JP2793208B2 - Distillation purification method - Google Patents
Distillation purification methodInfo
- Publication number
- JP2793208B2 JP2793208B2 JP30001188A JP30001188A JP2793208B2 JP 2793208 B2 JP2793208 B2 JP 2793208B2 JP 30001188 A JP30001188 A JP 30001188A JP 30001188 A JP30001188 A JP 30001188A JP 2793208 B2 JP2793208 B2 JP 2793208B2
- Authority
- JP
- Japan
- Prior art keywords
- solution substance
- solution
- closed container
- substance
- container
- 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
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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
精製方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial application field) The present invention relates to a distillation purification method for purifying a solution reagent 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. Currently, 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
ための蒸留装置（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
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、金属不純物を含んだミ
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;
A cooling tank with a lower slope disposed at the upper part of the distillation tank, and a distillate which is inserted through the bottom of the distillation tank through the bottom from the upper part of the distillation tank, and is condensed and dropped in the cooling tank into a collecting bottle. And a conduit for guiding. However, in such a distillation apparatus, when the solution substance contained in the distillation tank is heated and boiled by the heater, mist containing metal impurities is generated, and the mist adheres to the cooling tank and is condensed with the condensate of the vapor of the solution substance. Since it is introduced into the collection bin through a conduit, 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、金属不純物の混入のない高純度の試薬等を精
製し得る蒸溜精製方法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 in order to solve the above-mentioned conventional problems, and it is an object of the present invention to provide a distillation purification method capable of purifying a high-purity reagent and the like without contamination of metal impurities. Is what you do.
［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設され、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、前記溶液物質の液
面上方に位置する前記密閉容器内に配置されたフィルタ
板と、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設
けられた遮蔽板を具備した蒸溜装置を用いて溶液物質を
蒸溜精製する方法において、前記溶液物質に予め硫酸及
びリン酸のうちの一方又は両者の添加することを特徴と
する蒸溜精製方法である。[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 having a tapered lower portion, and an upper end arranged close to a lower portion of the cooling bath in the closed container. A collecting conduit having a lower end extending downward through the bottom of the container, a collecting container for the distilled liquid into which the lower end of the collecting conduit is inserted, and a liquid collecting material above the liquid surface. A filter plate disposed in the closed container, and a shield plate provided on an inner surface portion of the closed container and an outer surface portion of the collection conduit located between the lower portion of the cooling tank and the surface of the solution substance. Method for distilling and refining a solution substance using a distilled distillation apparatus It is a distillation purification process, characterized by the addition of one or both of the pre-sulfuric acid and phosphoric acid to the solution material.
上記溶液物質としては、例えば塩酸、硝酸、弗化水素
酸、水等を挙げることができる。Examples of the solution substance include hydrochloric acid, nitric acid, hydrofluoric acid, and water.
上記溶液物質に対する硫酸及びリン酸のうちの一方又
は両者の添加割合は、溶液物質中の金属不純物を含むミ
ストの発生を抑制する観点から、0.1重量％以上とする
ことが望ましい。但し、前記硫酸等の添加上限について
は多くし過ぎると精製された溶液物質に硫酸等が多量混
入する恐れがあるため、実用上、５重量％とすることが
望ましい。The addition ratio of one or both of sulfuric acid and phosphoric acid to the solution substance is desirably 0.1% by weight or more from the viewpoint of suppressing generation of mist containing metal impurities in the solution substance. However, if the upper limit of the addition of sulfuric acid or the like is too large, a large amount of sulfuric acid or the like may be mixed into the purified solution substance.
なお、蒸溜精製に用いる上記蒸溜装置としては強磁性
金属不純物を含むミストの発生をより低減させる観点か
ら密閉容器内の溶液物質に磁界を与えるための磁界発生
手段を付設することが望ましい。The distillation apparatus used for distillation purification preferably has a magnetic field generating means for applying a magnetic field to the solution substance in the closed vessel from the viewpoint of further reducing generation of mist containing ferromagnetic metal impurities.
