JP2002180140A - Purification method of platinum sponge - Google Patents
Purification method of platinum spongeInfo
- Publication number
- JP2002180140A JP2002180140A JP2000379597A JP2000379597A JP2002180140A JP 2002180140 A JP2002180140 A JP 2002180140A JP 2000379597 A JP2000379597 A JP 2000379597A JP 2000379597 A JP2000379597 A JP 2000379597A JP 2002180140 A JP2002180140 A JP 2002180140A
- Authority
- JP
- Japan
- Prior art keywords
- platinum
- sponge
- sponge platinum
- washing
- chlorine
- 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
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000000746 purification Methods 0.000 title 1
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 43
- 239000000460 chlorine Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 22
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 7
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
(57)【要約】
【課題】スポンジ白金の精製方法
【解決手段】塩素品位が0.01重量%以下の高品位の
スポンジ白金を得ることができるスポンジ白金の精製方
法を提供する。
【解決手段】塩化白金酸アンモンを350〜450℃で
加熱して塩素分およびアンモニアを分解し、次いで、さ
らに昇温して850〜950℃でスポンジ白金を加熱
し、次いで、このスポンジ白金を粉砕することなく40
0g/L以下のパルプ濃度で、2回以上洗浄する方法。(57) Abstract: A method for purifying sponge platinum. A method for purifying sponge platinum capable of obtaining high-grade sponge platinum having a chlorine grade of 0.01% by weight or less. SOLUTION: Ammonium chloroplatinate is heated at 350 to 450 ° C. to decompose chlorine and ammonia, and then heated further to heat sponge platinum at 850 to 950 ° C. Then, the sponge platinum is pulverized. 40 without doing
A method of washing twice or more at a pulp concentration of 0 g / L or less.
Description
【0001】[0001]
【発明の属する技術分野】本発明は、塩化白金酸アンモ
ンからスポンジ白金を精製する白金の精製方法に係り、
特に、スポンジ白金に付着した塩素を効率的に除去して
高品位のスポンジ白金を得る技術に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for purifying sponge platinum from ammonium chloroplatinate and to a method for purifying platinum.
In particular, the present invention relates to a technique for efficiently removing chlorine adhering to sponge platinum to obtain high-quality sponge platinum.
【0002】[0002]
【従来の技術】従来、スポンジ白金の精製に際しては、
塩化白金酸アンモンを400℃程度で加熱分解し、さら
にそれを水素ガス中で800℃程度に加熱していた。こ
の最後の加熱は、白金以外の成分等である塩素を水素で
還元するとともに、スポンジを構成する粉体状の白金ど
うしを燒結させて取り易くするために行っていた。2. Description of the Related Art Conventionally, when purifying sponge platinum,
Ammonium chloroplatinate was thermally decomposed at about 400 ° C. and further heated to about 800 ° C. in hydrogen gas. This last heating was performed to reduce chlorine, which is a component other than platinum, with hydrogen, and to sinter powdery platinum constituting the sponge to facilitate removal.
【0003】[0003]
【発明が解決しようとする課題】ところで、上記のよう
な方法で精製されるスポンジ白金は、塩素を0.1〜
0.5重量%含有しているが、塩素品位をより低くし、
消費者の要請に合う製品を製造したい。また、上記従来
技術では、2回目の加熱を水素ガス雰囲気で行っている
が、水素ガスは取扱いに注意をようするため使用を避け
たいとの要請もあった。したがって、本発明は、水素還
元をすることなく塩素品位を飛躍的に低くすることがで
き、例えば塩素品位を0.01重量%以下にすることが
可能なスポンジ白金の精製方法を提供することを目的と
している。By the way, sponge platinum purified by the above-mentioned method has a chlorine content of 0.1 to 0.1%.
0.5% by weight, but lower the chlorine grade,
We want to manufacture products that meet the needs of consumers. Further, in the above-mentioned prior art, the second heating is performed in a hydrogen gas atmosphere, but there has been a request to avoid using hydrogen gas in order to pay attention to handling. Accordingly, the present invention is to provide a method for purifying sponge platinum, which can drastically lower the chlorine grade without hydrogen reduction, for example, can reduce the chlorine grade to 0.01% by weight or less. The purpose is.
【0004】[0004]
【課題を解決するための手段】本発明者らは、スポンジ
白金に塩素が含有される原因について検討した結果、最
終の加熱において蒸発した塩素がスポンジ白金のフィラ
メントの表面に再び付着するのが原因であるとの推論に
達した。そこで、加熱後のスポンジ白金を水洗したとこ
ろ、塩素品位が飛躍的に低下することを見出した。The present inventors have studied the causes of chlorine contained in platinum sponge and found that chlorine evaporated in the final heating adheres again to the surface of the filament of platinum sponge. The inference was reached. Then, when the sponge platinum after heating was washed with water, it was found that the chlorine quality was dramatically reduced.
