JPS5835242B2 - Method for producing fine particulate metal nickel powder - Google Patents
Method for producing fine particulate metal nickel powderInfo
- Publication number
- JPS5835242B2 JPS5835242B2 JP52009938A JP993877A JPS5835242B2 JP S5835242 B2 JPS5835242 B2 JP S5835242B2 JP 52009938 A JP52009938 A JP 52009938A JP 993877 A JP993877 A JP 993877A JP S5835242 B2 JPS5835242 B2 JP S5835242B2
- Authority
- JP
- Japan
- Prior art keywords
- nickel
- nickel powder
- hydrazine
- fine particulate
- producing fine
- 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
Description
【発明の詳細な説明】
この発明は微粒子状の金属ニッケル粉末の製造方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fine particulate metallic nickel powder.
従来、金属ニッケル粉末を製造する方法としては、■セ
ンド法、■電解、■水素還元、■熱分解など種々の方法
があるが、金属ニッケル粉末を工業的に製造する上で必
要な条件としては、製造が簡単で安全であり、しかも金
属ニッケルの純度が高く、液相反応で生成することがで
き、公害間項を引き起こさないなど種々の条件が要求さ
れる。Conventionally, there are various methods for producing metallic nickel powder, such as ■ send method, ■ electrolysis, ■ hydrogen reduction, and ■ thermal decomposition, but the conditions necessary for industrially producing metallic nickel powder are as follows. It is simple and safe to manufacture, has high purity metal nickel, can be produced by liquid phase reaction, and does not cause pollution, among other requirements.
上記したような条件を考慮した金属ニッケル粉末の製造
方法としては、ニッケル含有溶液にヒドラジンあるいは
ヒドラジン化合物を添加し、反応終了後の最終ｐＨが７
．０以上となるようにｐＨを調節し、攪拌しなから１０
０’Ｃ以上の温度に加熱することによって金属ニッケル
粉末を還元析出させる方法があった。A method for producing metallic nickel powder that takes into account the above conditions is to add hydrazine or a hydrazine compound to a nickel-containing solution, and adjust the final pH after the reaction to 7.
．． Adjust the pH so that it is 0 or more, and do not stir.
There is a method in which metallic nickel powder is reduced and precipitated by heating to a temperature of 0'C or higher.
しかしながらこの方法によれば、還元反応を１００℃以
上で行なわせるため、温度管理上密閉容器を用いなけれ
ばならず、また、混合溶液を高速で攪拌しなければ析出
したニッケル粉末が器壁に付着するという欠点が見られ
た。However, according to this method, since the reduction reaction is carried out at 100°C or higher, a closed container must be used for temperature control, and if the mixed solution is not stirred at high speed, the precipitated nickel powder will adhere to the vessel wall. There were drawbacks to doing so.
この発明は、このようなヒドラジンあるいは、ヒドラジ
ン化合物を還元剤として使用する金属ニッケル粉末の製
造方法をさらに押し進めたもので、ｐＨの調節が不要で
、１００℃以下の温度で加熱しても金属ニッケル粉末が
製造でき、しかも常圧下で反応させることのできる金属
ニッケル粉末の製造方法を提供せんとするものである。This invention further advances the method for producing metallic nickel powder using hydrazine or a hydrazine compound as a reducing agent, and eliminates the need for pH adjustment and produces metallic nickel powder even when heated at temperatures below 100°C. It is an object of the present invention to provide a method for producing metallic nickel powder that can be produced into powder and can be reacted under normal pressure.
すなわち、この発明の要旨とするところは、塩化ニッケ
ル、炭酸ニッケル、酢酸ニッケルのうちいずれか一種を
含むニッケル含有溶液に、ヒドラジンあるいはヒドラジ
ン化合物を添加、混合して１００℃以下で加熱すること
を特徴とするものである。That is, the gist of this invention is that hydrazine or a hydrazine compound is added to a nickel-containing solution containing any one of nickel chloride, nickel carbonate, and nickel acetate, mixed, and heated at 100°C or less. That is.
ここで、ヒドラジンあるいはヒドラジン化合物としては
、ヒドラジンはもちろん、ヒドラジンヒトラード、硫酸
ヒドラジン、硫酸ヒドラゾニウム、塩化ヒドラゾニウム
などがある。Here, examples of hydrazine or hydrazine compounds include hydrazine, hydrazine hydride, hydrazine sulfate, hydrazonium sulfate, and hydrazonium chloride.
