JPH01104337A - Manufacture of silver colloid - Google Patents
Manufacture of silver colloidInfo
- Publication number
- JPH01104337A JPH01104337A JP26050387A JP26050387A JPH01104337A JP H01104337 A JPH01104337 A JP H01104337A JP 26050387 A JP26050387 A JP 26050387A JP 26050387 A JP26050387 A JP 26050387A JP H01104337 A JPH01104337 A JP H01104337A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- solution
- colloid
- added
- ascorbic acid
- 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
- 239000000084 colloidal system Substances 0.000 title claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 29
- 239000004332 silver Substances 0.000 title claims abstract description 29
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000000243 solution Substances 0.000 claims abstract description 33
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 20
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 7
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 7
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 4
- 150000000994 L-ascorbates Chemical class 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 229910001961 silver nitrate Inorganic materials 0.000 abstract description 5
- 229920000084 Gum arabic Polymers 0.000 abstract description 4
- 241000978776 Senegalia senegal Species 0.000 abstract description 4
- 235000010489 acacia gum Nutrition 0.000 abstract description 4
- 239000000205 acacia gum Substances 0.000 abstract description 4
- 229920000159 gelatin Polymers 0.000 abstract description 4
- 235000019322 gelatine Nutrition 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 102000009027 Albumins Human genes 0.000 abstract description 2
- 108010088751 Albumins Proteins 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract 3
- 239000001828 Gelatine Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 108010010803 Gelatin Proteins 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000008273 gelatin Substances 0.000 description 3
- 235000011852 gelatine desserts Nutrition 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 238000001246 colloidal dispersion Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 150000000996 L-ascorbic acids Chemical class 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229940072107 ascorbate Drugs 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 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）
本発明は安定な銀コロイド溶液の製造方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for producing a stable silver colloid solution.
（従来の技術とその問題点）
従来、銀コロイドの製造方法としては硝酸銀水ｍＷにア
ンモニア水を加えて銀のアンモニウム錯体を作り、これ
をホルマリンで還元する方法が用いられてきた。ところ
が、この方法では析出した銀粒子が比較的大きいために
コロイド分散が不安定であり、凝集による銀の沈殿を生
じやすいという欠点を有していた。(Prior Art and its Problems) Conventionally, as a method for producing silver colloid, a method has been used in which ammonia water is added to silver nitrate water (mW) to form a silver ammonium complex, and this is reduced with formalin. However, this method has the drawback that colloidal dispersion is unstable because the precipitated silver particles are relatively large, and silver precipitation due to aggregation is likely to occur.
（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、安定な恨コロイドの製造方法を提供せんとするも
のである。(Objective of the Invention) The present invention has been made to solve the above-mentioned drawbacks, and aims to provide a method for producing a stable colloid.
（問題点を解決するための手段）
本発明は銀のアンモニウム錯体溶液を還元して銀コロイ
ドを製造する方法において、還元剤としてのし一アスコ
ルビン酸又はＬ−アスコルビン酸塩類溶液又はＰＨを８
〜１３に調整した銀のアンモニウム錯体溶液のいずれか
又は両方に保護コロイドを添加し、次いで上記２つの溶
液を１００℃以下にて混合することにより安定な銀コロ
イドを得ることを特徴とするものである。(Means for Solving the Problems) The present invention provides a method for producing silver colloid by reducing an ammonium complex solution of silver, in which ascorbic acid or L-ascorbate salt solution or pH 8
A stable silver colloid is obtained by adding a protective colloid to either or both of the silver ammonium complex solutions adjusted to a temperature of 13 to 13, and then mixing the two solutions at 100°C or less. be.
（作用）
而して本発明の製造方法において、Ｌ−アスコルビン酸
及びＬ−アスコルビン酸塩類を用いる理由は、これらの
酸化還元電位が銀のアンモニウム錯体溶液を還元するの
に適当であるためであるやまた銀のアンモニウム錯体溶
液のＰＨを８〜１３にする理由は、ＰＨが８より低いと
銀の酸化物が生成し、１３より高いとアンモニアガスの
発生が多くなり反応が遅くなるためである。また２溶液
の混合を１００℃以下にて行なう理由は、１００℃を超
えると、粒子同士の凝集が激しくなるためである。(Function) The reason why L-ascorbic acid and L-ascorbate salts are used in the production method of the present invention is that their redox potential is suitable for reducing the ammonium complex solution of silver. The reason why the pH of the silver ammonium complex solution is set to 8 to 13 is that if the pH is lower than 8, silver oxide will be produced, and if it is higher than 13, ammonia gas will be generated more and the reaction will be slower. . Further, the reason why the two solutions are mixed at 100°C or lower is that if the temperature exceeds 100°C, the particles will agglomerate more intensely.