【0005】本発明は、上記知見に基づいてなされたも
ので、 (1)塩化白金酸アンモンを350〜450℃で加熱し
て塩素分およびアンモニアを分解し、次いで、さらに昇
温して850〜950℃でスポンジ白金を加熱し、次い
で、このスポンジ白金を粉砕することなく400g/L
以下のパルプ濃度で、2回以上洗浄するスポンジ白金の
精製方法。 (2)上記(1)の2回以上の洗浄後直ちに乾燥するこ
とを特徴とするスポンジ白金の精製方法。The present invention has been made based on the above findings. (1) Ammonium chloroplatinate is heated at 350 to 450 ° C. to decompose chlorine and ammonia, and then further heated to 850 to 850 ° C. The sponge platinum is heated at 950 ° C. and then 400 g / L without grinding the sponge platinum.
A method for purifying sponge platinum which is washed at least twice with the following pulp concentrations. (2) A method for purifying platinum sponge, comprising drying immediately after washing two or more times in (1).
【0006】本発明によれば、1段目の350〜450
℃の加熱で分解した塩素分、アンモニア分更にSe等の
不純物が2段目の850〜950℃の加熱で蒸発し、白
金は、焼結する。その際、蒸発した塩素がスポンジ白金
に再付着するが、スポンジ白金を水洗することで塩素を
効率的に除去することができる。ここで、スポンジ白金
と水との比率は400g/L以下であることが望まし
い。なお、本発明では、スポンジ白金を水洗後に速やか
に乾燥することが不純物の混入を防ぐ上で望ましい。According to the present invention, the first stage 350 to 450
Impurities such as chlorine and ammonia decomposed by heating at ℃ and Se and the like are evaporated by heating at 850 to 950 ° C. in the second stage, and platinum is sintered. At this time, the evaporated chlorine adheres again to the sponge platinum, but the chlorine can be efficiently removed by washing the sponge platinum with water. Here, the ratio of sponge platinum to water is desirably 400 g / L or less. In the present invention, it is desirable to dry the sponge platinum quickly after washing with water in order to prevent contamination of impurities.
【0007】[0007]
【実施例1】次に実施例を示して、本発明をさらに詳細
に説明する。塩化白金酸アンモンを大気中で400℃で
2時間加熱し、次いで加熱炉を900℃に昇温して3時
間保持した。こうして得たロットの異なる2種類のスポ
ンジ白金を3,000g、及び4,000g採取した。
次いで、洗浄タンクに純水を10Lを注入し、その中に
スポンジ白金をそれぞれ入れて、30分間攪拌洗浄し
た。その後、濾過を行い分析試料用試料として、数gの
洗浄濾過後のスポンジ白金を採取して分析した。この操
作を2回行った。なお、2回目の水洗は、その都度純水
を新しいものに取替えて行った。Embodiment 1 Next, the present invention will be described in more detail with reference to embodiments. Ammonium chloroplatinate was heated in the air at 400 ° C. for 2 hours, and then the heating furnace was heated to 900 ° C. and held for 3 hours. 3,000 g and 4,000 g of two kinds of sponge platinum from different lots thus obtained were collected.
Next, 10 L of pure water was poured into the washing tank, and sponge platinum was put into each of the tanks and washed with stirring for 30 minutes. Thereafter, filtration was performed, and several g of the sponge platinum after washing and filtration was collected and analyzed as a sample for an analysis sample. This operation was performed twice. The second washing was carried out by replacing the pure water with new one each time.
【0008】洗浄前、1回目洗浄後、2回目洗浄後のス
ポンジ白金中のCl品位を表1に示す。[0008] Table 1 shows the Cl grade in the sponge platinum before washing, after the first washing, and after the second washing.
【0009】[0009]
【表1】 [Table 1]
【0010】表1より、実施例1の純水量に対するスポ
ンジ白金の割合が300g/Lの条件では、スポンジ白金
中のCl品位は洗浄前の0.40%が1回目洗浄で0.
02%まで低減し、更に洗浄を繰り返すと<0.01%
まで低下した。また、実施例2の純水量に対するスポン
ジ白金の割合が400g/Lの条件では、スポンジ白金中
のCl品位は0.4%が1回目洗浄までに0.03%ま
で低減し、更に洗浄を繰り返すと<0.01%まで低下
して、管理値の0.01%未満を満足する。一方表1の
比較例1では、500g/Lとスポンジ白金のパルプ濃度
が高いために、第1回洗浄に於いて0.05%と高く、
第2回洗浄においても0.02%と低い値とならなかっ
た。According to Table 1, under the condition that the ratio of sponge platinum to the pure water amount in Example 1 is 300 g / L, the Cl grade in the sponge platinum is 0.40% before washing and is 0.1% in the first washing.
