JP5556681B2 - Method for producing readily soluble sponge platinum - Google Patents
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Description
本発明は、白金粉末の製造方法に関し、更に詳しくは王水に溶解する際に溶解残渣が実質的に発生しない白金粉末の製造方法に関する。 The present invention relates to a method for producing platinum powder, and more particularly to a method for producing platinum powder in which a dissolution residue is not substantially generated when dissolved in aqua regia.
従来から、白金粉末(以下、スポンジ白金と称する)の製造方法としては、塩酸酸性の白金溶液に塩化アンモニウムを添加して塩化白金酸アンモニウム(白金ケーキとも言われる:(NH4)2PtCl6)を得、これに水酸化ナトリウム(苛性ソーダ)等のアルカリを添加して溶解し、この溶液にヒドラジンなどの還元剤を添加して白金を沈殿させ、濾過及び洗浄した後、乾燥させてスポンジ白金を得ることが行われてきた。 Conventionally, as a method for producing platinum powder (hereinafter referred to as sponge platinum), ammonium chloride is added to an acidic platinum solution by adding ammonium chloride (also referred to as platinum cake: (NH 4 ) 2 PtCl 6 ). This is dissolved by adding an alkali such as sodium hydroxide (caustic soda), and a reducing agent such as hydrazine is added to this solution to precipitate platinum, filtered and washed, and then dried to obtain sponge platinum. It has been done.
上記の湿式法で製造されたスポンジ白金は、概ね粒径10μm程度の微細な粉末として得られる場合が多く、この湿潤状態のスポンジ白金を洗浄及び乾燥して製品としている。また、スポンジ白金を他の粉体と混合してペーストを製造する場合、粒度が10μm程度のものが良好な混合性を有するため好ましいとされている。更に、10μm程度の粒径のスポンジ白金は王水に溶解し、白金を含有する化合物などを製造する中間製品としても取り扱い易いという特長がある。このため、スポンジ白金の粒度は10μm程度を目安にすることが多かった。 Sponge platinum produced by the above wet method is often obtained as a fine powder having a particle size of approximately 10 μm, and the wet sponge platinum is washed and dried to produce a product. Further, when a paste is produced by mixing sponge platinum with other powders, those having a particle size of about 10 μm are preferred because they have good mixing properties. Furthermore, sponge platinum having a particle size of about 10 μm is featured in that it can be easily handled as an intermediate product for producing a compound containing platinum by dissolving in aqua regia. For this reason, the particle size of sponge platinum is often about 10 μm.
ところが、10μm程度の微細な粉末粒子の表面は酸化され易い性質がある。そのため、上記従来の方法で得られた粒径が10μm程度のスポンジ白金においても、その表面での酸化物の生成を完全に防ぐことは実質的に困難である。その結果、スポンジ白金の表面が酸化されると、王水を加えて溶解する際に溶解され難く、溶解残渣が発生する。具体的な例として、粒径が10μm程度のスポンジ白金の場合、スポンジ白金のおよそ2〜10重量%は王水に溶解しない酸化物の状態で存在することが知られている。 However, the surface of fine powder particles of about 10 μm is easily oxidized. Therefore, even in the case of sponge platinum having a particle size of about 10 μm obtained by the above conventional method, it is substantially difficult to completely prevent the formation of oxide on the surface. As a result, when the surface of the sponge platinum is oxidized, it is difficult to dissolve when the aqua regia is added and dissolved, and a dissolution residue is generated. As a specific example, in the case of sponge platinum having a particle size of about 10 μm, it is known that approximately 2 to 10% by weight of the sponge platinum exists in an oxide state that does not dissolve in aqua regia.
スポンジ白金を王水に溶解する際に溶解残渣が発生すると、溶解液との濾別が必要となるうえ、溶解残渣を繰り返して再度処理する必要がある。そのため、多くの手間がかかるうえ、溶解残渣を再処理するためにコストの増加をもたらし、生産性を低下させるなどの不都合が生じていた。 When a dissolved residue is generated when sponge platinum is dissolved in aqua regia, it is necessary to separate the dissolved residue from the solution, and it is necessary to repeatedly process the dissolved residue again. For this reason, it takes a lot of time and reprocessing the dissolved residue, resulting in an increase in cost and a decrease in productivity.
