JPH0211706A - Production of silver fine particle - Google Patents
Production of silver fine particleInfo
- Publication number
- JPH0211706A JPH0211706A JP16031988A JP16031988A JPH0211706A JP H0211706 A JPH0211706 A JP H0211706A JP 16031988 A JP16031988 A JP 16031988A JP 16031988 A JP16031988 A JP 16031988A JP H0211706 A JPH0211706 A JP H0211706A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- particle size
- groups
- silver nitrate
- water solution
- 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
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 18
- 239000004332 silver Substances 0.000 title claims abstract description 18
- 239000010419 fine particle Substances 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 claims abstract description 36
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 150000001491 aromatic compounds Chemical class 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 125000000524 functional group Chemical group 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 10
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000010946 fine silver Substances 0.000 abstract description 5
- 229940079877 pyrogallol Drugs 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 229910001923 silver oxide Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は微細な銀粒子の製造方法に関するものである。[Detailed description of the invention] (Industrial application field) The present invention relates to a method for producing fine silver particles.
（従来技術とその問題点）
従来、銀微粒子の製造方法としては、硝酸銀水溶液に水
酸化ナトリウムを加えて酸化銀を作り、これをホルマリ
ンで還元する方法が用いられてきた。(Prior art and its problems) Conventionally, as a method for producing silver fine particles, a method has been used in which silver oxide is produced by adding sodium hydroxide to an aqueous silver nitrate solution, and this is reduced with formalin.
ところが、この方法では、析出した微粒子同士が引き寄
せ合って凝集した、粒度分布の幅の広い銀粒子しか得ら
れず、粒径のコントロールが難しいという欠点を有して
いた。However, this method has the disadvantage that only silver particles with a wide particle size distribution in which the precipitated fine particles are attracted to each other and aggregate are obtained, and that it is difficult to control the particle size.
（発明の目的）
本発明は上記の欠点を解消せんがためになされたもので
あり、分散した、粒度分布の幅の狭い微細な銀粒子の粒
径コントロール可能な製造方法を提供せんとするもので
ある。(Object of the Invention) The present invention has been made to solve the above-mentioned drawbacks, and it is an object of the present invention to provide a method for producing dispersed fine silver particles with a narrow particle size distribution, in which the particle size can be controlled. It is.
（問題点を解決するための手段）
本発明は硝酸銀水溶液を還元して銀微粒子を製造する方
法において還元剤としてＯＨ基を２個とＯＨ基、Ｈ基以
外の官能基を１個り上官するか又はＯＨ基を３個以上有
する芳香族化合物水溶液を用い、さらに硝酸銀水溶液の
ｐＨを０１〜７、前記芳香族化合物水溶液のｐＨを０１
以上、反応温度を１００℃以下に保つことによって単分
散した銀微粒子を得ることを特徴とするものである。(Means for Solving the Problems) The present invention uses two OH groups and one functional group other than the OH group and the H group as a reducing agent in a method for producing silver fine particles by reducing an aqueous silver nitrate solution. or using an aqueous solution of an aromatic compound having three or more OH groups, and further adjusting the pH of the silver nitrate aqueous solution to 01 to 7 and the pH of the aromatic compound aqueous solution to 01.
As described above, the method is characterized in that monodispersed silver particles are obtained by keeping the reaction temperature at 100° C. or lower.
而して本発明の製造方法において、ＯＨ基を２個とＯＨ
基、Ｈ基以外の官能基を１個以上有するか又はＯＨ基を
３個以上有する芳香族化合物水溶液を用いる理由は、こ
れらの酸化還元電位が硝酸銀水溶液を還元するのに適当
であると同時に粒子同士の凝集を防ぐ働きがあるためで
ある。Therefore, in the production method of the present invention, two OH groups and OH
The reason for using an aqueous solution of an aromatic compound having one or more functional groups other than H groups or H groups or having three or more OH groups is that these redox potentials are suitable for reducing the silver nitrate aqueous solution, and at the same time, the particles This is because it has the function of preventing agglomeration between them.
また、硝酸銀水溶液のｐＨを０．１〜７にする理由は、
ｐＨが０．１よりも低いと反応が遅くなり７よりも高い
と銀の酸化物が生成するためである。In addition, the reason why the pH of the silver nitrate aqueous solution is set to 0.1 to 7 is as follows.
This is because when the pH is lower than 0.1, the reaction is slow, and when it is higher than 7, silver oxide is produced.
また、芳香族化合物水溶液のｐＨを０．１以上にする理
由は、ｐＨが０．１よりも低いと反応が極端に遅くなる
ためである。また、反応温度を１００℃以下に保つ理由
は１００℃を超えると、銀微粒子が凝集してくるととも
に、粒度分布の幅が広くなってしまうた約である。Moreover, the reason why the pH of the aromatic compound aqueous solution is set to 0.1 or more is that if the pH is lower than 0.1, the reaction becomes extremely slow. The reason for keeping the reaction temperature below 100°C is that if it exceeds 100°C, the fine silver particles will aggregate and the width of the particle size distribution will become wider.
また、本発明の請求範囲においてＯＨ基を２個とＯＨ基
、Ｈ基以外の官能基を１個以上有するか又はＯＨ基を３
個以上有する芳香族化合物としては、ピロガロール、三
四ジヒドロキシトルエンである。In addition, within the scope of the claims of the present invention, it may have two OH groups and one or more functional groups other than OH groups or H groups, or it may have three OH groups.
