JPH0220575B2 - - Google Patents
Info
- Publication number
- JPH0220575B2 JPH0220575B2 JP26262985A JP26262985A JPH0220575B2 JP H0220575 B2 JPH0220575 B2 JP H0220575B2 JP 26262985 A JP26262985 A JP 26262985A JP 26262985 A JP26262985 A JP 26262985A JP H0220575 B2 JPH0220575 B2 JP H0220575B2
- Authority
- JP
- Japan
- Prior art keywords
- solution
- cation exchange
- liquid
- perrhenate
- exchange resin
- 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
Links
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 14
- 239000003729 cation exchange resin Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 239000011591 potassium Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000007788 liquid Substances 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 5
- QSHYGLAZPRJAEZ-UHFFFAOYSA-N 4-(chloromethyl)-2-(2-methylphenyl)-1,3-thiazole Chemical compound CC1=CC=CC=C1C1=NC(CCl)=CS1 QSHYGLAZPRJAEZ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000004040 coloring Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 208000005156 Dehydration Diseases 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229940023913 cation exchange resins Drugs 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Description
【発明の詳細な説明】
発明の技術分野
本発明は、過レニウム酸アンモニウムの製造方
法に関する。DETAILED DESCRIPTION OF THE INVENTION Technical Field of the Invention The present invention relates to a method for producing ammonium perrhenate.
発明の従来技術
従来過レニウム酸アンモニウムを製造する方法
としては、アンモニアで飽和した過レニウム酸溶
液を蒸発する方法、過レニウム酸バリウム溶液に
硫酸アンモニウムあるいは炭酸アンモニウム溶液
を加える方法等が行われている。Prior Art of the Invention Conventionally, methods for producing ammonium perrhenate include a method of evaporating a perrhenic acid solution saturated with ammonia, a method of adding an ammonium sulfate or ammonium carbonate solution to a barium perrhenate solution, and the like.
本発明においては、過レニウム酸カリ溶液を出
発原料として、容易に過レニウム酸アンモニウム
を製造する方法を検討した。 In the present invention, a method for easily producing ammonium perrhenate using a potassium perrhenate solution as a starting material was studied.
発明の構成
本発明は、即ち、
(1) 過レニウム酸カリ溶液を陽イオン交換樹脂と
接触後、精製液をアンモニア水で中和し、過
する過レニウム酸アンモニウムの製造方法。Components of the Invention The present invention provides: (1) A method for producing ammonium perrhenate, which comprises contacting a potassium perrhenate solution with a cation exchange resin, neutralizing the purified solution with aqueous ammonia, and filtering the solution.
(2) 中和後液を90〜105℃加温し濃縮後、冷却す
る(1)記載の過レニウム酸アンモニウムの製造方
法。(2) The method for producing ammonium perrhenate according to (1), wherein the neutralized solution is heated to 90 to 105°C, concentrated, and then cooled.
(3) 陽イオン交換樹脂の洗浄及び又はアンモニア
中和後の過において純水を用いる(1)記載の過
レニウム酸アンモニウムの製造方法。(3) The method for producing ammonium perrhenate according to (1), in which pure water is used in washing the cation exchange resin and/or filtering after neutralizing ammonia.
発明の具体的説明
過レニウム酸カリを水に溶解する。または、過
レニウム酸カリの溶液を処理対象液とする。DETAILED DESCRIPTION OF THE INVENTION Potassium perrhenate is dissolved in water. Alternatively, a solution of potassium perrhenate is used as the liquid to be treated.
該液と陽イオン交換樹脂と接触し、カリウムそ
の他の微量の不純物を液から除去する。 The liquid is brought into contact with a cation exchange resin to remove potassium and other trace impurities from the liquid.
このときの液のPHは、１以下であることが好ま
しい。溶解度が、充分あるからである。 The pH of the liquid at this time is preferably 1 or less. This is because it has sufficient solubility.
接触の容量比は、上該樹脂に対し、１〜３倍容
量／時間の上記処理液を接することが好ましい。 The volume ratio of the contact is preferably 1 to 3 times the volume/hour of the treatment liquid to the resin.
処理液温度は常温から50℃で良いが、好ましく
は、30〜50℃である。 The temperature of the treatment solution may range from room temperature to 50°C, but preferably from 30 to 50°C.
温度があまり低いとKReO4の溶解度が低くな
り、取扱い液量が多くなるためである。 This is because if the temperature is too low, the solubility of KReO 4 will be low and the amount of liquid to be handled will be large.
また、あまり温度が高いと、樹脂が劣化し好ま
しくないためである。 Moreover, if the temperature is too high, the resin will deteriorate, which is not preferable.
陽イオン交換樹脂としては、例えばスチレン系
強酸性陽イオン交換樹脂がある。 Examples of the cation exchange resin include styrene-based strongly acidic cation exchange resins.