また、加熱温度は１００００以下であるが、特に７０〜
９６°Ｃの温度範囲が金属ニッケル粉末を生成させる上
で好ましい。In addition, the heating temperature is 10,000℃ or less, but especially 70℃~
A temperature range of 96°C is preferred for producing metallic nickel powder.
炭酸ニッケルの場合は室温で攪拌するだけで、かなり金
属ニッケル粉末の生成が見られた。In the case of nickel carbonate, considerable formation of metallic nickel powder was observed just by stirring at room temperature.
また、反応時間は特に限定されないが、１５分間では一
応ニッケル析出は見られるものの、青いニッケルのうわ
ずみ液が残る。Further, the reaction time is not particularly limited, but after 15 minutes, some nickel precipitation is observed, but a blue nickel liquid remains.
６０分間反応させると、はぼ反応は終了しており、金属
ニッケル粉末を生成させるに十分な時間であることが確
認できた。It was confirmed that the reaction was completed after 60 minutes of reaction, which was sufficient time to generate metallic nickel powder.
ニッケル塩とヒドラジンあるいはヒドラジン化合物の混
合比は、たとえば塩基性炭酸ニッケルとヒドラジンヒト
ラードの場合、炭酸ニッケル１モルに対しヒドラジンヒ
トラードは３〜２０モルが適当である。As for the mixing ratio of nickel salt and hydrazine or hydrazine compound, for example, in the case of basic nickel carbonate and hydrazine hydroxide, the appropriate mixing ratio is 3 to 20 mol of hydrazine hydroxide per 1 mol of nickel carbonate.
３モル未満の場合は反応速度が遅く工業的生産には適さ
ない。If it is less than 3 moles, the reaction rate is slow and it is not suitable for industrial production.
また、２０モルを越えると歩留り、粒径において所期の
効果が得られなかった。Moreover, when the amount exceeds 20 mol, the desired effects on yield and particle size cannot be obtained.
また、この場合４モルにしたとき金属ニッケルの一次粒
子径は１μ、７モルのときは０．７μ、１４モルのとき
は０．３μであった。In this case, the primary particle diameter of metallic nickel was 1 μ when the amount was 4 mol, 0.7 μ when the amount was 7 mol, and 0.3 μ when the amount was 14 mol.
したがって還元剤量を変化させることにより用途に適し
た粒径を得ることができる。Therefore, by changing the amount of reducing agent, a particle size suitable for the application can be obtained.
以下にこの発明を実施例に従って詳述する。This invention will be described in detail below according to examples.
実施例 ＊； 第
１表に示すように、各ニッケル塩を水に溶かし、ヒドラ
ジンあるいはヒドラジン化合物を加えて混合して攪拌し
た。Example *: As shown in Table 1, each nickel salt was dissolved in water, hydrazine or a hydrazine compound was added, mixed and stirred.
このまま室温で放置しておくと少しづづ金属ニッケル粉
末が析出した。When left as it was at room temperature, metallic nickel powder gradually precipitated.
徐々に湿度を上げると青緑色のけん濁液になった。When the humidity was gradually increased, it became a blue-green suspension.
さらに温度を上げ最高温度を第１表に示す温度とすると
液は透明になった。When the temperature was further increased to the maximum temperature shown in Table 1, the liquid became transparent.
１時間放置して冷却し、室温下でグラスフィルターを用
いて液をろ過し、水洗したのちアセトンで洗浄して乾燥
した。The mixture was left to cool for 1 hour, and the liquid was filtered at room temperature using a glass filter, washed with water, and then washed with acetone and dried.
得られた各金属ニッケル粉末の粒径は第１表に示すとお
りであった。The particle size of each of the obtained metallic nickel powders was as shown in Table 1.
なお、参考例として硫酸ニッケルアンモニウム、硫酸ニ
ッケル、ギ酸ニッケル、硝酸ニッケル、水酸化ニッケル
について、第１表に示した条件で前記実施例と同様に処
理したところ、硫酸ニッケルアンモニウム、硫酸ニッケ
ルについては、金属ニッケル粉末の析出は認められなか
った。As a reference example, nickel ammonium sulfate, nickel sulfate, nickel formate, nickel nitrate, and nickel hydroxide were treated in the same manner as in the above example under the conditions shown in Table 1. As for nickel ammonium sulfate and nickel sulfate, No precipitation of metallic nickel powder was observed.