溶解残渣の発生を抑制するためには、スポンジ白金における酸化物の生成をできるだけ抑制すると共に、生成した酸化物をメタルに戻すことが望ましい。例えば、特許文献1には、白金の溶解残渣を低減するための技術として、スポンジ白金を予め2mm以下に粗粉砕し、還元炉に入れて水素ガスを流しながら600〜800℃の温度に保持して脱酸素を行う方法が記載されている。この方法によれば、スポンジ白金中の酸化物が除去されるため、王水に溶解する際の溶解速度が向上し、溶解残渣を低減できるとされている。 In order to suppress the generation of dissolution residues, it is desirable to suppress the generation of oxide in sponge platinum as much as possible and return the generated oxide to metal. For example, in Patent Document 1, as a technique for reducing the dissolution residue of platinum, sponge platinum is coarsely pulverized to 2 mm or less in advance, and is placed in a reduction furnace and maintained at a temperature of 600 to 800 ° C. while flowing hydrogen gas. A method for performing deoxygenation is described. According to this method, since the oxide in the sponge platinum is removed, the dissolution rate when dissolved in aqua regia is improved, and the dissolution residue can be reduced.
しかしながら、特許文献1のような高温下において水素ガスを用いた還元炉で操業を行うことは、水素ガスが爆発する危険性があるため、防爆仕様の機器の使用並びに警報装置や遮断装置の設置、更に換気など厳重な安全対策が必要となる。このため設備投資や管理費用がかさむうえ、水素ガス自体のコストも無視できないことから、工業的に容易に実施できる方法とはいえなかった。 However, operating in a reducing furnace using hydrogen gas at a high temperature as in Patent Document 1 has a risk of explosion of hydrogen gas, so use of explosion-proof equipment and installation of alarm devices and shut-off devices In addition, strict safety measures such as ventilation are required. For this reason, capital investment and management costs increase, and the cost of hydrogen gas itself cannot be ignored. Therefore, it cannot be said that the method can be easily implemented industrially.
また、水素を用いた還元を白金などのように水素を吸蔵しやすいメタルの処理に用いると、供給された水素が白金メタル中に吸蔵され、反応終了後に大気雰囲気に接したとき発熱ないし発火して再酸化が促進されることがある。このため、水素還元が終わった後、炉内を減圧するか若しくは不活性ガスに置換するなどの方法を用いて、白金に吸蔵された水素ガスを放出させる処理を施す必要であった。 In addition, when reduction using hydrogen is used for the treatment of metals that easily store hydrogen, such as platinum, the supplied hydrogen is stored in platinum metal, and it generates heat or ignites when it comes into contact with the atmosphere after the reaction is completed. Reoxidation may be promoted. For this reason, after the hydrogen reduction is completed, it is necessary to perform a process of releasing the hydrogen gas occluded in platinum by using a method such as depressurizing the inside of the furnace or replacing the furnace with an inert gas.
本発明は、上記した従来のスポンジ白金の製造方法における問題点に鑑み、操業が簡単で且つ操業中の安全に関するリスクがなく、コスト的にも有利であって、王水に溶解する際に簡単に溶解して溶解残渣が発生しない、易溶性のスポンジ白金の製造方法を提供することを目的とする。 In view of the above-described problems in the conventional method for producing sponge platinum, the present invention is easy to operate, has no risk regarding safety during operation, is advantageous in terms of cost, and is simple when dissolved in aqua regia. It is an object of the present invention to provide a method for producing easily soluble sponge platinum which is not dissolved in a solution and does not generate a dissolution residue.
上記目的を達成するため本発明が提供する易溶性スポンジ白金の製造方法は、塩化白金酸アンモニウムにアルカリを加えて溶解し、得られた溶液に還元剤を添加してスポンジ白金を得た後、分離回収した湿潤状態のスポンジ白金を800〜1000℃の温度に昇温して焙焼し、得られた焙焼物を解砕することを特徴とするものである。 In order to achieve the above object, the method for producing a readily soluble sponge platinum provided by the present invention is obtained by adding alkali to ammonium chloroplatinate to dissolve it, and after adding a reducing agent to the resulting solution to obtain sponge platinum, The wet platinum sponge separated and recovered is heated to a temperature of 800 to 1000 ° C. and baked, and the obtained baked product is crushed.
上記本発明の易溶性スポンジ白金の製造方法においては、前記焙焼を不活性雰囲気中にて行うことが好ましい。また、前記焙焼物を解砕する際には、粒径が1〜3mmの範囲になるように解砕することが好ましい。 In the method for producing the readily soluble sponge platinum of the present invention, the roasting is preferably performed in an inert atmosphere. Moreover, when crushing the roasted product, it is preferable to crush so that the particle diameter is in the range of 1 to 3 mm.
本発明によれば、安全で且つコスト的にも有利な方法により、王水に容易に溶解して溶解残渣が発生しないスポンジ白金を製造することができる。 ADVANTAGE OF THE INVENTION According to this invention, sponge platinum which melt | dissolves easily in aqua regia and does not generate | occur | produce a melt | dissolution residue can be manufactured by a safe and cost-effective method.