例えば、下記の構造のものである。 For example, it has the following structure.
陽イオン交換樹脂と、過レニウム酸カリ溶液と
接する前は、過工程を経由し、不溶解残渣は予
め除去しておくことが望ましい。 Before contacting the cation exchange resin with the potassium perrhenate solution, it is desirable to remove undissolved residues in advance through a step.
また、使用する溶解水等は、純水を用いること
が好ましい。製品となる過レニウム酸が着色する
ことがあるためである。 Moreover, it is preferable to use pure water as the dissolution water and the like. This is because the perrhenic acid product may become colored.
陽イオン交換樹脂と接触した処理後液中には、
Ｋのほとんど含まない液となつている。例えば、
処理液中0.001ｇ／以下となるのである。 In the treated solution that came into contact with the cation exchange resin,
The liquid contains almost no K. for example,
The amount is 0.001g/or less in the processing solution.
陽イオン交換樹脂には、カリウムおよび他の不
純物が回収された。他の不純物としては、Fe，
Hg，Se等があつた。レニウムは、ほとんど吸着
されず、分布率としては0.1％以下であつた。 Potassium and other impurities were recovered in the cation exchange resin. Other impurities include Fe,
Hg, Se, etc. were present. Rhenium was hardly adsorbed, and the distribution ratio was less than 0.1%.
陽イオン交換樹脂は、吸着後、好ましくは純水
で洗浄される。過レニウム酸に着色が生じないよ
うにするためである。 After adsorption, the cation exchange resin is preferably washed with pure water. This is to prevent coloring of perrhenic acid.
さらに、陽イオン交換樹脂と接触し、得られる
後液（精製液）にアンモニア水を加え中和する。 Furthermore, it is brought into contact with a cation exchange resin, and aqueous ammonia is added to the resulting liquid (purified liquid) to neutralize it.
中和後、過するのであるが、好ましくは90〜
105℃に加温し、濃縮する。温度は、高いほど良
いが、あまり高いとレニウムが揮発ロスするので
好ましくない。その後冷却し、過あるいは脱水
処理する方が、より過時間、過設備が不要と
なり好ましい。 After neutralization, the temperature is preferably 90~
Warm to 105°C and concentrate. The higher the temperature, the better; however, if the temperature is too high, rhenium will volatilize and be lost, which is not preferable. After that, it is preferable to cool and perform filtration or dehydration treatment because it requires less time and equipment.
中和後の過等においても、純水を用いて、洗
浄を行うことが好ましい。 Even in the filtration after neutralization, it is preferable to use pure water for washing.
製品である過レニウム酸アンモニウムの着色を
防止できるからである。 This is because the product, ammonium perrhenate, can be prevented from coloring.
純水を用いることにより、着色防止のため活性
炭に液を通過させることを要しなくなるのであ
る。 By using pure water, there is no need to pass the liquid through activated carbon to prevent coloring.
発明の効果
以上のように本発明を実施することにより、以
下の効果を得ることができた。Effects of the Invention By implementing the present invention as described above, the following effects could be obtained.
(1) 高純度の過レニウム酸アンモニウムが、容易
に得られる。(1) High purity ammonium perrhenate can be easily obtained.
(2) 取扱い液量を、極力減らした状態で処理が可
能である。(2) Processing is possible with the amount of liquid handled being reduced as much as possible.
(3) 活性炭を使用せずとも、過レニウム酸アンモ
ニウムに着色が生じないものを製造し得る。(3) It is possible to produce ammonium perrhenate without coloration without using activated carbon.
実施例
過レニウム酸カリを純水に溶解し、過し溶解
後液と陽イオン交換樹脂である、スチレン系強酸
性陽イオン交換樹脂SK−IB（商品名；三菱化成
(株)製造）と接触させた。Example Potassium perrhenate was dissolved in pure water, and the solution after filtration and the cation exchange resin were styrene-based strongly acidic cation exchange resin SK-IB (trade name: Mitsubishi Kasei Co., Ltd.).
Manufacturing Co., Ltd.).
液温度40℃、液組成はRe15.4ｇ／，K3.29
ｇ／であつた液が接触後、後液中にRe15.3
ｇ／，K0.001ｇ／以下の液が得られた。 Liquid temperature 40℃, liquid composition Re15.4g/, K3.29
After contact with the hot liquid, Re15.3
g/, K0.001 g/or less liquid was obtained.
上記樹脂は、接触後純水で、吸着したＫを除い
た。 After contacting the resin, adsorbed K was removed with pure water.
上記の実施において用いた水は、純水を用いた
ため、活性炭を用いずとも過レニウム酸には着色
が生じなかつた。 Since the water used in the above implementation was pure water, perrhenic acid was not colored even if activated carbon was not used.