Examples of the aromatic compound having more than 100 esters include pyrogallol and 34-dihydroxytoluene.
ここで本発明の実施例について説明する。Examples of the present invention will now be described.
（実施例）
硝酸銀結晶２５０ｇを水に溶解し１ｐの水溶液とした後
、希硝酸を加えてｐＨ＝１．０に調整する。(Example) After dissolving 250 g of silver nitrate crystals in water to make a 1p aqueous solution, dilute nitric acid was added to adjust the pH to 1.0.
また、ピロガロール１３０ｇを水に溶解し５００証の水
溶液にする。Also, dissolve 130 g of pyrogallol in water to make a 500 proof aqueous solution.
ここでこの２液を７０℃にし硝酸銀水溶液を撹拌しなが
らピロガロール水溶液を添加し２０分間反応させる。Here, the two liquids are heated to 70°C, and while stirring the silver nitrate aqueous solution, the pyrogallol aqueous solution is added, and the mixture is allowed to react for 20 minutes.
得られた銀微粒子は濾過、洗浄して、粒度分布測定及び
電子顕微鏡観察を行った。The obtained silver particles were filtered, washed, and subjected to particle size distribution measurement and electron microscopy observation.
その結果、この銀微粒子は球状で平均粒径が１．０μｍ
１粒度分布は０８〜１２μｍに７０％が入るンヤプなも
のであった。As a result, the silver particles were spherical and had an average particle size of 1.0 μm.
The particle size distribution was 70% in the range of 08 to 12 μm.
（従来例）
硝酸銀１５ｇを３０ｄの水に溶解し、これに４８％水酸
化ナトリウム水溶液を加え酸化銀の粒子を沈殿させ、こ
の粒子をホルマリンで還元して銀粒子を作った。(Conventional Example) 15 g of silver nitrate was dissolved in 30 d of water, and a 48% aqueous sodium hydroxide solution was added thereto to precipitate silver oxide particles, and the particles were reduced with formalin to produce silver particles.
得られた銀微粒子は濾過、洗浄して粒度分布及び電子顕
微鏡観察を行った。The obtained silver particles were filtered and washed, and the particle size distribution and electron microscope observation were performed.
その結果、この銀微粒子は平均粒径６．２μｍで粒度分
布の幅の広い凝集したものであった。As a result, the silver particles were aggregated with an average particle size of 6.2 μm and a wide particle size distribution.
（発明の効果）
上記の説明で明らかなように本発明の製造方法は硝酸銀
水溶液を還元して銀微粒子を製造する方法において、還
元剤としてＯＨ基を２個とＯＨ基、Ｈ基以外の官能基を
１個以上有するか又はＯＨ基を３個以上有する芳香族化
合物溶液を用いてさらに硝酸銀水溶液のｐＨを０．１〜
７、前記芳香族化合物溶液のｐＨを０．１以上、反応温
度を１００℃以下に保つことにより、従来法では得られ
なかった単分散した粒度分布の幅の狭い微細な銀粒子を
粒径をコントロールして製造できるので、従来の製造方
法にとって代わることのできる画期的なものと言える。(Effects of the Invention) As is clear from the above explanation, the production method of the present invention is a method for producing silver fine particles by reducing an aqueous silver nitrate solution. Further, the pH of the silver nitrate aqueous solution is adjusted to 0.1 to 1 using an aromatic compound solution having one or more groups or three or more OH groups.
7. By keeping the pH of the aromatic compound solution at 0.1 or higher and the reaction temperature at 100°C or lower, fine silver particles with a narrow particle size distribution that is monodisperse, which could not be obtained by conventional methods, can be produced with a small particle size. Since it can be manufactured in a controlled manner, it can be said to be an epoch-making product that can replace conventional manufacturing methods.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
おいて、還元剤としてＯＨ基を２個とＯＨ基、Ｈ基以外
の官能基を１個以上有するか又はＯＨ基を３個以上有す
る芳香族化合物水溶液を用い、さらに硝酸銀水溶液のｐ
Ｈを０．１〜７、前記芳香族化合物溶液のｐＨを０．１
以上、反応温度を１００℃以下に保つことによって単分
散した銀微粒子を得ることを特徴とする銀微粒子の製造
方法。1. In the method of producing silver fine particles by reducing an aqueous silver nitrate solution, the reducing agent is an aromatic compound having two OH groups and one or more functional groups other than OH and H groups, or having three or more OH groups. Using a compound aqueous solution, further p of silver nitrate aqueous solution
H from 0.1 to 7, and the pH of the aromatic compound solution to 0.1.
As described above, the method for producing silver particles is characterized in that monodispersed silver particles are obtained by maintaining the reaction temperature at 100° C. or lower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16031988A JPH0211706A (en) | 1988-06-28 | 1988-06-28 | Production of silver fine particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16031988A JPH0211706A (en) | 1988-06-28 | 1988-06-28 | Production of silver fine particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0211706A true JPH0211706A (en) | 1990-01-16 |
Family
ID=15712384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16031988A Pending JPH0211706A (en) | 1988-06-28 | 1988-06-28 | Production of silver fine particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0211706A (en) |
-
1988
- 1988-06-28 JP JP16031988A patent/JPH0211706A/en active Pending
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