本発明は、湿式法により塩化白金酸アンモニウムからスポンジ白金を得る工程と、得られたスポンジ白金を湿潤状態のまま焙焼する工程と、その焙焼物を解砕する工程とからなる。更に具体的には、スポンジ白金を得る工程では、公知の湿式法に従って、塩化白金酸アンモニウムを苛性ソーダなどに溶解してアルカリ溶液とし、ヒドラジン等の還元剤により白金を還元し、生成したスポンジ白金を固液分離して回収する。 The present invention comprises a step of obtaining sponge platinum from ammonium chloroplatinate by a wet method, a step of roasting the obtained sponge platinum in a wet state, and a step of crushing the roasted product. More specifically, in the step of obtaining sponge platinum, according to a known wet method, ammonium chloroplatinate is dissolved in caustic soda to obtain an alkaline solution, and platinum is reduced by a reducing agent such as hydrazine, and the produced sponge platinum is obtained. Collect by solid-liquid separation.
湿式法により塩化白金酸アンモニウムから得られたスポンジ白金は、次の焙焼工程に移る前に洗浄することが好ましい。例えば、回収したスポンジ白金を純水中に懸濁させ、撹拌することにより付着している還元母液を分離する。このようにして得られた湿潤状態のスポンジ白金を次の焙焼工程に供給する。 Sponge platinum obtained from ammonium chloroplatinate by a wet method is preferably washed before moving to the next roasting step. For example, the recovered sponge platinum is suspended in pure water and stirred to separate the attached reduced mother liquor. The wet sponge platinum thus obtained is supplied to the next roasting step.
ここで、湿潤状態のスポンジ白金とは、例えば、常温下で固液分離し若しくは更に洗浄した後のスポンジ白金で、表面が水分によりコーティングされている程度の水分状態のものを言う。尚、スポンジ白金の湿潤状態での具体的な水分率については、一概に規定できないが、スポンジ白金の表面が水分によりコーティングされる程度、具体的には数〜20重量%程度であることが好ましい。 Here, the sponge platinum in a wet state refers to, for example, sponge platinum that has been subjected to solid-liquid separation or further washing at room temperature, and is in a moisture state in which the surface is coated with moisture. The specific moisture content of the sponge platinum in a wet state cannot be generally specified, but is preferably such that the surface of the sponge platinum is coated with moisture, specifically about several to 20% by weight. .
上記の湿潤状態のスポンジ白金は、次の焙焼工程において、湿潤状態のまま加熱炉などに装入し、大気雰囲気若しくは不活性ガス雰囲気の下において800〜1000℃の範囲の温度まで昇温して焙焼する。この焙焼処理によって、スポンジ白金中に含まれている水分は熱分解して分離される。尚、加熱炉としては、通常の電気炉などを用いることができる。 In the next roasting step, the sponge platinum in the wet state is charged into a heating furnace or the like in a wet state, and heated to a temperature in the range of 800 to 1000 ° C. in an air atmosphere or an inert gas atmosphere. And roast it. By this roasting treatment, the moisture contained in the sponge platinum is thermally decomposed and separated. In addition, a normal electric furnace etc. can be used as a heating furnace.
上記焙焼処理の温度(焙焼温度)が800℃未満では、得られるスポンジ白金の王水への溶解性が悪くなる。逆に焙焼温度が1000℃を超えると、焙焼が進み過ぎて塊状のスポンジ白金が生成し、ハンドリングが難しくなるなどの不都合が生じるため好ましくない。尚、目標とする焙焼温度は、予め少量での焙焼テストを実施して、得られるスポンジ白金の解砕後の粒径が最適な粒径になる焙焼温度を求めれば良い。また、室温からの昇温時間、即ち昇温時の温度勾配は特に限定されるものではない。 If the temperature of the roasting treatment (roasting temperature) is less than 800 ° C., the solubility of the resulting sponge platinum in aqua regia is poor. On the other hand, if the roasting temperature exceeds 1000 ° C., roasting proceeds too much to produce lump sponge platinum, which is not preferable because handling becomes difficult. The target roasting temperature may be obtained by conducting a roasting test with a small amount in advance and obtaining the roasting temperature at which the particle size after crushing of the obtained sponge platinum is optimum. Further, the temperature rise time from room temperature, that is, the temperature gradient at the time of temperature rise is not particularly limited.
