JP2603508B2 - Pack for preparing palladium organosol and method for producing the same - Google Patents
Pack for preparing palladium organosol and method for producing the sameInfo
- Publication number
- JP2603508B2 JP2603508B2 JP63081613A JP8161388A JP2603508B2 JP 2603508 B2 JP2603508 B2 JP 2603508B2 JP 63081613 A JP63081613 A JP 63081613A JP 8161388 A JP8161388 A JP 8161388A JP 2603508 B2 JP2603508 B2 JP 2603508B2
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- organosol
- pack
- colloid
- organic solvent
- 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.)
- Expired - Fee Related
Links
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims description 170
- 229910052763 palladium Inorganic materials 0.000 title claims description 85
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 150000002940 palladium Chemical class 0.000 claims description 3
- 238000005345 coagulation Methods 0.000 claims description 2
- 230000015271 coagulation Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 description 20
- 239000007864 aqueous solution Substances 0.000 description 17
- 238000002360 preparation method Methods 0.000 description 17
- 238000007747 plating Methods 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 239000000123 paper Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 238000012856 packing Methods 0.000 description 5
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 4
- 230000001112 coagulating effect Effects 0.000 description 4
- 239000004745 nonwoven fabric Substances 0.000 description 4
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 239000012279 sodium borohydride Substances 0.000 description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 241001122767 Theaceae Species 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 1
- 229910001617 alkaline earth metal chloride Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical class [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Colloid Chemistry (AREA)
- Catalysts (AREA)
- Chemically Coating (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、パラジウムオルガノゾル調製用パック及び
その製造法に関するものであり、本発明に係るパラジウ
ムオルガノゾル調製用パックは、無電解金属めっきを施
す際の触媒付与のために使用される。Description: TECHNICAL FIELD The present invention relates to a palladium organosol preparation pack and a method for producing the same, and the palladium organosol preparation pack according to the present invention comprises an electroless metal plating. Used for application of catalyst during application.
紙や不織布などの繊維成形物、ガラス、セラミックス
及び高分子材料の基材は本来絶縁体であるが、これら基
材に無電解金属めっきを施して各種金属を付与すること
により、磁気的性質及び導電性等の電気的性質を持たせ
ることが行われている。Fiber substrates such as paper and nonwoven fabrics, glass, ceramics and polymer materials are originally insulators, but by applying electroless metal plating to these substrates and adding various metals, their magnetic properties and 2. Description of the Related Art Electrical properties such as conductivity have been provided.
また、金属や金属酸化物の場合も、これら基材に無電
解金属めっきを施して、他の各種金属を付与することに
より、磁気的、電気的性質を改良したり、又は、本来有
する特性とは全く別の新しい磁気的、電気的性質を持た
せることが行われている。Also, in the case of metals and metal oxides, by applying electroless metal plating to these substrates and adding other various metals, the magnetic and electrical properties are improved, or the properties originally possessed Has been given a completely new magnetic and electrical properties.
従来より、無電解金属めっきを施すに当たって、被め
っき物に、有機溶媒を分散媒とするパラジウムオルガノ
ゾルを付着させた後、該分散媒である有機溶媒を蒸発さ
せることによりパラジウムコロイドを付与し、次いで、
無電解金属めっきする方法（特開昭61−227175号公報）
が提案されている。Conventionally, in performing electroless metal plating, on the object to be plated, after adhering a palladium organosol having an organic solvent as a dispersion medium, evaporating the organic solvent as a dispersion medium to give a palladium colloid, Then
Electroless metal plating method (JP-A-61-227175)
Has been proposed.
上記の無電解金属めっきに用いられているパラジウム
オルガノゾルは、パラジウムヒドロゾルから凝集沈澱物
を形成させた後、水溶液部分を過またはデカンテーシ
ョンにより除き、または水溶液共存下に有機溶媒を加え
て再溶解させてなる溶液である。The palladium organosol used in the above electroless metal plating forms an aggregated precipitate from the palladium hydrosol, and then removes the aqueous solution portion by excess or decantation, or adds an organic solvent in the coexistence of the aqueous solution to re-use. It is a solution that is dissolved.
