JPH0248036A - Preparation of noble metal organosol - Google Patents
Preparation of noble metal organosolInfo
- Publication number
- JPH0248036A JPH0248036A JP19846788A JP19846788A JPH0248036A JP H0248036 A JPH0248036 A JP H0248036A JP 19846788 A JP19846788 A JP 19846788A JP 19846788 A JP19846788 A JP 19846788A JP H0248036 A JPH0248036 A JP H0248036A
- Authority
- JP
- Japan
- Prior art keywords
- noble metal
- organosol
- solution
- fine particles
- org
- 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
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 48
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 239000010419 fine particle Substances 0.000 claims description 29
- 239000003960 organic solvent Substances 0.000 claims description 29
- 150000002736 metal compounds Chemical class 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 abstract description 17
- 238000003756 stirring Methods 0.000 abstract description 13
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 12
- 239000008096 xylene Substances 0.000 abstract description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract 4
- 239000002923 metal particle Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 239000010970 precious metal Substances 0.000 description 8
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 6
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 6
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 description 6
- 229910052763 palladium Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 229910052741 iridium Inorganic materials 0.000 description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229940117955 isoamyl acetate Drugs 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002894 organic compounds Chemical group 0.000 description 2
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 125000005595 acetylacetonate group Chemical group 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- RFYYQFJZJJCJNT-UHFFFAOYSA-N pentane-2,4-dione;ruthenium Chemical compound [Ru].CC(=O)CC(C)=O RFYYQFJZJJCJNT-UHFFFAOYSA-N 0.000 description 1
- SVOOVMQUISJERI-UHFFFAOYSA-K rhodium(3+);triacetate Chemical compound [Rh+3].CC([O-])=O.CC([O-])=O.CC([O-])=O SVOOVMQUISJERI-UHFFFAOYSA-K 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Colloid Chemistry (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、触媒、各種ペースト、プリントの材料、その
他電気材料分野に利用される貴金属微粒子を有機溶媒中
に安定させた状態で分散させる貴金属微粒子の調整方法
に関する。Detailed Description of the Invention (Industrial Field of Application) The present invention is a method for stably dispersing precious metal fine particles in an organic solvent for use in catalysts, various pastes, printing materials, and other electrical material fields. This article relates to a method for adjusting fine particles.
（従来技術とその問題点）
有機溶媒中に貴金属微粒子を分散させたものの利用とし
て、貴金属を含有するペースト、インキの原料や、触媒
、機能膜等に貴金属を担持、あるいは被膜を形成する等
、その利用範囲は多く、しかも高価な貴金属を有効に活
用するため、粒子径が用途に合った大きさで、貴金属濃
度に左右されにくい粒子径の安定したもの、および溶液
中で均分散し安定していることが望まれている。(Prior art and its problems) Precious metal fine particles dispersed in organic solvents can be used to support noble metals on pastes and ink materials, catalysts, functional films, etc., or to form coatings. They have a wide range of uses, and in order to make effective use of expensive precious metals, we need particles that have a particle size that is suitable for the application, have a stable particle size that is not affected by the precious metal concentration, and that are uniformly dispersed and stable in solutions. It is hoped that the
また、有機溶媒中に分散させた貴金属微粒子以外の共存
成分が分解或いは除去処理において他に影響を与えにく
いものであること等も望まれている。It is also desired that the coexisting components other than the noble metal fine particles dispersed in the organic solvent do not easily affect other components during decomposition or removal treatment.
しかし、従来法は貴金属塩化物が多く用いられ、該塩化
物を水に溶解し界面活性剤や水溶性高分子の存在下で貴
金属を還元し、次いで有機溶媒中に分散させる方法が用
いられている。However, conventional methods often use noble metal chlorides, and the method involves dissolving the chloride in water, reducing the noble metal in the presence of a surfactant or water-soluble polymer, and then dispersing it in an organic solvent. There is.
上記、従来法の欠点は界面活性剤や水溶性高分子を用い
ているため有機溶媒中で貴金属微粒子はエマルジョン状
態で分散しており、安定性に欠ける点と貴金属濃度を高
めて還元すると微粒子の粒子径がバラツキを生じやすく
なり、貴金属微粒子を数多く分散させるとエマルジョン
が不安定になりやすいという欠点があった。The disadvantages of the conventional method mentioned above are that because surfactants and water-soluble polymers are used, the noble metal fine particles are dispersed in an emulsion state in the organic solvent, which lacks stability, and that when the noble metal concentration is increased and reduced, the fine particles are This has disadvantages in that the particle diameter tends to vary and the emulsion tends to become unstable when a large number of noble metal fine particles are dispersed.