（作用） 本発明によれば、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した蒸溜装置を用いて精製す
ることによって、密閉容器内の溶液物質を加熱、蒸気化
する際、突沸によるミスト発生を抑制でき、かつ冷却槽
下部と溶液物質液面の間に位置する前記密閉容器内の内
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。しかも、溶液物質に硫酸及び
リン酸のうちの一方又は両者を添加することによって、
溶液物質中のＵ、Th、Fe等の金属不純物イオンと反応し
て高沸点の硫酸化合物もしくはリン酸化合物が生成する
ため、金属不純物の蒸発を低下でき、これら不純物を含
むミストの発生を抑制できる。(Function) According to the present invention, when a solution substance in a closed container is heated and vaporized by purifying using a distillation apparatus in which a filter plate is arranged in a closed container located above the liquid surface of the solution substance. Mist generation due to bumping can be suppressed, and by providing a shielding plate on the inner surface portion in the closed vessel and the outer surface portion of the collection conduit located between the lower part of the cooling tank and the liquid surface of the solution substance, respectively, When the solution substance in the closed container is heated and vaporized, the solution substance can be prevented from rising along the inner surface of the closed container or the outer surface of the collecting conduit by the respective shield plates, and the solution substance itself is transferred from the upper end of the conduit to the inside thereof. Can be prevented. Moreover, by adding one or both of sulfuric acid and phosphoric acid to the solution substance,
It reacts with metal impurity ions such as U, Th, and Fe in the solution substance to generate a high-boiling sulfuric acid compound or a phosphoric acid compound, so that the evaporation of metal impurities can be reduced and the generation of mist containing these impurities can be suppressed. .
従って、溶液物質の高純度の蒸気のみを冷却槽で凝縮
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、金属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。Therefore, only the high-purity vapor of the solution substance is condensed in the cooling bath, and is introduced as droplets through the collection conduit to the collection container, so that a high-purity distillate containing extremely little metal impurities can be obtained.
（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。(Example) Hereinafter, an example of the present invention will be described in detail with reference to FIG.
実施例１ 図中の１は、底部付近に蒸溜精製するための溶液物質
２が収容された例えば空間体積が約15000cm3の密閉容器
である。この密閉溶器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が配設されている。このヒータ
３の底面には、例えばポリテトラフルオロエチレンでコ
ートされた直径25cm、厚さ0.5cmで8KGaussの永久磁石か
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。Example 1 Reference numeral 1 in the figure denotes a closed container having a space volume of about 15000 cm 3 , for example, in which a solution substance 2 for distillation and purification is accommodated near the bottom. A heater 3 for heating the solution substance 2 is provided on the bottom of the closed melting vessel 1. A magnetic field generating member 4 made of a permanent magnet having a diameter of 25 cm, a thickness of 0.5 cm, and a thickness of 8 kgauss and coated with, for example, polytetrafluoroethylene is provided on the bottom surface of the heater 3. A sealed container 1 in which such a heater 3 and a magnetic field generating member 4 are sequentially arranged on the bottom surface.
Is installed on the support base 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の上部側壁に閉口
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18のオーバーフロー部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. It is composed of a closed cooling water inlet 11 and a cooling water outlet 12 formed at the 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 container 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 surface 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
An overflow section 20 for cooling water 18 is provided on the upper side wall of the cooling water 18.
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お
り、具体的には直径24mm、厚さ0.2cmの穴が約5000個く
り抜かれたポリテトラフルオロエチレン製板から形成さ
れている。なお、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。前記冷却槽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、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は夫々高純度石英により形成されている。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 having an opening in the center through which the collection conduit 13 penetrates.Specifically, a hole having a diameter of 24 mm and a thickness of 0.2 cm is formed. It is formed from approximately 5,000 hollow polytetrafluoroethylene plates. Each of the filters 21a and 21b may be formed as a single sheet, or may be formed by stacking a plurality of filters at a predetermined interval. A plurality of first shielding plates 22 that are parallel to each other and that are inclined downward are provided on the inner surface of the closed vessel 1 located between the lower portion of the cooling tank 8 and the liquid surface of the solution substance 2. The outer surface of the collecting conduit 13 located between the lower part of the cooling bath 8 and the liquid surface of the solution substance 2 has a plurality of second
Are provided 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. Note that the solution substance 2, the hermetically sealed container 1, the collection conduit 13, the collection container 15, and the shielding plates 22, 23, which are in contact with the evaporating substance and the distillate, are each formed of high-purity quartz.
次に、前述した第１図図示の蒸溜装置を用いて硝酸の
蒸溜精製方法を説明する。Next, a method for distilling and purifying nitric acid using the distillation apparatus shown in FIG. 1 will be described.
まず、硝酸10000mlにリン酸を50ml添加した溶液物質
２を注入部６から密閉容器１内に注入し、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を貯蔵した。
つづいて、磁界発生部材４から溶液物質２に8KGaussの
磁界を与え、かつ冷却槽８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119℃に加熱した。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21
a、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、前記磁界波生部材４からの磁界の作用により
ミスト中にFe、Co、Ni等の強磁性金属不純物が混入する
のを防止できる。更に、溶液物質２には予めリン酸が添
加されているため、硝酸中のＵ、Th、Fe等の金属不純物
イオンが該リン酸と反応して高沸点のリン酸化合物を生
成するため、金属不純物の蒸発が少なくなり、これら金
属不純物を含むミストの発生が抑制される。その上、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, a solution substance 2 obtained by adding 50 ml of phosphoric acid to 10,000 ml of nitric acid was injected into the closed vessel 1 from the injection section 6 and discharged from the discharge section 7 to store a certain amount of the solution substance 2 in the vessel 1.