さらに、前記樹脂に接触後、後液にアンモニア
水を添加し、過レニウム酸アンモニウムを得る。 Furthermore, after contacting the resin, aqueous ammonia is added to the after-liquid to obtain ammonium perrhenate.
この際、アンモニア水添加後、100℃に加熱し、
Re濃度で15.3ｇ／から200ｇ／までに濃縮し
た。 At this time, after adding ammonia water, heat to 100℃,
The Re concentration was concentrated from 15.3g/ to 200g/.
濃縮後過し、純水で洗浄後、純白の過レニウ
ム酸アンモニウムを得た。 After concentration, filtration, and washing with pure water, pure white ammonium perrhenate was obtained.
純水を用いない場合は、黄かつ色を程するため
処理液を活性炭に通過させることを要したが、本
方法によりそのような煩雑な操作は不要であつ
た。 When pure water is not used, it is necessary to pass the treatment liquid through activated carbon to reduce the yellow color, but this method eliminates the need for such complicated operations.
Claims (1)
接触後、精製液をアンモニア水で中和し、過す
ることを特徴とする過レニウム酸アンモニウムの
製造方法。 ２ 中和後液を90〜105℃加温し濃縮後、冷却す
ることを特徴とする特許請求の範囲第１項記載の
過レニウム酸アンモニウムの製造方法。 ３ 陽イオン交換樹脂の洗浄及び又はアンモニア
中和後の過において純水を用いることを特徴と
する特許請求の範囲第１項記載の過レニウム酸ア
ンモニウムの製造方法。[Claims] 1. A method for producing ammonium perrhenate, which comprises contacting a potassium perrhenate solution with a cation exchange resin, neutralizing the purified solution with aqueous ammonia, and filtering. 2. The method for producing ammonium perrhenate according to claim 1, wherein the neutralized solution is heated to 90 to 105°C, concentrated, and then cooled. 3. The method for producing ammonium perrhenate according to claim 1, characterized in that pure water is used in the washing of the cation exchange resin and/or in the filtering after neutralizing ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26262985A JPS62123021A (en) | 1985-11-25 | 1985-11-25 | Production of ammonium perrhenate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26262985A JPS62123021A (en) | 1985-11-25 | 1985-11-25 | Production of ammonium perrhenate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62123021A JPS62123021A (en) | 1987-06-04 |
| JPH0220575B2 true JPH0220575B2 (en) | 1990-05-09 |
Family
ID=17378446
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26262985A Granted JPS62123021A (en) | 1985-11-25 | 1985-11-25 | Production of ammonium perrhenate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62123021A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9624561B2 (en) | 2012-12-28 | 2017-04-18 | Pan Pacific Copper Co., Ltd. | Method for producing aqueous solution of perrhenic acid from rhenium sulfide |
| US9631259B2 (en) | 2012-12-28 | 2017-04-25 | Pan Pacific Copper Co., Ltd. | Method for producing aqueous solution of perrhenic acid from rhenium sulfide |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008026910A1 (en) * | 2008-06-05 | 2009-12-10 | H.C. Starck Gmbh | Process for the preparation of pure ammonium barrier phenate |
| JP5378813B2 (en) * | 2009-01-23 | 2013-12-25 | Ｄｏｗａメタルマイン株式会社 | Rhenium recovery method |
| JP5375664B2 (en) * | 2010-02-26 | 2013-12-25 | 住友金属鉱山株式会社 | Method for producing ammonium perrhenate |
| JP6314044B2 (en) * | 2014-07-01 | 2018-04-18 | パンパシフィック・カッパー株式会社 | Method for producing aqueous perrhenic acid solution from crude rhenium sulfide |
| JP6317197B2 (en) * | 2014-07-01 | 2018-04-25 | パンパシフィック・カッパー株式会社 | Method for producing perrhenic acid aqueous solution, method for producing potassium perrhenate, method for producing ammonium perrhenate, and method for producing rhenium metal |
| JP6317196B2 (en) * | 2014-07-01 | 2018-04-25 | パンパシフィック・カッパー株式会社 | Method for producing perrhenic acid aqueous solution and method for producing potassium perrhenate, ammonium perrhenate and rhenium metal using the same |
| CN115072789A (en) * | 2022-08-08 | 2022-09-20 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of high-purity ammonium rhenate |
-
1985
- 1985-11-25 JP JP26262985A patent/JPS62123021A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9624561B2 (en) | 2012-12-28 | 2017-04-18 | Pan Pacific Copper Co., Ltd. | Method for producing aqueous solution of perrhenic acid from rhenium sulfide |
| US9631259B2 (en) | 2012-12-28 | 2017-04-25 | Pan Pacific Copper Co., Ltd. | Method for producing aqueous solution of perrhenic acid from rhenium sulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62123021A (en) | 1987-06-04 |
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