JPH01104338A - Manufacture of silver colloid - Google Patents
Manufacture of silver colloidInfo
- Publication number
- JPH01104338A JPH01104338A JP26050487A JP26050487A JPH01104338A JP H01104338 A JPH01104338 A JP H01104338A JP 26050487 A JP26050487 A JP 26050487A JP 26050487 A JP26050487 A JP 26050487A JP H01104338 A JPH01104338 A JP H01104338A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- colloid
- solution
- ascorbic acid
- silver nitrate
- 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 31
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 26
- 239000004332 silver Substances 0.000 title claims abstract description 26
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 27
- 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 22
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 17
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 6
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 4
- 239000012266 salt solution Substances 0.000 claims description 3
- 150000000994 L-ascorbates Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 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
- 150000003839 salts Chemical class 0.000 abstract 2
- 239000001828 Gelatine Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 239000011668 ascorbic acid Substances 0.000 description 5
- 235000010323 ascorbic acid Nutrition 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 108010010803 Gelatin Proteins 0.000 description 3
- 150000000996 L-ascorbic acids Chemical class 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 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
- 238000003756 stirring Methods 0.000 description 2
- 102000009027 Albumins Human genes 0.000 description 1
- 108010088751 Albumins Proteins 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 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
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling 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
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 description 1
- 159000000000 sodium salts Chemical class 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溶液にア
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 aqueous ammonia is added to an aqueous solution of silver nitrate to form an ammonium complex of silver, 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、安定な銀コロイドの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 aims to provide a method for producing a stable silver colloid.
（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０．１〜７に調
整した硝酸銀水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″Ｃ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 aqueous silver nitrate solution, in which ascorbic acid or L-ascorbic acid salt solution or a pH of 0.1 to 7 is used as a reducing agent. A stable silver colloid is obtained by adding a protective colloid to either or both of the aqueous silver nitrate solutions prepared in the following manner, and then mixing the two solutions at 100''C or less.
（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
酸化還元電位が硝酸銀水溶液を還元するのに適当である
ためである。(Function) The reason why L-ascorbic acid and L-ascorbic acid salts are used in the production method of the present invention is that their redox potential is suitable for reducing an aqueous silver nitrate solution.
また硝酸銀水溶液のＰＨを０．１〜７にする理由は、Ｐ
Ｈが０．１より低いと反応が遅くなり、７よりも高い銀
の酸化物が生成するためである。また２溶液の混合を１
００″Ｃ以下にて行う理由は、１００℃を超えると、粒
子同士の凝集が激しくなるためである。また、反応溶液
中に保護コロイドを添加する理由は、硝酸銀溶液を還元
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。The reason for setting the pH of the silver nitrate aqueous solution to 0.1 to 7 is that P
This is because if H is lower than 0.1, the reaction will be slow and a silver oxide higher than 7 will be produced. Also, when mixing two solutions,
The reason why the temperature is 00"C or lower is that if the temperature exceeds 100"C, the particles will agglomerate to each other. Also, the reason why a protective colloid is added to the reaction solution is that by reducing the silver nitrate solution, This is to prevent silver particles precipitated from increasing in size and to maintain a stable colloidal dispersion so that the particles do not aggregate with each other and cause silver precipitation.
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１００ｍｊ２
にし、この溶液に保護コロイドゼラチン水溶液を３００
ｍ１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″Ｃ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戚にした後、
ＰＨを２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２２０人で非
常に安定に分散した銀コロイドであった。(Example 1) Dissolve 12 g of L-ascorbic acid in water to 100 mj2
and add 300% of a protective colloid gelatin aqueous solution to this solution.
Add 16 g of silver nitrate in water and stir in a Teflon-coated beaker while keeping the solution temperature at 20"C. In another beaker, dissolve 16 g of silver nitrate in water to make 500% solution.
Adjust the pH to 2 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 silver colloid was very stably dispersed with an average particle size of 220 mm.
（実施例２）
し−アスコルビン酸９ｇを水に溶解して１００ｄにし、
この溶液に保護コロイドアラビアゴム水溶液を３００ｍ
１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℃に保ち撹拌しておく。(Example 2) 9 g of ascorbic acid was dissolved in water to make 100 d,
Add 300ml of protective colloid gum arabic aqueous solution to this solution.
1 and stir in a Teflon-coated beaker while keeping the dissolution temperature at 30°C.