前述のパラジウムオルガノゾルの製造には、パラジウ
ムヒドロゾルを凝集沈澱させた後、有機溶媒に再溶解さ
せる工程、又は、水溶液共存下に有機溶媒を加え後、水
相と有機溶媒相とを分離する為の工程に特殊な大型分液
装置が必須不可欠とされている。In the production of the above-mentioned palladium organosol, a step of coagulating and precipitating the palladium hydrosol and then re-dissolving it in an organic solvent, or adding an organic solvent in the presence of an aqueous solution, and separating an aqueous phase and an organic solvent phase It is considered that a special large-sized liquid separation device is indispensable for the process.
また、多量の有機溶媒を使用する上、パラジウムオル
ガノゾルを製造後に貯蔵しておく場合には安全で耐有機
溶媒性で且つパラジウムに腐食されない特殊な容器が必
要となる。更には、工程の安全面、或いはパラジウムオ
ルガノゾルの輸送面に対しても注意する必要があり、全
般的にその取扱いには不便であるという諸問題があっ
た。In addition, when a palladium organosol is stored after production, in addition to using a large amount of organic solvent, a special container that is safe, resistant to organic solvents and not corroded by palladium is required. Furthermore, it is necessary to pay attention to the safety of the process and the transportation of the palladium organosol, and there is a problem that the handling is generally inconvenient.
本発明は、上記諸問題を解決することを技術的課題と
するものである。An object of the present invention is to solve the above-mentioned problems.
本発明者らは、前記技術的課題を解決するために長期
に亘り鋭意検討を重ねた結果、有機溶媒で再溶解させる
前のパラジウムヒドロゾルを凝集沈澱させたパラジウム
コロイドに着目し、予め該パラジウムコロイドを担持さ
せた担持物を得、次いでこの担持物を有機溶媒中に投入
し、担持されているパラジウムコロイドを機械的に解膠
してパラジウムオルガノゾルを調製することができれ
ば、パラジウムオルガノゾルの製造時における従来の特
殊な大型分液装置の必要性が無くなると同時に、パラジ
ウムコロイドを担持させてなる担持物には有機溶媒が含
んでおらず、よって貯蔵に際しても特別な容器は必要も
なく、増やして、安全衛生、輸送面に対しても特別注意
を払うことも回避できると考えた。更に本発明者は取扱
い至便の為にパラジウムコロイドを担持させた担持物の
パック化という着想を得、本発明を完成するに至ったの
である。The present inventors have conducted intensive studies over a long period of time in order to solve the technical problem, and as a result, focused on a palladium colloid obtained by coagulating and precipitating a palladium hydrosol before re-dissolving with an organic solvent, If a supported material carrying a colloid is obtained, and then the loaded material is poured into an organic solvent, and the supported palladium colloid can be mechanically peptized to prepare a palladium organosol, a palladium organosol can be prepared. At the same time as the necessity of a conventional special large-sized liquid separation device at the time of production is eliminated, the organic material is not contained in the carrier that carries the palladium colloid, so that no special container is required for storage, We thought that it would be possible to avoid paying special attention to health and safety and transportation. Further, the inventor of the present invention obtained the idea of packing a loaded material carrying a palladium colloid for convenient handling, and completed the present invention.
即ち、本発明は、パラジウムコロイドを担持させた担
持物を通液性パック材に封入してなるパラジウムオルガ
ノゾル調製用パック及びパラジウム塩水溶液を還元処理
して得られたパラジウムヒドロゾル中に電解質を添加し
てパラジウムコロイドを凝集沈澱させ、次いで水洗し、
材を用いて別することにより該材にパラジウムコ
ロイドを担持させ、続いて該担持物を乾燥した後、通液
性パック材に封入することを特徴とするパラジウムオル
ガノゾル調製用パックの製造法である。That is, the present invention provides an electrolyte in a palladium organosol preparation pack and a palladium salt aqueous solution obtained by reduction treatment of a palladium salt aqueous solution obtained by enclosing a loaded material carrying a palladium colloid in a liquid-pack material. Addition to coagulate and precipitate the palladium colloid, followed by washing with water,
The palladium colloid is supported on the material by separating using a material, and then the supported material is dried, and then sealed in a liquid-permeable pack material. is there.
