for interference absorption correction; use halogen tungsten lamp for Na and K, and deuterium lamp for Fe and Cr.
以上の結果を下記第１表に示す。なお、第１表中には
蒸溜する前の硝酸（原液）の分析値を併記した。The above results are shown in Table 1 below. In Table 1, the analysis values of nitric acid (stock solution) before distillation are also shown.
実験例２ 溶液物質として塩酸10000ml、蒸溜温度を107℃とした
以外、実験例１と同様な蒸溜装置、条件で塩酸の蒸溜を
行なった。 EXPERIMENTAL EXAMPLE 2 Distillation of hydrochloric acid was carried out using the same distillation apparatus and conditions as in Experimental Example 1 except that the solution substance was 10000 ml of hydrochloric acid and the distillation temperature was 107 ° C.
比較例２ 磁界発生部材及びフィルタを用いない以外、前記実験
例２と同様な方法により塩酸の蒸溜を行なった。Comparative Example 2 Distillation of hydrochloric acid was performed in the same manner as in Experimental Example 2 except that the magnetic field generating member and the filter were not used.
しかして、本実験例２及び比較例２により得られた塩
酸蒸溜液中のNa、Ｋ、Fe及びCrを実験例１と同様な条件
のフレームレス原子吸光装置により分析した。その結果
を下記第２表に示した。なお、第２表中には蒸溜する前
の塩酸（原液）の分析値を併記した。Then, Na, K, Fe and Cr in the hydrochloric acid distilled liquid obtained in Experimental Example 2 and Comparative Example 2 were analyzed by a flameless atomic absorption apparatus under the same conditions as in Experimental Example 1. The results are shown in Table 2 below. In Table 2, the analysis values of hydrochloric acid (stock solution) before distillation are also shown.
実験例３ 溶液物質として弗化水素酸10000ml、蒸溜温度を110
℃、蒸溜装置の各部材の材質を全てポリテトラフルオロ
エチレンで形成した以外、実験例１と同様な条件で弗化
水素酸の蒸溜を行なった。 Experimental Example 3 10000 ml of hydrofluoric acid as a solution substance and a distillation temperature of 110
Distillation of hydrofluoric acid was carried out under the same conditions as in Experimental Example 1 except that all the materials of the members of the distillation apparatus were made of polytetrafluoroethylene at a temperature of ° C.
比較例３ 磁界発生部材及びフィルタを用いない以外、前記実験
例３と同様な方法により弗化水素酸の蒸溜を行なった。Comparative Example 3 Hydrofluoric acid was distilled in the same manner as in Experimental Example 3 except that the magnetic field generating member and the filter were not used.
しかして、本実験例３及び比較例３により得られた弗
化水素酸蒸溜液中のNa、Ｋ、Fe及びCrを実験例１と同様
な条件のフレームレス原子吸光装置により分析した。そ
の結果を下記第３表に示した。なお、第３表中には蒸溜
する前の弗化水素酸（原液）の分析値を併記した。Then, Na, K, Fe and Cr in the hydrofluoric acid distilled liquid obtained in Experimental Example 3 and Comparative Example 3 were analyzed by a flameless atomic absorption apparatus under the same conditions as in Experimental Example 1. The results are shown in Table 3 below. In Table 3, the analytical values of hydrofluoric acid (stock solution) before distillation are also shown.
上記第１表〜第３表から明かなように、本発明の蒸溜
装置によれば比較例１〜３に比べて極めて高純度の硝
酸、塩酸、弗化水素酸を蒸溜、精製できることがわか
る。 As is clear from Tables 1 to 3, the distillation apparatus of the present invention can distill and purify nitric acid, hydrochloric acid, and hydrofluoric acid, which are extremely high in purity, as compared with Comparative Examples 1 to 3.
なお、上記実施例では磁界発生部材を永久磁石で形成
したが、電磁石で形成してもよい。In the above embodiment, the magnetic field generating member is formed of a permanent magnet, but may be formed of an electromagnet.
上記実施例では、捕集導管13として直線状のものを使
用したが、蒸溜液滴の捕集効果を向上させるために途中
をコイル状とした捕集導管を用いてもよい。In the above embodiment, a straight collecting pipe is used as the collecting pipe 13. However, a collecting pipe having a coiled portion may be used in order to improve the collecting effect of the distilled droplets.