また、界面活性剤等の共存が用途により問題であった。Furthermore, the coexistence of surfactants and the like has been a problem depending on the application.
（発明の目的）
本発明は、上記従来法の欠点を解決するためになされた
もので、有機溶媒中に分散した貴金属微粒子の粒子径の
バラツキが貴金属濃度を変化させた場合でもその影響を
受けにくく、有機溶媒中に貴金属微粒子が均一に分散し
ているものの調製方法を提供するものである。(Purpose of the Invention) The present invention has been made to solve the drawbacks of the above-mentioned conventional methods, and even if the variation in the particle diameter of precious metal fine particles dispersed in an organic solvent changes the precious metal concentration, it will not be affected. The present invention provides a method for preparing noble metal fine particles uniformly dispersed in an organic solvent.
（問題点を解決するための手段）
本発明は、有機貴金属化合物を有機溶媒に溶解した溶液
に還元剤を加えて有機溶媒中に貴金属微粒子を分散させ
ることを特徴とする貴金属オルガノゾルの調整方法であ
る。(Means for Solving the Problems) The present invention is a method for preparing a noble metal organosol, which is characterized by adding a reducing agent to a solution of an organic noble metal compound dissolved in an organic solvent to disperse noble metal fine particles in the organic solvent. be.
以下、本発明の詳細について説明する。The details of the present invention will be explained below.
本発明に用いる有機貴金属化合物としては、トリスまた
はビス（アセチルアセトナト）貴金属化合物、貴金属酢
酸塩、アセチルアセトン貴金属化合物、貴金属レジネー
ト等で、有機溶媒としては、キシレン、ブロモベンゼン
、メチルイソブチルケトン（ＭＩＢＫ）、酢酸イソアミ
ル、クロロホルム等で上記貴金属有機化合物を溶解する
ものを主に用いて均一な溶液とすることができ、他にジ
オキサン、トリエチルアミン、アセトン、エーテノペア
ルコール、ジブチルカルピトール（ＤＢＣ）等を加えて
もよく、その加える量は有機溶媒により変化させるが、
おおむね１０％以下で、還元剤を有機溶媒中に分散させ
反応を速やかに行わせると共に、ゾルの安定性を高める
ためである。Examples of the organic noble metal compound used in the present invention include tris or bis(acetylacetonato) noble metal compound, noble metal acetate, acetylacetone noble metal compound, and noble metal resinate, and examples of the organic solvent include xylene, bromobenzene, and methyl isobutyl ketone (MIBK). , isoamyl acetate, chloroform, etc., which dissolve the above-mentioned noble metal organic compounds, can be used to make a homogeneous solution.In addition, dioxane, triethylamine, acetone, ethenope alcohol, dibutylcarpitol (DBC), etc. can be used. It may be added, and the amount added varies depending on the organic solvent, but
This is in order to disperse the reducing agent in the organic solvent to speed up the reaction and to improve the stability of the sol.
該有機貴金属化合物を有機溶媒に溶解した溶液に還元剤
を加えて貴金属を還元する方法は、有機貴金属化合物を
０．５〜４．０ミＩＪモル／ｌになるように有機溶媒に
溶解しておき、別に還元剤を貴金属に対して還元当量の
１，２〜２． ０倍量になるように有機溶媒に溶解調製
して還元剤を十分に分散させた溶液を、上記有機貴金属
化合物を溶解した溶液を十分攪拌しながら、還元剤を分
散させた溶液を加えて還元すると貴金属オルガノゾルが
得られる。The method of reducing the noble metal by adding a reducing agent to a solution of the organic noble metal compound dissolved in an organic solvent involves dissolving the organic noble metal compound in an organic solvent to a concentration of 0.5 to 4.0 mmol/l. Separately, add a reducing agent to the noble metal at a reducing equivalent of 1.2 to 2. A solution in which the reducing agent is sufficiently dispersed by dissolving it in an organic solvent so that the volume is 0 times the volume is reduced by adding the solution in which the reducing agent is dispersed while thoroughly stirring the solution in which the above-mentioned organic noble metal compound is dissolved. Then, a noble metal organosol is obtained.
有機貴金属化合物を溶解する有機溶媒と、貴金属を還元
するための還元剤を溶解する有機溶媒とは、はぼ同一の
ものとすることが望ましい。It is desirable that the organic solvent in which the organic noble metal compound is dissolved and the organic solvent in which the reducing agent for reducing the noble metal is dissolved are almost the same.