先ず、本発明において最も重要な点は、パラジウムヒ
ドロゾルを凝集沈澱させ得られるパラジウムコロイドを
担持させた担持物を通液性のパック材に封入した点にあ
る。このパラジウムオルガノゾル調製用パックを、無電
解金属めっきにおける触媒付与のために使用する場合に
は、該パックを所要の有機溶媒中に投入し、パック内の
担持物に担持されているパラジウムコロイドを機械的に
解膠することによってパラジウムオルガノゾルを調製し
て使用することができる。この際、使用されるパックの
量に応じて所望の量の有機溶媒で賭うことができる。First, the most important point in the present invention is that a carrier carrying palladium colloid obtained by coagulating and precipitating a palladium hydrosol is enclosed in a liquid-permeable packing material. When the palladium organosol preparation pack is used for providing a catalyst in electroless metal plating, the pack is charged into a required organic solvent, and the palladium colloid supported on a carrier in the pack is removed. A palladium organosol can be prepared and used by mechanical peptization. At this time, it is possible to bet with a desired amount of the organic solvent according to the amount of the pack used.
次に、本発明実施にあたっての諸条件について述べ
る。Next, conditions for implementing the present invention will be described.
本発明におけるパラジウムオルガノゾル調製用パック
の出発物であるパラジウムヒドロゾルは、次の方法によ
り調製することができる。The palladium hydrosol which is the starting material of the palladium organosol preparation pack in the present invention can be prepared by the following method.
陽イオン、陰イオン性及び非イオン性界面活性剤の一
種又は二種以上の存在下、パラジウム（II）塩水溶液、
好ましくは塩化パラジウム（II）水溶液を水素化ホウ素
ナトリウム、ジメチルアミンボラン、ヒドラジンなどの
還元剤で還元処理して得られる（特開昭61−207666号公
報）。An aqueous solution of palladium (II) salt in the presence of one or more cationic, anionic and nonionic surfactants,
It is preferably obtained by reducing an aqueous palladium (II) chloride solution with a reducing agent such as sodium borohydride, dimethylamine borane, hydrazine or the like (JP-A-61-207666).
また、上記方法で得られるパラジウムヒドロゾルから
凝集沈澱物を形成させるためには、パラジウムヒドロゾ
ル中に電解質を添加する方法がとられる。電解質として
は、塩化カリウム、塩化バリウム、臭化ナトリウム、硝
酸カルシウム等のアルカリ土類金属の塩化物、臭化物、
又は、硝酸塩の水溶液又は固体が使用できる。この場合
電解質の濃度がパラジウムのモル比に対して30倍以上で
あれば凝集沈澱させることができる。In order to form an aggregated precipitate from the palladium hydrosol obtained by the above method, a method of adding an electrolyte to the palladium hydrosol is used. As the electrolyte, potassium chloride, barium chloride, sodium bromide, alkaline earth metal chlorides such as calcium nitrate, bromide,
Alternatively, an aqueous solution or solid of nitrate can be used. In this case, if the concentration of the electrolyte is at least 30 times the molar ratio of palladium, coagulation and precipitation can be performed.
生成した凝集沈澱物は、水洗後、ヌッチェ等で濾過す
ることにより水溶液部分は除去され、担持物となる材
上にパラジウムコロイドが担持される。次いで、該パラ
ジウムコロイドを担持している材を乾燥して通液性の
パック材に封入してパラジウムオルガノゾル調製用パッ
クを得る。The resulting aggregated precipitate is washed with water and then filtered with a Nutsche or the like to remove the aqueous solution portion, and the palladium colloid is supported on the material to be supported. Next, the material carrying the palladium colloid is dried and sealed in a liquid-permeable pack material to obtain a palladium organosol preparation pack.
材としては、紙、メンブランフィルタ、布等が
使用できる。As the material, paper, a membrane filter, cloth, or the like can be used.
乾燥温度はパラジウム金属が酸化されない温度範囲で
且つ材が焼けない温度範囲であればよい。The drying temperature may be within a temperature range where the palladium metal is not oxidized and a temperature range where the material is not burned.