上記実施例では、溶液物質２の上方にフィルタ21bを
配置するのみならず、溶液物質２中にもフィルタ21aを
配置したが、該フィルタ21aを省略してもよい。In the above embodiment, not only the filter 21b is disposed above the solution substance 2 but also the filter 21a is disposed in the solution substance 2, but the filter 21a may be omitted.
［発明の効果］ 以上詳述した如く、本発明によれば不純物の混入のな
い高純度の硝酸、塩酸、弗化水素酸等の試薬を精製し得
る蒸溜装置を提供できる。[Effects of the Invention] As described above in detail, according to the present invention, it is possible to provide a distillation apparatus capable of purifying a high-purity reagent such as nitric acid, hydrochloric acid, hydrofluoric acid or the like without contamination of impurities.
第１図は、本発明の一実施例を示す蒸溜装置の概略図で
ある。 １……密閉容器、２……溶液物質、３……ヒータ、４…
…磁界発生部材、８……冷却槽、13……捕集導管、15…
…捕集容器、17……冷却容器、21a、21b……フィルタ、
22、23……遮蔽板、26……蒸気、27……蒸溜液滴、28…
…蒸溜液。FIG. 1 is a schematic view of a distillation apparatus showing one embodiment of the present invention. 1 ... closed container, 2 ... solution substance, 3 ... heater, 4 ...
... magnetic field generating member, 8 ... cooling tank, 13 ... collection conduit, 15 ...
… Collection container, 17… Cooling container, 21a, 21b …… Filter,
22, 23 ... shielding plate, 26 ... steam, 27 ... distilled droplets, 28 ...
... distilled liquid.
Claims (1)
と、この密閉容器の側壁に連結された溶液物質の注入部
及び排出部と、前記密閉容器内の溶液物質を加熱するた
めの加熱手段と、前記密閉容器の上部に挿置され、下部
がテーパ状をなす冷却槽と、上端が前記密閉容器内の冷
却槽下部に近接して配置され、かつ下端を該容器底面を
貫通して下方に延出させた捕集導管と、この捕集導管の
下端が挿入される蒸溜液の捕集容器とを具備した蒸溜装
置において、前記密閉容器内の溶液物質に磁界を与える
ための磁界発生手段を配置し、かつ前記溶液物質の液面
上方に位置する前記密閉容器内にフィルタ板を配置し、
更に前記冷却槽下部と溶液物質液面の間に位置する前記
密閉容器の内面部分及び前記捕集導管の外面部分に遮蔽
板を夫々設けたことを特徴とする蒸溜装置。1. A closed container containing a solution substance near a bottom, an inlet and an outlet for a solution substance connected to a side wall of the closed container, and a heating device for heating the solution substance in the closed container. Means, a cooling tank inserted in the upper part of the closed container, a lower part having a tapered shape, and an upper end arranged near the lower part of the cooling tank in the closed container, and a lower end penetrating the bottom of the container. In a distillation apparatus including a collection pipe extending downward and a collection container for a distilled liquid into which a lower end of the collection pipe is inserted, a magnetic field generation for applying a magnetic field to the solution substance in the closed container is performed. Disposing means, and disposing a filter plate in the closed container located above the level of the solution substance;
A distillation apparatus, further comprising shielding plates provided on an inner surface portion of the closed vessel and an outer surface portion of the collection conduit located between the lower part of the cooling tank and the surface of the solution substance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP73588A JP2624734B2 (en) | 1988-01-07 | 1988-01-07 | Distillation equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP73588A JP2624734B2 (en) | 1988-01-07 | 1988-01-07 | Distillation equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01180202A JPH01180202A (en) | 1989-07-18 |
| JP2624734B2 true JP2624734B2 (en) | 1997-06-25 |
Family
ID=11481982
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP73588A Expired - Fee Related JP2624734B2 (en) | 1988-01-07 | 1988-01-07 | Distillation equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2624734B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398895B (en) * | 2010-09-16 | 2014-09-24 | 上海化学试剂研究所 | Production method of ultra-pure electronic grade chemical reagent |
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1988
- 1988-01-07 JP JP73588A patent/JP2624734B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01180202A (en) | 1989-07-18 |
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