また、反応溶液中に保護コロイドを添加する理由は、恨
のアンモニウム錯体溶液を還元することによって水溶液
中に析出する銀粒子が大きくなることを防ぎ、また粒子
同士が凝集して銀の沈殿を生じないようコロイド分散を
安定に保つようにするためである。In addition, the reason for adding a protective colloid to the reaction solution is to prevent the silver particles precipitated in the aqueous solution from increasing in size by reducing the ammonium complex solution, and also to prevent the particles from coagulating with each other and causing silver precipitation. This is to keep the colloidal dispersion stable so that it does not occur.
本発明の請求範囲においてＬ−アスコルビン酸塩類とし
ては、ナトリウム塩、カリウム塩、アンモニウム塩等は
問わない。また、反応溶液中に添加する保護コロイドと
してはゼラチン、アラビアゴム、アルブミン、プロタル
ピン酸、リサルピン酸等を問わない。In the scope of the present invention, L-ascorbic acid salts include sodium salts, potassium salts, ammonium salts, and the like. Further, the protective colloid to be added to the reaction solution may be gelatin, gum arabic, albumin, protalpic acid, resalpic acid, or the like.
（実施例１）
Ｌ−アスコルビン酸１２ｇを水に溶解して１００＋＋ｊ
！にし、この溶液に保護コロイドゼラチン水溶液を３０
０ｄ添加してテフロンコーティングしたビーカーの中で
溶液温度を２０℃に保ち撹拌しておく。また別のビーカ
ーで硝酸銀１６ｇを水に溶解し、５００成にした後、２
８％のアンモニア水を加えて銀のアンモニウム錯体溶液
としそのＰＨを１１に調整し、溶液温度を２０℃にする
。これを先のし一アスコルビン酸＋ゼラチン溶液中に一
度に添加して７分間撹拌した。得られた銀コロイドは透
過型電子顕微鏡で観察を行った。その結果、平均粒径２
２０人で非常に安定に分散した銀コロイドであった。(Example 1) Dissolve 12g of L-ascorbic acid in water to give 100++j
! and add 30% of a protective colloid gelatin aqueous solution to this solution.
Add 0d and stir the solution while keeping the temperature at 20°C in a Teflon-coated beaker. In another beaker, dissolve 16g of silver nitrate in water and make 500% solution, then 2
Add 8% ammonia water to prepare a silver ammonium complex solution, adjust its pH to 11, and bring the solution temperature to 20°C. This was added all at once to the above ascorbic acid + gelatin solution and stirred for 7 minutes. The obtained silver colloid was observed using a transmission electron microscope. As a result, the average particle size 2
The silver colloid was dispersed very stably in 20 samples.
（実施例２）
Ｌ−アスコルビン酸９ｇを水に溶解して１００ｍ１にし
、この溶液に保護コロイドアラビアゴム水溶液を３００
ｒｄ添加してテフロンコーティングしたビーカーの中で
溶解温度を３０℃に保ち撹拌してお（。(Example 2) 9 g of L-ascorbic acid was dissolved in water to make 100 ml, and 300 ml of protective colloid gum arabic aqueous solution was added to this solution.
rd was added and stirred in a Teflon-coated beaker, keeping the dissolution temperature at 30°C (.
また別のビーカーで硝酸銀１０ｇを水に溶解し、５００
ｍ１にした後、２８％のアンモニア水を加えて銀のアン
モニウム錯体溶液としそのＰ Ｈを１０に調整し、溶液
温度を３０℃にする。これを先のし一アスコルビン酸＋
アラビアゴム溶液中に一度に添加して７分゛間撹拌した
。得られた銀コロイドは透過型電子顕微鏡で観察を行っ
た。その結果、平均粒径２００人で非常に安定に分散し
た銀コロイドであった。In another beaker, dissolve 10g of silver nitrate in water,
ml, add 28% ammonia water to make a silver ammonium complex solution, adjust its pH to 10, and bring the solution temperature to 30°C. Ascorbic acid +
It was added all at once to the gum arabic solution and stirred for 7 minutes. The obtained silver colloid was observed using a transmission electron microscope. As a result, the silver colloid was very stably dispersed with an average particle size of 200 particles.