また、通液性のパック材としては、使用する有機溶媒
の浸透可能のもので、且つ不溶なものであれば使用で
き、特に強い湿潤強度を有し、通気性のある材質のパッ
ク材が好ましい。例えば、紙、不織布の素材が使用でき
る。紙の場合には比較的繊維長の長いパルプ、あるいは
合成繊維や半合成繊維をパルプ状にしたもの、不織布の
場合には合成樹脂（ポリエチレン、ポリプロピレン、ポ
リアミドなど）からなる繊維や半合成繊維（レーヨン、
アセテートなど）が好ましい。紙や不織布は従来のどの
ような方法によって製造されたものでもよいが、あまり
目の詰まったものや、厚めのものは好ましくない。例え
ば目付量で示すと20〜40g/m2範囲のものが好ましい。As the liquid-permeable packing material, any packing material that can penetrate the organic solvent to be used and that is insoluble can be used, and a packing material having a particularly strong wet strength and a gas-permeable material is preferable. . For example, materials of paper and nonwoven fabric can be used. In the case of paper, pulp with a relatively long fiber length, or pulp made of synthetic or semi-synthetic fibers, and in the case of non-woven fabric, fibers or semi-synthetic fibers made of synthetic resin (polyethylene, polypropylene, polyamide, etc.) Rayon,
Acetate) is preferred. The paper or nonwoven fabric may be manufactured by any conventional method, but not so tight or thick. For example, in terms of the basis weight, those having a range of 20 to 40 g / m 2 are preferable.
本発明のパラジウムオルガノゾル調製用パックを用い
て、無電解金属めっきにおける触媒付与させるには、該
パックを有機溶媒中に投入し、パック内に封入されてい
る担持物に担持されているパラジウムコロイドを機械的
な処理で解膠してパラジウムオルガノゾルを調製する。Using the palladium organosol preparation pack of the present invention to apply a catalyst in electroless metal plating, the pack is put into an organic solvent, and the palladium colloid supported on the carrier encapsulated in the pack is charged. Is peptized by mechanical treatment to prepare a palladium organosol.
パラジウムコロイドを解膠させる機械的な処理として
は超音波照射処理が好ましい。As a mechanical treatment for peptizing the palladium colloid, an ultrasonic irradiation treatment is preferable.
パラジウムオルガノゾルを調製する際に、有機溶媒と
して用いられる物質としては、ヘキサン、ベンゼン等の
炭化水素、クロロホルム等のハロゲン置換炭化水素が使
用できる。When preparing a palladium organosol, as a substance used as an organic solvent, hydrocarbons such as hexane and benzene, and halogen-substituted hydrocarbons such as chloroform can be used.
本発明のパラジウムオルガノゾル調製用パックを用い
て調製されるパラジウムオルガノゾルは、その分散状態
が極めて安定で、空気中で数ケ月以上の長期間に亘っ
て、沈澱を生じることなく均一透明な状態でも保存でき
る。The palladium organosol prepared using the palladium organosol preparation pack of the present invention has an extremely stable dispersion state, and is uniform and transparent without precipitation for a long period of several months or more in air. But you can save.
次に、実施例及び使用例により本発明を説明する。 Next, the present invention will be described with reference to examples and use examples.
尚、表面抵抗は、MCP−TESTER・LORESTA低抵抗表面抵
抗計（三菱油化（株）製）により測定したものである。The surface resistance was measured by using an MCP-TESTER LORESTA low resistance surface resistance meter (manufactured by Mitsubishi Yuka Corporation).
めっきの密着性は、めっき終了１時間後にスコッチメ
ンディングテープ（住友スリーエム（株））をめっき物
上に強く貼り付け、引きはがすことにより調べた。One hour after the completion of the plating, the adhesion of the plating was examined by strongly attaching a Scotch mending tape (Sumitomo 3M Limited) on the plating and peeling it off.
〔実施例１〕 無水塩化パラジウム（II）1m molを塩化ナトリウム5m
molを含む純水10mlに溶解し、純水で930mlに希釈し
た。この溶液を激しく撹拌しながら、ドデシルベンゼン
スルホン酸ナトリウム0.2gの水溶液20mlを加え、これに
水素化ホウ素ナトリウム4m molの水溶液50mlを滴下する
と溶液の色が黒褐色に急変し、均一透明なパラジウムヒ
ドロゾル１が得られた。続いて該パラジウムヒドロゾ
ル中に硝酸カルシウム66m mol水溶液100mlを加え、一夜
放置して黒色沈澱を形成させた後、水洗し、ヌッチェで
過することにより紙（No.6）にパラジウムコロイド
を担持させ、次いで60℃で乾燥して0.10gのパラジウム
コロイドを担持した担持物を得た。[Example 1] 1 mmol of anhydrous palladium (II) chloride was added to 5 m of sodium chloride.