上記焙焼処理に要する時間(焙焼時間)は、スポンジ白金の水分率や焙焼温度によって異なるが、所定の焙焼温度に到達後少なくとも5分以上保持することが好ましい。また、焙焼雰囲気については、酸素を供給するなど極端に酸化を促進する雰囲気でなければ良く、通常の大気雰囲気中で行うことも可能であるが、窒素やアルゴンなどの不活性ガス雰囲気がより好ましい。 The time required for the roasting treatment (roasting time) varies depending on the moisture content of the sponge platinum and the roasting temperature, but it is preferable to hold at least 5 minutes after reaching the predetermined roasting temperature. The roasting atmosphere may be an atmosphere that does not promote oxidation extremely, such as supplying oxygen, and can be performed in a normal air atmosphere, but an inert gas atmosphere such as nitrogen or argon is more suitable. preferable.
上記焙焼工程で得られた焙焼物は、簡単に解砕できる状態となっている。最後の解砕工程においては、この焙焼物を粒径が1〜3mmになるように解砕して製品とする。スポンジ白金の粒径を1〜3mmの範囲とする理由は、1mm未満では容器や袋に静電気で付着しやすくなり、秤量が困難となるなど取り扱い上の問題が生じる。更に、1mm未満の微粉は溶解時に激しい溶解反応を起こし、安全上も問題である。一方、粒径が3mmを超えると反応槽で混合にする際に分散しにくく、溶解が困難となり、また溶解槽の磨耗や破損を促進するために好ましくない。 The roasted product obtained in the roasting step is in a state that can be easily crushed. In the final crushing step, the roasted product is crushed so as to have a particle size of 1 to 3 mm to obtain a product. The reason why the particle size of the sponge platinum is in the range of 1 to 3 mm is that if it is less than 1 mm, it easily adheres to the container or bag due to static electricity, and it becomes difficult to weigh. Furthermore, a fine powder of less than 1 mm causes a severe dissolution reaction during dissolution, which is also a safety problem. On the other hand, if the particle size exceeds 3 mm, it is difficult to disperse when mixing in the reaction tank, dissolution becomes difficult, and it is not preferable because it promotes wear and breakage of the dissolution tank.
本発明においては、上記したように湿潤状態のスポンジ白金を、湿潤状態のまま加熱炉などを用いて焙焼することによって、スポンジ白金に含まれる酸化物が熱分解を開始するまでの間、スポンジ白金の表面に存在している水分が一種の保護皮膜として作用するため、スポンジ白金の再酸化を効果的に防止することができる。また、焙焼温度に達した加熱炉などに直接スポンジ白金を添加しないので、水蒸気爆発を生じる心配はなく、安全に操業することができる。 In the present invention, as described above, the sponge platinum in a wet state is roasted in a wet state using a heating furnace or the like until the oxide contained in the sponge platinum starts thermal decomposition. Since moisture present on the surface of platinum acts as a kind of protective film, reoxidation of sponge platinum can be effectively prevented. Further, since sponge platinum is not added directly to a heating furnace or the like that has reached the roasting temperature, there is no fear of causing a steam explosion, and it can be operated safely.
[実施例1]
白金を含む原料の精製により得られた塩酸酸性の白金溶液に、塩化アンモニウムを添加して塩化白金酸アンモニウムを生成させ、濾過して分離した。この塩化白金酸アンモニウムを、図1に示すように、水酸化ナトリウムに溶解した後、その溶液にヒドラジンを添加して還元し、スポンジ白金を生成させた。生成したスポンジ白金を濾別し、純水を加えてレパルプ洗浄した後、5C濾紙とヌッチェを用いて真空ポンプで吸引して濾過し、スポンジ白金から分離された水分が濾瓶内に滴下しない状態となったところで濾過を止めた。
[Example 1]
Ammonium chloride was added to a hydrochloric acid acidic platinum solution obtained by refining the raw material containing platinum to produce ammonium chloroplatinate, which was separated by filtration. As shown in FIG. 1, this ammonium chloroplatinate was dissolved in sodium hydroxide and then reduced by adding hydrazine to the solution to produce sponge platinum. The produced sponge platinum is filtered, purified water is added and washed with repulp, then filtered by suction with a vacuum pump using 5C filter paper and Nutsche, and water separated from sponge platinum is not dripped into the filter bottle. Then, the filtration was stopped.