また別のビーカーで硝酸銀Ｌｏｇを水に溶解し、５００
滅にした後、ＰＨを４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。In another beaker, dissolve silver nitrate Log in water and add 500
After cooling, adjust the pH to 4 and bring the solution temperature to 30°C. This was added all at once to the above ascorbic acid + gum arabic solution and stirred for 7 minutes.
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。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１００−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-g water, add 28% aqueous ammonia 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硝酸銀
水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０．１〜７に調整した硝酸銀水溶
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
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 uses ascorbic acid or L-ascorbate salt solution or PH as a reducing agent in the method of producing silver colloid by reducing an aqueous silver nitrate solution. By adding a protective colloid to one or both of silver nitrate aqueous solutions adjusted to 0.1 to 7, and then mixing the two solutions above at 100°C or less, stable and fine silver colloids that could not be obtained by conventional methods can be obtained. It can be said that it is an epoch-making method 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)
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０．１〜７に調整した硝
酸銀水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銀コ
ロイドの製造方法。In a method for producing silver colloid by reducing an aqueous silver nitrate solution, a protective colloid is added to either or both of an L-ascorbic acid or L-ascorbate salt solution as a reducing agent or an aqueous silver nitrate solution whose pH is adjusted to 0.1 to 7. A method for producing a silver colloid, which comprises adding a stable silver colloid to the solution, and then mixing the two solutions at a temperature of 100° C. or lower to obtain a stable silver colloid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26050487A JPH01104338A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26050487A JPH01104338A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01104338A true JPH01104338A (en) | 1989-04-21 |
Family
ID=17348882
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26050487A Pending JPH01104338A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01104338A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100425976B1 (en) * | 2001-04-30 | 2004-04-06 | 주식회사 화진 | Preparation Method of the Silver Colloids with Nanometer Size Irradiated by Radiation and Its Silver Colloid with Nanometer Size |
| WO2005075133A1 (en) * | 2004-02-10 | 2005-08-18 | Mitsui Mining & Smelting Co., Ltd. | Highly crystalline silver powder and method for production thereof |
| JP2007016258A (en) * | 2005-07-05 | 2007-01-25 | Mitsui Mining & Smelting Co Ltd | High crystal silver powder, and method for producing the high crystal silver powder |
| CN101460271A (en) * | 2006-06-02 | 2009-06-17 | E.I.内穆尔杜邦公司 | Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom |
| JP2010209366A (en) * | 2009-03-06 | 2010-09-24 | Dic Corp | Method for producing metal nanoparticle |
| CN102198514A (en) * | 2011-05-12 | 2011-09-28 | 中南大学 | Method for preparing ultrafine grain wolfram carbide/cobalt composite powder |
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
| CN113600825A (en) * | 2021-07-22 | 2021-11-05 | 厦门大学 | Micron-sized spherical silver powder and preparation method thereof |
-
1987
- 1987-10-15 JP JP26050487A patent/JPH01104338A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100425976B1 (en) * | 2001-04-30 | 2004-04-06 | 주식회사 화진 | Preparation Method of the Silver Colloids with Nanometer Size Irradiated by Radiation and Its Silver Colloid with Nanometer Size |
| WO2005075133A1 (en) * | 2004-02-10 | 2005-08-18 | Mitsui Mining & Smelting Co., Ltd. | Highly crystalline silver powder and method for production thereof |
| JP2005226094A (en) * | 2004-02-10 | 2005-08-25 | Mitsui Mining & Smelting Co Ltd | High crystallinity silver powder and its production method |
| JP2007016258A (en) * | 2005-07-05 | 2007-01-25 | Mitsui Mining & Smelting Co Ltd | High crystal silver powder, and method for producing the high crystal silver powder |
| CN101460271A (en) * | 2006-06-02 | 2009-06-17 | E.I.内穆尔杜邦公司 | Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom |
| JP2009540111A (en) * | 2006-06-02 | 2009-11-19 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Method for producing highly dispersible spherical silver powder particles and silver particles formed therefrom |
| JP2010209366A (en) * | 2009-03-06 | 2010-09-24 | Dic Corp | Method for producing metal nanoparticle |
| CN102198514A (en) * | 2011-05-12 | 2011-09-28 | 中南大学 | Method for preparing ultrafine grain wolfram carbide/cobalt composite powder |
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
| CN103567431B (en) * | 2012-07-24 | 2015-08-26 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of nano-class silver colloidal solution and preparation method thereof |
| CN113600825A (en) * | 2021-07-22 | 2021-11-05 | 厦门大学 | Micron-sized spherical silver powder and preparation method thereof |
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