It was dissolved in 10 ml of pure water containing mol and diluted to 930 ml with pure water. While vigorously stirring this solution, 20 ml of an aqueous solution of 0.2 g of sodium dodecylbenzenesulfonate was added, and 50 ml of an aqueous solution of 4 mmol of sodium borohydride was added dropwise.The color of the solution rapidly changed to black-brown, and a uniform transparent palladium hydrosol was added. 1 was obtained. Subsequently, 100 ml of a 66 mM aqueous solution of calcium nitrate was added to the palladium hydrosol, and the mixture was allowed to stand overnight to form a black precipitate. Then, the precipitate was washed with water and passed through a nutsche to support the palladium colloid on paper (No. 6). Then, the support was dried at 60 ° C. to obtain 0.10 g of a support carrying palladium colloid.
得られたパラジウムコロイド担持物を、目付が約20g/
m2のティーバッグフィルター紙（ヒートパックMW（日本
紙業（株）製）を用いて得た3cm×4cmの大きさで紐を附
した袋に封入し、袋の口を加熱して溶融接着してパラジ
ウムオルガノゾル調製用パックを得た。The obtained palladium colloid carrier has a basis weight of about 20 g /
m 2 tea bag filter paper (sealed in bags denoted by the string in the size of 3 cm × 4 cm was obtained using a heat pack MW (manufactured by Nippon Paper Co.), melt adhesion by heating the mouth of the bag Thus, a palladium organosol preparation pack was obtained.
〔実施例２〕 無水塩化パラジウム（II）2m molを塩化ナトリウム5m
molを含む純水10mlに溶解し、純水で860mlに希釈し
た。この溶液を激しく撹拌しながら、ステアリルトリメ
チルアンモニウムクロライド0.4gの水溶液40mlを加え、
これに水素化ホウ素ナトリウム8m molの水溶液100mlを
滴下すると溶液の色が黒褐色に急変し、均一透明なパラ
ジウムヒドロゾル１が得られた。続いて該パラジウム
ヒドロゾル中に塩化カルシウム400m mol水溶液100mlを
加え、一夜放置して黒色沈澱を形成させた後、水洗し、
ヌッチェで過することによりメンブランフィルター上
にパラジウムコロイドを担持させ、次いで70℃で乾燥し
て0.21gのパラジウムコロイドを担持した担持物を得
た。[Example 2] 2 mmol of anhydrous palladium (II) chloride was added to 5 m of sodium chloride.
It was dissolved in 10 ml of pure water containing mol and diluted to 860 ml with pure water. While vigorously stirring this solution, an aqueous solution of 0.4 g of stearyltrimethylammonium chloride 0.4 g was added,
When 100 ml of an aqueous solution of 8 mmol of sodium borohydride was added dropwise thereto, the color of the solution rapidly changed to black-brown, and uniform transparent palladium hydrosol 1 was obtained. Subsequently, 100 ml of a 400 mM aqueous solution of calcium chloride was added to the palladium hydrosol, and the mixture was allowed to stand overnight to form a black precipitate.
The palladium colloid was supported on the membrane filter by passing through a nutsche, and then dried at 70 ° C. to obtain 0.21 g of a supported palladium colloid.
得られたパラジウムコロイド担持物を、目付が約20g/
m2のティーバッグフィルター紙（ヒートロンGS（日本紙
業（株）製）を用いて得た3cm×4cmの大きさで紐を附し
た袋に封入し、袋の口を加熱して溶融接着してパラジウ
ムオルガノゾル調製用パックを得た。The obtained palladium colloid carrier has a basis weight of about 20 g /
sealed in bags denoted by the string in m 2 of the tea bag filter paper (Hitoron GS (size of 3 cm × 4 cm was obtained using the Nippon Paper Co., Ltd.), melt bonded by heating the mouth of the bag Thus, a palladium organosol preparation pack was obtained.