得られた湿潤状態のスポンジ白金を坩堝に入れ、電気炉に装入して室温から900℃まで30分かけて昇温した。900℃に達した後5分間保持し、その後放冷した。回収した焙焼後のスポンジ白金は、従来の乾燥品と比べると良く焼き締まっていたが、乳鉢に入れ乳棒を用いれば手でも簡単に解砕することが可能であり、粒径1〜3mmの粉体を得ることができた。 The obtained wet sponge platinum was put in a crucible, charged in an electric furnace, and heated from room temperature to 900 ° C. over 30 minutes. After reaching 900 ° C., it was held for 5 minutes and then allowed to cool. The recovered sponge platinum after roasting was well baked compared to the conventional dry product, but it can be easily crushed by hand using a pestle in a mortar, with a particle size of 1 to 3 mm. A powder could be obtained.
次に、上記のごとく得られたスポンジ白金の粉末5gを採取し、ビーカーに入れた。これに濃塩酸40mlを添加し、次いで撹拌しながら濃硝酸13mlを徐々に添加して王水としたところ、溶液の色は透明感のあるオレンジ色となり、1時間も撹拌しないうちにスポンジ白金が完全に溶解し、ビーカーの底に溶解残渣は認められなかった。 Next, 5 g of sponge platinum powder obtained as described above was collected and placed in a beaker. To this, 40 ml of concentrated hydrochloric acid was added, and then 13 ml of concentrated nitric acid was gradually added while stirring to make aqua regia. As a result, the color of the solution became a transparent orange color, and sponge platinum was formed before stirring for 1 hour. It completely dissolved and no dissolution residue was observed at the bottom of the beaker.
[比較例1]
上記焙焼時の設定温度を700℃とした以外は、上記実施例1と同じ条件で焙焼した。得られたスポンジ白金の粉末5gを溶解試験に供し、上記実施例1と同じ方法で濃塩酸40mlを添加した後、撹拌しながら濃硝酸13mlを徐々に添加した。
[Comparative Example 1]
Roasting was performed under the same conditions as in Example 1 except that the set temperature during the roasting was set to 700 ° C. 5 g of the obtained sponge platinum powder was subjected to a dissolution test, 40 ml of concentrated hydrochloric acid was added in the same manner as in Example 1 above, and 13 ml of concentrated nitric acid was gradually added while stirring.
しかし、スポンジ白金が完全に溶解しなかったため、ビーカーをホットプレート上に載せて90℃以上に加熱した。1時間以上経過して反応がほぼ終了したと思われる状態であっても、溶液の色は黒く濁っており透明感がなかった。濾過して回収した溶解残渣の重量は、溶解試験に供したスポンジ白金の重量に対して3重量%であった。 However, since the sponge platinum was not completely dissolved, the beaker was placed on a hot plate and heated to 90 ° C. or higher. Even when the reaction seemed to be almost completed after 1 hour or more, the color of the solution was black and turbid and there was no transparency. The weight of the dissolution residue collected by filtration was 3% by weight with respect to the weight of sponge platinum subjected to the dissolution test.
[比較例2]
上記実施例1と同様にして、湿潤状態のスポンジ白金を得た。次に、図2に示す従来の方法に従って、得られたスポンジ白金を純水でレパルプ洗浄した後、乾燥機に入れて105℃にて24時間保持し、完全に乾燥したスポンジ白金を得た。得られたスポンジ白金の粒径は約10μmであった。
[Comparative Example 2]
In the same manner as in Example 1, wet platinum sponge was obtained. Next, according to the conventional method shown in FIG. 2, the obtained sponge platinum was repulped with pure water and then put into a drier and kept at 105 ° C. for 24 hours to obtain completely dried sponge platinum. The particle size of the obtained sponge platinum was about 10 μm.
上記従来の方法により得られたスポンジ白金を5g採取して溶解試験に供し、上記実施例1と同じ方法で濃塩酸40mlを添加した後、撹拌しながら濃硝酸13mlを徐々に添加した。しかし、スポンジ白金が完全に溶解しなかったため、ビーカーをホットプレート上に載せて90℃以上に加熱した。 5 g of sponge platinum obtained by the above-mentioned conventional method was collected and subjected to a dissolution test. After adding 40 ml of concentrated hydrochloric acid by the same method as in Example 1, 13 ml of concentrated nitric acid was gradually added while stirring. However, since the sponge platinum was not completely dissolved, the beaker was placed on a hot plate and heated to 90 ° C. or higher.
1時間以上経過して反応がほぼ終了したと思われる状態でも、溶液の色は黒く濁っており透明感がなかった。濾過して回収した溶解残渣の重量は、溶解試験に供したスポンジ白金の重量に対して5重量%であった。 Even in a state where the reaction was considered to be almost completed after 1 hour or more, the color of the solution was black and cloudy and there was no transparency. The weight of the dissolution residue collected by filtration was 5% by weight with respect to the weight of sponge platinum subjected to the dissolution test.
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