Subsequently, a magnetic field of 8 Kgauss is applied from the magnetic field generating member 4 to the solution substance 2, and cooling water is supplied from the cooling water inlet 11 of the cooling tank 8 and discharged from the cooling water outlet 12, and the outer cylinder of the cooling tank 8 is discharged. 9 was cooled, and the solution substance 2 in the closed vessel 1 was further heated to 119 ° C. by the heater 3. 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, and the filter plate 21 is placed in and above the solution substance 2.
Since the a and b are arranged respectively, 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, it is possible to prevent ferromagnetic metal impurities such as Fe, Co, and Ni from being mixed into the mist due to the action of the magnetic field from the magnetic field wave generating member 4. Furthermore, since phosphoric acid is added to the solution substance 2 in advance, metal impurity ions such as U, Th, and Fe in nitric acid react with the phosphoric acid to generate a high-boiling phosphoric acid compound. The evaporation of impurities is reduced, and the generation of mist containing these metal impurities is suppressed. In addition, when the solution substance 2 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, that is, so-called creeping is performed on the inner surface of the closed container 1 and the outer surface of the collecting conduit 13. The solution substance 2 itself is prevented from flowing into the inside from the collecting part 14 at the upper end of the collecting conduit 13 by the shielding plates 22 and 23 provided respectively.
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に集
り、落下する。落下した蒸溜液滴27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27
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に落下して硝酸の蒸溜液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 tank 8 gather at the lower portion along the tapered portion of the cooling tank 8 and fall. The fallen distillation droplets 27 are introduced into the collection conduit 13 from the collection unit 14 arranged near the lower part of the cooling tank 8. Distillation droplet 27 falling along the collection conduit 13
Is dropped from the lower end of the conduit 13 into the collection container 15 previously cooled by the cooling water 18 in the cooling container 17 and collected as a distilled liquid 28 of nitric acid.
比較例１ 硝酸にリン酸を添加しない溶液物質を用いた以外、前
記実施例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 Example 1 except that a solution substance in which phosphoric acid was not added to nitric acid was used.
しかして、本実施例１及び比較例１により得られた硝
酸蒸溜液中のＵ及びThを誘導結合プラズマ質量分析装
置、Fe及びCaをフレームレス原子吸光装置により夫々分
析した。その結果を下記第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。U and Th in the distillate of nitric acid obtained in Example 1 and Comparative Example 1 were analyzed by an inductively coupled plasma mass spectrometer, and Fe and Ca were analyzed by a flameless atomic absorption spectrometer. The results are shown in Table 1 below. In Table 1, the analysis values of nitric acid (stock solution) before distillation are also shown.
実施例２ 溶液物質として塩酸10000mlに硫酸を50mlを添加した
ものを用い、かつ蒸溜温度を107℃とした以外、実施例
１と同様な方法により塩酸の蒸溜を行なった。 Example 2 Distillation of hydrochloric acid was carried out in the same manner as in Example 1 except that a solution substance obtained by adding 50 ml of sulfuric acid to 10,000 ml of hydrochloric acid was used and the distillation temperature was changed to 107 ° C.
比較例２ 塩酸に硫酸を添加しない溶液物質を用いた以外、前記
実施例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 Example 2 except that a solution substance in which sulfuric acid was not added to hydrochloric acid was used.
しかして、本実施例２及び比較例２により得られた塩
酸蒸溜液中のＵ及びThを誘導結合プラズマ質量分析装
置、Fe及びCaをフレームレス原子吸光装置により夫々分
析した。その結果を下記第２表に示す。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。U and Th in the hydrochloric acid distilled liquid obtained in Example 2 and Comparative Example 2 were analyzed by an inductively coupled plasma mass spectrometer, and Fe and Ca were analyzed by a flameless atomic absorption spectrometer. The results are shown in Table 2 below. In Table 2, the analysis values of hydrochloric acid (stock solution) before distillation are also shown.
実施例３ 第１図図示の蒸溜装置における溶液物質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をポリテトロフルオロエチレ
ンにより形成し、溶液物質として弗化水素酸10000mlに
硫酸を50ml添加したものを用い、かつ蒸溜温度を110℃
とした以外、実施例１と同様な方法により弗化水素酸の
蒸溜を行なった。 Embodiment 3 In the distillation apparatus shown in FIG. 1, the solution substance 2, the hermetically sealed container 1, the collection conduit 13, the collection container 15, and the shielding plates 22, 23, which are in contact with the evaporated substance and the distillate, are made of polytetrofluoroethylene. Then, as a solution substance, a solution obtained by adding 50 ml of sulfuric acid to 10000 ml of hydrofluoric acid and using a distillation temperature of 110 ° C.