（従来例）
硝酸銀１５ｇを１００ｄの水に溶解し、これに２８％の
アンモニア水を加え、銀のアンモニウム錯体溶液とし、
この溶液をホルマリンで還元して銀コロイドを作った。(Conventional example) Dissolve 15 g of silver nitrate in 100 d of water, add 28% ammonia water to this to make a silver ammonium complex solution,
This solution was reduced with formalin to produce silver colloid.
得られた銀コロイドは透過型電子顕微鏡観察を行った。The obtained silver colloid was observed using a transmission electron microscope.
その結果この銀コロイドは平均粒径は４００人でありし
かも一昼夜放置した後凝集により銀の沈殿を生じた。As a result, this silver colloid had an average particle size of 400 particles, and silver precipitated due to coagulation after being left for a day and night.
（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銀のア
ンモニウム錯体溶液を還元して銀コロイドを製造する方
法において、還元剤としてのＬ−アスコルビン酸又はＬ
−アスコルビン酸塩［溶液又はＰＨを８〜１３に調整し
た銀のアンモニウム錯体溶液のいずれかまたは両方に保
護コロイドを添加し次いで上記の２つの溶液を１００℃
以下にて混合することにより従来法では得られなかった
安定で微細な銀コロイドを製造できるので、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いえる
。(Effects of the Invention) As is clear from the above explanation, the production method of the present invention is a method for producing silver colloid by reducing an ammonium complex solution of silver.
-Ascorbate [protective colloid is added to either or both of the solution or ammonium complex solution of silver whose pH is adjusted to 8 to 13, and then the above two solutions are heated to 100 °C
By mixing the following steps, stable and fine silver colloid, which could not be obtained by conventional methods, can be produced, so it can be said to be an epoch-making method that can replace conventional production methods.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
する方法において、還元剤としてのＬ−アスコルビン酸
又はＬ−アスコルビン酸塩類溶液又はＰＨを８〜１３に
調整した銀のアンモニウム錯体溶液のいずれか又は両方
に保護コロイドを添加し、次いで上記２つの溶液を１０
０℃以下にて混合することにより安定な銀コロイドを得
ることを特徴とする銀コロイドの製造方法。In the method of producing silver colloid by reducing a silver ammonium complex solution, either L-ascorbic acid or L-ascorbate salt solution as a reducing agent or a silver ammonium complex solution whose pH is adjusted to 8 to 13, or Add protective colloid to both and then mix the above two solutions for 10
A method for producing silver colloid, which comprises obtaining a stable silver colloid by mixing at 0°C or lower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26050387A JPH01104337A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26050387A JPH01104337A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01104337A true JPH01104337A (en) | 1989-04-21 |
Family
ID=17348869
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26050387A Pending JPH01104337A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01104337A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006118010A (en) * | 2004-10-22 | 2006-05-11 | Toda Kogyo Corp | Ag NANOPARTICLE, METHOD FOR PRODUCING THE SAME AND DISPERSED SOLUTION OF Ag NANOPARTICLE |
| JP2010209366A (en) * | 2009-03-06 | 2010-09-24 | Dic Corp | Method for producing metal nanoparticle |
| KR101353995B1 (en) * | 2012-06-20 | 2014-01-22 | (주)이건이엔씨 | Method for preparing silver cluster of micro-size consisting of agglomerate nano-silver particle |
| JP2015048531A (en) * | 2013-08-29 | 2015-03-16 | サムソン エレクトロ−メカニックス カンパニーリミテッド． | Metal powder production method and multilayer ceramic electronic component |
-
1987
- 1987-10-15 JP JP26050387A patent/JPH01104337A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006118010A (en) * | 2004-10-22 | 2006-05-11 | Toda Kogyo Corp | Ag NANOPARTICLE, METHOD FOR PRODUCING THE SAME AND DISPERSED SOLUTION OF Ag NANOPARTICLE |
| JP2010209366A (en) * | 2009-03-06 | 2010-09-24 | Dic Corp | Method for producing metal nanoparticle |
| KR101353995B1 (en) * | 2012-06-20 | 2014-01-22 | (주)이건이엔씨 | Method for preparing silver cluster of micro-size consisting of agglomerate nano-silver particle |
| JP2015048531A (en) * | 2013-08-29 | 2015-03-16 | サムソン エレクトロ−メカニックス カンパニーリミテッド． | Metal powder production method and multilayer ceramic electronic component |
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