その理由は密度や粘度に差があると、反応速度や溶液の
均一混合が不十分となり、微粒子の凝集や分散に影響す
るからである。The reason for this is that if there is a difference in density or viscosity, the reaction rate and uniform mixing of the solution will be insufficient, which will affect the aggregation and dispersion of fine particles.
得られる貴金属微粒子は粒子径５０〜２００人のもので
ある。The noble metal fine particles obtained have a particle size of 50 to 200 particles.
また、還元剤はヒドラジン、ベンズアルデヒド、ホルム
アルデヒド等で他の還元剤でも有機溶媒に溶解するもの
であれば用いられる。Further, the reducing agent may be hydrazine, benzaldehyde, formaldehyde, etc., and other reducing agents may be used as long as they are soluble in the organic solvent.
例えば、ギ酸、Ｌ−アスコルビン酸、ヒドロキノン等で
ある。For example, formic acid, L-ascorbic acid, hydroquinone, etc.
該貴金属オルガノゾルとして安定しているのは有機貴金
属化合物から貴金属を還元して貴金属微粒子を生成する
が、貴金属と結合していた有機化合物が分子として大き
いものや、有機溶媒と反応してより高分子なものとなり
貴金属微粒子の分散状態を安定にする作用をしていると
みられる。Stable noble metal organosols are produced by reducing the noble metal from an organic noble metal compound to produce noble metal fine particles, but those in which the organic compound bonded to the noble metal is large in molecular size, or in which it reacts with an organic solvent to form a higher molecule This seems to work to stabilize the dispersion state of precious metal fine particles.
以下、本発明の実施例を記載するが該実施例は本発明を
限定するものではない。Examples of the present invention will be described below, but the examples are not intended to limit the present invention.
（実施例１）
Ｐｄ （ａｃａｃ）２を有機溶媒として、夕日口ホル
ムを用いて１．０ミ’Ｊモル／ｌの溶液とし、その５０
ｍＡを攪拌しながら、別にクロロホルムにイソプロピル
アルコール２％を加えた溶液にヒドラジンをパラジウム
の還元当量の１．３倍量を加えて分散させた溶液５０ｍ
ｊｌ！を加えて、室温で反応させ１時間攪拌を続けたと
ころパラジウムの微粒子が生成して均一分散したオルガ
ノゾルを得た。(Example 1) Using Pd (acac)2 as an organic solvent, a solution of 1.0 mmol/l was made using Yuhiguchi form, and 50
While stirring mA, add 1.3 times the reduction equivalent of palladium to a solution of hydrazine and disperse it to a solution of 2% isopropyl alcohol in chloroform.
jl! was added, and the mixture was allowed to react at room temperature and stirring was continued for 1 hour. Palladium fine particles were produced to obtain a homogeneously dispersed organosol.
該パラジウムの微粒子の平均粒子径を測定したところ９
７八であった。When the average particle diameter of the palladium fine particles was measured, it was 9.
It was 78.
また、オルガノゾルの安定性を観察したところ２日間後
でもまったく変化なかった。Furthermore, when the stability of the organosol was observed, there was no change at all even after 2 days.
（実施例２）
Ｐｄ （ａｃａｃ）２を有機溶媒として、ＭＩＢＫとＯ
−キシレンを各１容づつ加えて混合した溶液を用いて、
０．８ミ！Ｊモル／ｌ溶液とし、その５０ｍｊ！を攪拌
しながら、別にＭＩＢＫと。−キシレンを各１容づつ加
えて混合した溶液にジオキサン１％を加えた溶液にベン
ズアルデヒドをパラジウムの還元当量の１．５倍量を加
えて分散させた溶液５０ｍ１を加えて、室温で反応させ
３０分間攪拌を続けたところパラジウムの微粒子が生成
して均一分散したオルガノゾルを得た。(Example 2) Using Pd (acac)2 as an organic solvent, MIBK and O
-Using a solution mixed by adding 1 volume each of xylene,
0.8 mi! J mol/l solution and its 50 mj! Separately with MIBK while stirring. - Add 50 ml of a solution prepared by adding 1.5 times the reduction equivalent of palladium and dispersing benzaldehyde to a solution in which 1% dioxane was added to a solution in which 1 volume of xylene was added and mixed, and the mixture was reacted at room temperature for 30 minutes. When stirring was continued for a minute, palladium fine particles were generated and a uniformly dispersed organosol was obtained.
該パラジウムの微粒子の平均粒子径を測定したところ９
３人であった。When the average particle diameter of the palladium fine particles was measured, it was 9.