The distillation of hydrofluoric acid was carried out in the same manner as in Example 1 except for the above.
比較例３ 弗化水素酸に硫酸を添加しない溶液物質を用いた以
外、前記実施例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 Example 3 except that a solution substance in which sulfuric acid was not added to hydrofluoric acid was used.
しかして、本実施例３及び比較例３により得られた弗
化水素酸蒸溜液中のＵ及びThを誘導結合プラズマ質量分
析装置、Fe及びCaをフレームレス原子吸光装置により夫
々分析した。その結果を下記第３表に示す。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。U and Th in the hydrofluoric acid distillate obtained in Example 3 and Comparative Example 3 were analyzed by an inductively coupled plasma mass spectrometer, and Fe and Ca were analyzed by a flameless atomic absorption spectrometer. The results are shown in Table 3 below. The third
The analytical values of hydrofluoric acid (stock solution) before distillation are also shown in the table.
上記第１表〜第３表から明かなように、本実施例の蒸
溜精製方法によれば比較例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 and purification method of the present example can distill and purify nitric acid, hydrochloric acid, and hydrofluoric acid with extremely high purity as compared with Comparative Examples 1 to 3. Recognize.
なお、上記実施例で用いた蒸溜装置において捕集導管
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 addition, in the distillation apparatus used in the above embodiment, the collecting conduit
Although a straight one is used as 13, a collection conduit having a coiled shape in the middle may be used to improve the effect of collecting the distilled droplets.
上記実施例で用いた蒸溜装置において、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 distillation apparatus used in the above embodiment, not only the filter 21b is disposed above the solution
Although the filter 21a is disposed therein, the filter 21a may be omitted.
［発明の効果］ 以上詳述した如く、本発明によれば金属不純物の混入
のない高純度の硝酸、塩酸、弗化水素酸等の試薬を精製
し得る蒸溜精製方法を提供できる。[Effects of the Invention] As described in detail above, according to the present invention, it is possible to provide a distillation purification method capable of purifying high purity reagents such as nitric acid, hydrochloric acid, hydrofluoric acid and the like without contamination of metal impurities.
第１図は、本発明の実施例で使用した蒸溜装置の一形態
を示す概略図である。 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 showing one embodiment of a distillation apparatus used in an 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.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) B01P 3/34 B01D 3/00 C01B 7/07 C01B 7/19──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 6 , DB name) B01P 3/34 B01D 3/00 C01B 7/07 C01B 7/19
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、前記溶液物質の液
面上方に位置する前記密閉容器内に配置されたフィルタ
板と、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設
けられた遮蔽板を具備した蒸溜装置を用いて溶液物質を
蒸溜精製する方法において、前記溶液物質に予め硫酸及
びリン酸のうちの一方又は両者を添加することを特徴と
する蒸溜精製方法。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 and having a lower part tapered, and an upper end disposed close to a lower part of the cooling tank in the closed container, and a lower end penetrating through the bottom of the container and extending downward. A collection conduit extended to, a collection container for a distilled liquid into which the lower end of the collection conduit is inserted, and a filter plate disposed in the closed container located above the liquid surface of the solution substance, A method for distilling and purifying a solution substance using a distillation apparatus having a shield plate provided on an inner surface portion of the closed vessel located between a lower portion of the cooling tank and a liquid surface of the solution material and an outer surface portion of the collection conduit. , The solution substance is previously added with sulfuric acid and phosphoric acid. Square or distillation purification process, characterized in that the addition of both.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30001188A JP2793208B2 (en) | 1988-11-28 | 1988-11-28 | Distillation purification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30001188A JP2793208B2 (en) | 1988-11-28 | 1988-11-28 | Distillation purification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02144101A JPH02144101A (en) | 1990-06-01 |
| JP2793208B2 true JP2793208B2 (en) | 1998-09-03 |
Family
ID=17879644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30001188A Expired - Fee Related JP2793208B2 (en) | 1988-11-28 | 1988-11-28 | Distillation purification method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2793208B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2659956B1 (en) * | 1990-03-21 | 1992-06-26 | Cogema | PROCESS FOR TREATING AN AQUEOUS SOLUTION CONTAINING MAINLY NITRIC ACID AND FLUORHYDRIC ACID. |
| 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 |
| CN102921180A (en) * | 2011-08-08 | 2013-02-13 | 四川西陇化工有限公司 | Preparation method of inorganic ultra-clean highly-pure reagent acid |
-
1988
- 1988-11-28 JP JP30001188A patent/JP2793208B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02144101A (en) | 1990-06-01 |
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