JPH01104339A - Manufacture of silver colloid - Google Patents
Manufacture of silver colloidInfo
- Publication number
- JPH01104339A JPH01104339A JP26050587A JP26050587A JPH01104339A JP H01104339 A JPH01104339 A JP H01104339A JP 26050587 A JP26050587 A JP 26050587A JP 26050587 A JP26050587 A JP 26050587A JP H01104339 A JPH01104339 A JP H01104339A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- colloid
- solutions
- solution
- added
- 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
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 30
- 239000004332 silver Substances 0.000 title claims abstract description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000000084 colloidal system Substances 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000000243 solution Substances 0.000 claims abstract description 32
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 4
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims description 9
- NGBNXJUWQPLNGM-UHFFFAOYSA-N silver;azane Chemical compound N.[Ag+] NGBNXJUWQPLNGM-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 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
- 229910001961 silver nitrate Inorganic materials 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 150000007513 acids Chemical class 0.000 abstract 2
- 239000001828 Gelatine Substances 0.000 abstract 1
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 108010010803 Gelatin Proteins 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
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 102000009027 Albumins Human genes 0.000 description 1
- 108010088751 Albumins Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration 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
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940026231 erythorbate Drugs 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 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
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できた。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吟、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 was used in which aqueous ammonia was added to an aqueous solution of silver nitrate to form a silver ammonium complex, and the complex was reduced with formalin. However, this method has the disadvantage that colloidal dispersion is unstable because the precipitated silver particles are relatively large, and silver tends to precipitate due to agglomeration.
（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Ｄ−エリソ
ルビン酸又はＤ−エリソ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°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 ammonium complex solution of silver, in which D-erythorbic acid or a solution of D-erythorbates as a reducing agent or a pH of 8
A method characterized by adding a protective colloid to either or both of the ammonium complex solutions of silver adjusted to a temperature of ~13 and then mixing the two solutions above at 100°C or less to obtain a stable silver colloid. It is.
（作用）
而して本発明の製造方法において、Ｄ−エリソルビン酸
及びＤ−エリソ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。(Function) The reason why D-erythorbic acid and D-erythorbic acid salts are used in the production method of the present invention is that their redox potential is suitable for reducing a silver ammonium complex solution. .
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、工３
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液の混合を１００°Ｃ以下にて
行う理由は、１００″Ｃ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、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。Also, the reason why the pH of the ammonium complex solution of silver is set to 8 to 13 is that when the pH is lower than 8, silver oxide is generated, and the
This is because if the temperature is higher, more ammonia gas will be generated and the reaction will be slower. The reason why the two liquids are mixed at 100°C or lower is that if the temperature exceeds 100''C, the particles will agglomerate together.Also, the reason why a protective colloid is added to the reaction solution is that This is to prevent the silver particles precipitated in the aqueous solution from increasing in size by reducing the ammonium complex solution, 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Ｄ−エリソルビン酸塩類とし
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, D-erythorbate 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）
Ｄ−エリソルビン酸１２ｇを水に溶解して１００ ｄに
し、この溶液に保護コロイドゼラチン水溶液を３００滅
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滅にした後、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ＰＨを１１に調整し、溶液温度を２０゛Ｃにする。(Example 1) 12 g of D-erythorbic acid was dissolved in water to make 100 d, and 300 g of a protective colloid gelatin aqueous solution was added to this solution, and the solution temperature was kept at 20° C. and stirred in a Teflon-coated beaker. put. In another beaker, dissolve 16g of silver nitrate in water and reduce to 500%, then 28%
Add ammonia water to make a silver ammonium complex solution, adjust the pH to 11, and bring the solution temperature to 20°C.
これを先のＤ−エリソルビン酸十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２２
０人で非常に安定に分散した銀コロイドであった。This was added all at once to the D-erythorbic acid deca 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 was 22
It was a very stably dispersed silver colloid.
（実施例２）
Ｄ−エリソルビン酸９ｇを水に溶解して１００滅にし、
この溶液に保護コロイドアラビアゴム水溶液を３００成
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 D-erythorbic acid was dissolved in water to 100%
To this solution, 300 g of an aqueous solution of protective colloid gum arabic is added and stirred in a Teflon-coated beaker while maintaining the dissolution temperature at 30°C.
また別のビーカーで硝酸１１Ｊ１０ｇを水に溶解し、５
００戚にした後、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ＰＨを１０に調整し、溶液
温度を３０°Ｃにする。これを先のＤ−エリソルビン酸
＋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 11J10g of nitric acid in water and
After adjusting the solution to 0.00%, 28% aqueous ammonia is added to form a silver ammonium complex solution, the pH of which is adjusted to 10, and the solution temperature is set to 30°C. This was added at once to the above D-erythorbic acid + 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１００７ｄ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
。得られた銀コロイドは透過型電子顕微鏡観察を行った
。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。(Conventional Example) Dissolve 15g of silver nitrate in 1007d of water and add 28%
of ammonia water was added to obtain a silver ammonium complex solution, and this solution was reduced with formalin to produce silver colloid. The obtained silver colloid was observed using a transmission electron microscope. 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恨コロイドを製造する方
法において、還元剤としてのＤ−エリソルビン酸又はＤ
−エリソルビン酸塩類ｍＨ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°Ｃ
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 description, the production method of the present invention is a method for producing a colloid by reducing an ammonium complex solution of silver, in which D-erythorbic acid or D
- Add a protective colloid to either or both of the silver ammonium complex solutions whose mH or pH has been adjusted to 8 to 13, and then heat the two solutions at 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Ｄ−エリソルビン酸
又はＤ−ユリソ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 D-erythorbic acid or D-urithorbic acid 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 |
|---|---|---|---|
| JP26050587A JPH01104339A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26050587A JPH01104339A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01104339A true JPH01104339A (en) | 1989-04-21 |
Family
ID=17348892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26050587A Pending JPH01104339A (en) | 1987-10-15 | 1987-10-15 | Manufacture of silver colloid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01104339A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010209366A (en) * | 2009-03-06 | 2010-09-24 | Dic Corp | Method for producing metal nanoparticle |
-
1987
- 1987-10-15 JP JP26050587A patent/JPH01104339A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010209366A (en) * | 2009-03-06 | 2010-09-24 | Dic Corp | Method for producing metal nanoparticle |
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