〔実施例３〕 無水塩化パラジウム（II）1m molを塩化ナトリウム5m
molを含む純水10mlに溶解し、純水で930mlに希釈し
た。この溶液を激しく撹拌しながら、ドデシルベンゼン
スルホン酸ナトリウム0.2gの水溶液20mlを加え、これに
水素化ホウ素ナトリウム4m molの水溶液50mlを滴下する
と溶液の色が黒褐色に急変し、均一透明なパラジウムヒ
ドロゾル１が得られた。続いて該パラジウムヒドロゾ
ル中に塩化カルシウム100m mol水溶液100mlを加え、一
夜放置して黒色沈澱を形成させた後、水洗し、ヌッチェ
で過することにより紙（No.6）上にパラジウムコロ
イドを担持させ、次いで80℃で乾燥して0.11gのパラジ
ウムコロイドを担持した担持物を得た。Example 3 1 mmol of anhydrous palladium (II) chloride was added to 5 m of sodium chloride
It was dissolved in 10 ml of pure water containing mol and diluted to 930 ml with pure water. While vigorously stirring this solution, 20 ml of an aqueous solution of 0.2 g of sodium dodecylbenzenesulfonate was added, and 50 ml of an aqueous solution of 4 mmol of sodium borohydride was added dropwise.The color of the solution rapidly changed to black-brown, and a uniform transparent palladium hydrosol was added. 1 was obtained. Subsequently, 100 ml of a 100 mM aqueous solution of calcium chloride was added to the palladium hydrosol, and the mixture was allowed to stand overnight to form a black precipitate, washed with water and passed through a nutsche to carry palladium colloid on paper (No. 6). Then, it was dried at 80 ° C. to obtain 0.11 g of a support carrying palladium colloid.
得られたパラジウムコロイド担持物を、目付が約40g/
m2のティーバッグフィルター紙（ヒートパックMC（日本
紙業（株）製）を用いて得た3cm×4cmの大きさで紐を附
した袋に封入し、袋の口を加熱して溶融接着してパラジ
ウムオルガノゾル調製用パックを得た。The obtained palladium colloid carrier has a basis weight of about 40 g /
m 2 tea bag filter paper (sealed in bags denoted by the string in the size of 3 cm × 4 cm was obtained using a heat pack MC (manufactured by Nippon Paper Co.), melt adhesion by heating the mouth of the bag Thus, a palladium organosol preparation pack was obtained.
実施例１により得られたパラジウムオルガノゾル調製
用パック２袋をトルエン１が存在する容器中に投入
し、超音波照射処理を30分間施してパック内の担持物に
吸着しているパラジウムコロイドを解膠させ、溶液中の
パラジウムコロイドの濃度が0.02％となった状態でパラ
ジウムオルガノゾル調製用パックを引き上げ、トルエン
を分散とする黒褐色透明なパラジウムオルガノゾルを調
製した。Two packs of the palladium organosol preparation pack obtained in Example 1 were put into a vessel containing toluene 1 and subjected to ultrasonic irradiation treatment for 30 minutes to dissolve palladium colloid adsorbed on the carrier in the pack. The palladium organosol preparation pack was pulled up in a state where the concentration of the palladium colloid in the solution was 0.02% to prepare a black-brown transparent palladium organosol in which toluene was dispersed.
酸化アルミニウム成型体（2.5cm×1.0cm×0.05cm）を
上記パラジウムオルガノゾル溶液中に２分間浸漬した
後、１分間加熱することにより有機溶媒であるトルエン
を蒸発させ、パラジウムコロイドが付与された酸化アル
ミニウム成型体を得た。An aluminum oxide molded body (2.5 cm × 1.0 cm × 0.05 cm) is immersed in the above-mentioned palladium organosol solution for 2 minutes, and then heated for 1 minute to evaporate toluene as an organic solvent, thereby oxidizing the palladium colloid. An aluminum molded body was obtained.
別に、0.8mol/のロッセル塩と0.8mol/の水酸化ナ
トリウム及び0.5mol/の硫酸銅（II）５水塩を純水に
溶解して100mlとし、さらに35％ホルムアルデヒド溶液1
00mlを加えて混合して無電解金属めっき液を調製した。Separately, 0.8 mol / rossel salt, 0.8 mol / sodium hydroxide and 0.5 mol / copper (II) sulfate pentahydrate are dissolved in pure water to make 100 ml, and a 35% formaldehyde solution 1
00 ml was added and mixed to prepare an electroless metal plating solution.
この無電解銅めっき液に、上記パラジウムコロイドが
付与された酸化アルミニウム成型体25℃で30分間浸漬し
た後、水洗、乾燥した。The aluminum oxide molded body provided with the above-mentioned palladium colloid was immersed in the electroless copper plating solution at 25 ° C. for 30 minutes, washed with water and dried.