There were three people.
また、オルガノゾルの安定性を観察したところ２日間後
でもまったく変化なかった。Furthermore, when the stability of the organosol was observed, there was no change at all even after 2 days.
（実施例３）
アセチルアセトンルテニウムを有機溶媒として、ＭＩＢ
Ｋを用いて１．０ミＩＪモル／１溶液とし、その、５０
＋ｎｊ！を攪拌しながら、別にＭＩＢＫにＤＢＣ２％を
加えた溶液にヒドラジンをルテニウムの還元当量の１．
２倍量を加えて分散させた溶液５０ｍＡ’を加えて、
室温で反応させ４５分間攪拌を続けたところルテニウム
の微粒子が生成して均一分散したオルガノゾルを得た。(Example 3) Using ruthenium acetylacetone as an organic solvent, MIB
K was used to make 1.0 μIJ mol/1 solution, and 50
+nj! Separately, add hydrazine to a solution of MIBK and 2% DBC while stirring to add 1.5% of the reducing equivalent of ruthenium.
Add 50 mA' of a solution made by adding twice the amount and dispersing it,
When the reaction was carried out at room temperature and stirring was continued for 45 minutes, ruthenium fine particles were generated to obtain a uniformly dispersed organosol.
該ルテニウムの微粒子の平均粒子径を測定したところ８
３人であった。When the average particle diameter of the ruthenium fine particles was measured, it was 8.
There were three people.
また、オルガノゾルの安定性を観察したところ２日間後
でもまったく変化なかった。Furthermore, when the stability of the organosol was observed, there was no change at all even after 2 days.
（実施例４）
酢酸ロジウムを有機溶媒として、０−キシレンを用いて
、１．０ミ！Ｊモル／β溶液とし、その５０ｍ（ｌを攪
拌しながら、別に０−キシレンにイソプロピルアルコー
ル３％を加えた溶液にギ酸をロジウムの還元当量の１．
３倍量を加えて分散させた溶液５０ｍＡを加えて、室温
で反応させ４５分間攪拌を続けたところロジウムの微粒
子が生成して均一分散したオルガノゾルを得た。(Example 4) Using rhodium acetate as an organic solvent and using 0-xylene, 1.0 m! J mol/β solution, and while stirring 50 ml of the solution, add 1.
50 mA of a solution obtained by adding and dispersing 3 times the amount was added, and the mixture was allowed to react at room temperature. Stirring was continued for 45 minutes, and fine particles of rhodium were generated to obtain a homogeneously dispersed organosol.
該ロジウムの微粒子の平均粒子径を測定したところ９０
人であった。When the average particle diameter of the rhodium fine particles was measured, it was 90.
It was a person.
また、オルガノゾルの安定性を観察したところ２日間後
でもまったく変化なかった。Furthermore, when the stability of the organosol was observed, there was no change at all even after 2 days.
（実施例５）
イリジウムレジネートを有機溶媒として、酢酸イソアミ
ルとクロロホルムを各１容づつ加えて混合した溶液を用
いて、１．ＯミＵモル／ｌ溶液とし、その５０ｍＡを攪
拌しながら、別に酢酸イソアミルとクロロホルムを各１
容づつ加えて混合した溶液にＤＢＣ２％を加えた溶液に
ヒドラジンをイリジウムの還元当量の１．２倍量を加え
て分散させた溶液５０ｍｊ２を加えて、室温で反応させ
４５分間攪拌を続けたところイリジウムの微粒子が生成
して均一分散したオルガノゾルを得た。(Example 5) Using a solution prepared by adding and mixing one volume each of isoamyl acetate and chloroform to iridium resinate as an organic solvent, 1. Make a solution of OmiU mol/l, and add 1 each of isoamyl acetate and chloroform while stirring at 50 mA.
50 mj2 of a solution prepared by adding and dispersing hydrazine in an amount of 1.2 times the reduction equivalent of iridium was added to a solution in which 2% DBC was added to the mixed solution, and the mixture was allowed to react at room temperature and stirring was continued for 45 minutes. An organosol in which iridium fine particles were generated and uniformly dispersed was obtained.
該イリジウムの微粒子の平均粒子径を測定したところ８
９八であった。When the average particle diameter of the iridium particles was measured, it was 8.
It was 98.
また、オルガノゾルの安定性を観察したところ２日間後
でもまったく変化なかった。Furthermore, when the stability of the organosol was observed, there was no change at all even after 2 days.