また、ギ酸ニッケル、硝酸ニッケル、水酸化ニッケルに
ついては器壁に金属ニッケル粉末がわずかに析出し、未
反応物も多く、十分な生成反応が見られなかつｆ（。In addition, for nickel formate, nickel nitrate, and nickel hydroxide, a small amount of metallic nickel powder precipitates on the vessel wall, and there are many unreacted substances, and sufficient production reaction is not observed.
第１図は実施例中、試料番号２についての顕微鏡写真（
Ｘ３０００）である。Figure 1 is a micrograph of sample number 2 in the examples (
X3000).
図から０．７μ程度の金属ニッケル粉末の生成されてい
ることが確認できる。From the figure, it can be confirmed that metallic nickel powder of about 0.7μ was produced.
以上説明したように、従来ヒドラジンあるいはヒドラジ
ン化合物を用いる場合、ｐＨ調整後１００’Ｃ，Ｉｌ上
に加熱しなければ金属ニッケル粉末の生成がみられなか
ったが、この発明によれば、塩化ニッケル、炭酸ニッケ
ル、酢酸ニッケルのうちいずれか一種を含むニッケル含
有溶液にヒドラジンあるいはヒドラジン化合物を添加、
混合して１００℃以下で加熱することによって、十分に
金属ニッケル粉末の析出が認められ、低い温度で反応さ
せることができるため、製造が簡単なばかりでなく、し
かもｐＨ調整も要らないため工程管理がきわめて容易で
あるという効果を有する。As explained above, when using hydrazine or a hydrazine compound, the formation of metallic nickel powder was not seen unless it was heated to 100'C, Il after adjusting the pH, but according to the present invention, nickel chloride, Adding hydrazine or a hydrazine compound to a nickel-containing solution containing either nickel carbonate or nickel acetate,
By mixing and heating at below 100°C, sufficient precipitation of metallic nickel powder is observed, and the reaction can be carried out at a low temperature, which not only simplifies production, but also eliminates the need for pH adjustment, which facilitates process control. This has the effect that it is extremely easy.
第１図はこの発明の実施例によって得られた金属ニッケ
ル粉末の顕微鏡写真である。FIG. 1 is a microscopic photograph of metallic nickel powder obtained according to an example of the present invention.
Claims (1)
いずれか一種を含むニッケル含有溶液に、ヒドラジンあ
るいはヒドラジン化合物を添加、混合して１００℃以下
に加熱することを特徴とする微粒子状金属ニッケル粉末
の製造方法。1. A method for producing fine particulate metallic nickel powder, which comprises adding hydrazine or a hydrazine compound to a nickel-containing solution containing any one of nickel chloride, nickel carbonate, and nickel acetate, mixing the mixture, and heating the mixture to 100°C or below. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP52009938A JPS5835242B2 (en) | 1977-01-31 | 1977-01-31 | Method for producing fine particulate metal nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP52009938A JPS5835242B2 (en) | 1977-01-31 | 1977-01-31 | Method for producing fine particulate metal nickel powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5395165A JPS5395165A (en) | 1978-08-19 |
| JPS5835242B2 true JPS5835242B2 (en) | 1983-08-01 |
Family
ID=11733951
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP52009938A Expired JPS5835242B2 (en) | 1977-01-31 | 1977-01-31 | Method for producing fine particulate metal nickel powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5835242B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56130412A (en) * | 1980-03-17 | 1981-10-13 | Sanyo Electric Co Ltd | Production of metallic nickel for electrode |
| JPS59162206A (en) * | 1983-03-08 | 1984-09-13 | Mitsui Mining & Smelting Co Ltd | Manufacture of fine nickel and cobalt powder |
| CN103706804A (en) * | 2013-12-25 | 2014-04-09 | 南昌航空大学 | Environment-friendly preparing method of nickel nanocrystalline |
-
1977
- 1977-01-31 JP JP52009938A patent/JPS5835242B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5395165A (en) | 1978-08-19 |
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