得られた酸化アルミニウム成型体の表面は、銅めっき
による赤色を帯びた金属光沢を呈していた。The surface of the obtained aluminum oxide molded body exhibited a metallic luster with a reddish color due to copper plating.
この酸化アルミニウム成型体にメンディングテープを
強く貼り引き剥がしたところ銅被膜は剥離しなかった。
また、この酸化アルミニウム成型体の表面抵抗は0.1Ω
／□であった。When a mending tape was strongly adhered to the aluminum oxide molded product and peeled off, the copper film was not peeled off.
The surface resistance of this aluminum oxide molded product is 0.1Ω.
/ □.
尚、パラジウムオルガノゾル調製用パックで調製した
パラジウムオルガノゾルは、空気中、常温で約６ケ月後
においても沈澱を生じることなく均一透明なものであっ
た。The palladium organosol prepared with the palladium organosol preparation pack was uniform and transparent without precipitation even after about 6 months at room temperature in the air.
本発明に係るパラジウムオルガノゾル調製用パックを
使用してパラジウムオルガノゾルを調製する場合には、
従来のパラジウムオルガノゾルの調製時に見られるよう
な、パラジウムヒドロゾルを凝集沈澱させた後、有機溶
媒に再溶解させる工程及び水相と有機溶媒相とを分離す
る為の工程に必要とされている特殊な大型分液装置は不
必要となる。When preparing a palladium organosol using the palladium organosol preparation pack according to the present invention,
It is required for a process of coagulating and precipitating a palladium hydrosol and then re-dissolving it in an organic solvent and a process of separating an aqueous phase and an organic solvent phase, such as those found in the preparation of conventional palladium organosols. A special large liquid separation device is unnecessary.
また、パラジウムオルガノゾル調製用パックは、有機
溶媒を全く使用しておらず、大量に製造してもこの貯
蔵、輸送面に対して安全で衛生的であると同時に、所定
量の有機溶媒に所定量のパックを投入し、ついで機械的
な処理等で担持物に担持されているパラジウムコロイド
を解膠させ容易にパラジウムオルガノゾルを調製するこ
とができる携帯に便利でしかも長期間の保存に耐えるこ
とができるものである。In addition, the palladium organosol preparation pack does not use any organic solvent, and is safe and sanitary for storage and transportation even when manufactured in large quantities, and at the same time, it can be stored in a predetermined amount of organic solvent. A palladium organosol can be easily prepared by pulverizing the palladium colloid carried on the carrier by mechanical treatment, etc. Can be done.
Claims (2)
通液性パック材に封入してなるパラジウムオルガノゾル
調製用パック。1. A pack for preparing a palladium organosol, wherein a carrier carrying a palladium colloid is enclosed in a liquid-pack material.
たパラジウムヒドロゾル中に電解質を添加してパラジウ
ムコロイドを凝集沈澱させ、次いで水洗し、濾材を用い
て濾別することにより該濾材にパラジウムコロイドを担
持させ、続いて該担持物を乾燥した後、通液性パック材
に封入することを特徴とするパラジウムオルガノゾル調
製用パックの製造法。2. An electrolyte is added to a palladium hydrosol obtained by reducing an aqueous palladium salt solution to cause coagulation and precipitation of a palladium colloid, followed by washing with water and filtration using a filter medium, whereby palladium is added to the filter medium. A method for producing a palladium organosol-preparing pack, comprising supporting a colloid, subsequently drying the supported substance, and enclosing in a liquid-permeable pack material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63081613A JP2603508B2 (en) | 1988-04-01 | 1988-04-01 | Pack for preparing palladium organosol and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63081613A JP2603508B2 (en) | 1988-04-01 | 1988-04-01 | Pack for preparing palladium organosol and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01255673A JPH01255673A (en) | 1989-10-12 |
| JP2603508B2 true JP2603508B2 (en) | 1997-04-23 |
Family
ID=13751170
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63081613A Expired - Fee Related JP2603508B2 (en) | 1988-04-01 | 1988-04-01 | Pack for preparing palladium organosol and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2603508B2 (en) |
-
1988
- 1988-04-01 JP JP63081613A patent/JP2603508B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01255673A (en) | 1989-10-12 |
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