02% and <0.01% after repeated washing
Down to Further, under the condition that the ratio of the sponge platinum to the pure water amount in Example 2 was 400 g / L, the Cl grade in the sponge platinum was reduced from 0.4% to 0.03% by the first washing, and further washing was repeated. And <0.01%, satisfying less than 0.01% of the control value. On the other hand, in Comparative Example 1 of Table 1, since the pulp concentration of the sponge platinum was as high as 500 g / L, it was as high as 0.05% in the first washing.
Even in the second washing, the value was not as low as 0.02%.
【0011】表1に示すように、スポンジ白金のパルプ
濃度が400g/L以下の場合は、洗浄の水洗回数を2回
行えば、スポンジ白金中の塩素品位はいずれも0.01
重量%未満であり、十分な品位を備えている。これに対
して水洗を行わない場合には、スポンジ白金の塩素品位
は0.1〜0.4重量%であり、本発明と比較してかな
り低品位であった。As shown in Table 1, when the pulp concentration of the sponge platinum is 400 g / L or less, if the number of times of washing is twice, the chlorine quality in the sponge platinum becomes 0.01.
It is less than 10% by weight and has sufficient quality. On the other hand, when the washing was not performed, the chlorine grade of the sponge platinum was 0.1 to 0.4% by weight, which was considerably lower than that of the present invention.
【0012】[0012]
【発明の効果】以上のように、本発明のスポンジ白金の
精製方法においては、塩化白金酸アンモンを350〜4
50℃で加熱して塩素分およびアンモニア分を分解し、
次いで、さらに昇温して850〜950℃でスポンジ白
金を加熱し、次いで、スポンジ白金を2回以上400/L
以下のスポンジ白金の低いパルプ濃度において、水洗す
ることにより、水素還元を行うことなく塩素品位の低い
高品位のスポンジ白金を得ることができる。As described above, in the method for purifying sponge platinum of the present invention, ammonium chloroplatinate is used in an amount of 350 to 4%.
Heat at 50 ° C to decompose chlorine and ammonia,
Next, the temperature was further increased to heat the sponge platinum at 850 to 950 ° C., and then the sponge platinum was heated twice or more at 400 / L
By washing with water at the following low pulp concentration of sponge platinum, high-grade sponge platinum with low chlorine grade can be obtained without performing hydrogen reduction.
Claims (2)
加熱して塩素分およびアンモニアを分解し、次いで、さ
らに昇温して850〜950℃でスポンジ白金を加熱
し、次いで、このスポンジ白金を粉砕することなく40
0g/L以下のパルプ濃度で、2回以上洗浄することを
特徴とするスポンジ白金の精製方法。(1) Ammonium chloroplatinate is heated at 350 to 450 ° C. to decompose chlorine and ammonia, and then heated to 850 to 950 ° C. to heat the sponge platinum. 40 without crushing
A method for purifying sponge platinum, comprising washing at least twice with a pulp concentration of 0 g / L or less.
ることを特徴とするスポンジ白金の精製方法。2. A method for purifying sponge platinum, comprising drying immediately after washing two or more times according to claim 1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000379597A JP2002180140A (en) | 2000-12-14 | 2000-12-14 | Purification method of platinum sponge |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000379597A JP2002180140A (en) | 2000-12-14 | 2000-12-14 | Purification method of platinum sponge |
Publications (1)
Publication Number | Publication Date |
---|---|
JP2002180140A true JP2002180140A (en) | 2002-06-26 |
Family
ID=18847929
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2000379597A Pending JP2002180140A (en) | 2000-12-14 | 2000-12-14 | Purification method of platinum sponge |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2002180140A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006089808A (en) * | 2004-09-24 | 2006-04-06 | Nippon Mining & Metals Co Ltd | Sponge platinum deoxygenation method, hydrogen reduction furnace used in said method, and sponge platinum pulverization method |
-
2000
- 2000-12-14 JP JP2000379597A patent/JP2002180140A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006089808A (en) * | 2004-09-24 | 2006-04-06 | Nippon Mining & Metals Co Ltd | Sponge platinum deoxygenation method, hydrogen reduction furnace used in said method, and sponge platinum pulverization method |
CN1318620C (en) * | 2004-09-24 | 2007-05-30 | 日矿金属株式会社 | Spongy platinum deoxidation method and hydrogen reducing furnace using the method and spongy platinum crushing method |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
A711 | Notification of change in applicant |
Free format text: JAPANESE INTERMEDIATE CODE: A712 Effective date: 20060510 |