（実施例６）
ビス（アセチルアセトナト）白金を有機溶媒として、Ｍ
ＩＢＫと０−キシレンを各１容づつ加えて混合した溶液
を用いて、１．０ミ！１モル／ｌ溶液とし、その５０ｒ
ｒ＋ｊ！を攪拌しながら、別にＭＩＢＫと０−キシレン
を各１容づつ加えて混合した溶液にジオキサン１％を加
えた溶液にヒドラジンを白金の還元当量の１．２倍量を
加えて分散させた溶液５０ｍ１ｔを加えて、室温で反応
させ４５分間攪拌を続けたところ白金の微粒子が生成し
て均一分散したオルガノゾルを得た。(Example 6) Using bis(acetylacetonato)platinum as an organic solvent, M
Using a mixed solution of 1 volume each of IBK and 0-xylene, 1.0 mi! 1 mol/l solution and its 50r
r+j! While stirring, separately add 1 volume each of MIBK and 0-xylene, add 1% dioxane to the mixed solution, add hydrazine in an amount of 1.2 times the reduction equivalent of platinum, and disperse the solution to 50 ml 1 t. was added, and the mixture was allowed to react at room temperature and stirred for 45 minutes to produce a uniformly dispersed organosol in which fine particles of platinum were produced.
該白金の微粒子の平均粒子径を測定したところ９０Ａで
あった。The average particle size of the platinum fine particles was measured and found to be 90A.
また、オルガノゾルの安定性を観察したところ２日間後
でもまったく変化なかった。Furthermore, when the stability of the organosol was observed, there was no change at all even after 2 days.
（発明の効果）
本発明は、従来法では問題となっていた有機溶媒中に貴
金属微粒子の数を多くすると貴金属微粒子の粒子径がバ
ラツキを生じ易くなることとオルガノゾルとしての安定
性に欠ける点と、さらにゾルとしての安定性を高めるた
めに加える界面活性剤等が共存するという点を有機貴金
属化合物を有機溶媒に溶解し溶液に還元剤を加えて貴金
属を還元する方法により、粒子径のバラツキも少ない貴
金属微粒子を生成でき、しかも貴金属オルガノゾルとし
て安定したものが得られ、共存成分も比較的単純な有機
化合物から成るもので調製することができ、化学工業、
電気工業、電子工業等のおける利用分野の拡大に貢献で
きるものである。(Effects of the Invention) The present invention solves the problem of the conventional method, which is that when the number of noble metal fine particles is increased in an organic solvent, the particle diameter of the noble metal fine particles tends to vary and the organosol lacks stability. In addition, the method of dissolving the organic noble metal compound in an organic solvent and adding a reducing agent to the solution to reduce the noble metal, which involves the coexistence of a surfactant etc. that is added to increase the stability of the sol, also reduces the variation in particle size. It is possible to generate a small number of precious metal fine particles, and to obtain a stable noble metal organosol, and the coexisting components can be prepared from relatively simple organic compounds, making it suitable for the chemical industry,
This can contribute to the expansion of fields of use in the electrical industry, electronic industry, etc.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
剤を加えて有機溶媒中に貴金属微粒子を分散させること
を特徴とする貴金属オルガノゾルの調整方法。1. A method for preparing a noble metal organosol, which comprises adding a reducing agent to a solution of an organic noble metal compound dissolved in an organic solvent to disperse noble metal fine particles in the organic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19846788A JPH0248036A (en) | 1988-08-09 | 1988-08-09 | Preparation of noble metal organosol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19846788A JPH0248036A (en) | 1988-08-09 | 1988-08-09 | Preparation of noble metal organosol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0248036A true JPH0248036A (en) | 1990-02-16 |
Family
ID=16391592
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19846788A Pending JPH0248036A (en) | 1988-08-09 | 1988-08-09 | Preparation of noble metal organosol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0248036A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6051614A (en) * | 1991-12-28 | 2000-04-18 | Hidefumi Hirai | Method for preparing a non-aqueous dispersion of particles of a metal and/or a metal compound |
| CN114559030A (en) * | 2022-03-07 | 2022-05-31 | 石河子大学 | Noble metal nano sol and preparation method thereof |
-
1988
- 1988-08-09 JP JP19846788A patent/JPH0248036A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6051614A (en) * | 1991-12-28 | 2000-04-18 | Hidefumi Hirai | Method for preparing a non-aqueous dispersion of particles of a metal and/or a metal compound |
| CN114559030A (en) * | 2022-03-07 | 2022-05-31 | 石河子大学 | Noble metal nano sol and preparation method thereof |
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