JP3164969B2 - Method for producing gold compound for organic gold paste - Google Patents
Method for producing gold compound for organic gold pasteInfo
- Publication number
- JP3164969B2 JP3164969B2 JP13108294A JP13108294A JP3164969B2 JP 3164969 B2 JP3164969 B2 JP 3164969B2 JP 13108294 A JP13108294 A JP 13108294A JP 13108294 A JP13108294 A JP 13108294A JP 3164969 B2 JP3164969 B2 JP 3164969B2
- Authority
- JP
- Japan
- Prior art keywords
- gold
- gold compound
- producing
- organic
- 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.)
- Expired - Lifetime
Links
Description
【０００１】[0001]
【産業上の利用分野】本発明は、有機金ペーストの原料
として用いられるバルサム金と呼ばれる金化合物の製造
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a gold compound called balsam gold used as a raw material for an organic gold paste.
【０００２】[0002]
【従来の技術】有機金ペーストは、従前彩飾に用いられ
る金液の原料として用いられてきたが、現在ではサーマ
ルプリンタ（感熱式プリンタ）におけるサーマルヘッド
の電極部等にも用いられている。従来、有機金ペースト
の原料となる金化合物は、硫黄華をテルペンと共に煮沸
して茶褐色のオイル状を呈する硫黄バルサム（Ｓ Ｂａ
ｌｓａｍ）を作製する一方、塩化金酸結晶（ＨＡｕＣｌ
4 ）にエタノールを溶媒として加えて溶解し、この溶液
に上記硫黄バルサムを撹拌しながら反応させた後、これ
にエタノールを加えて金化合物を結晶化させ、生成され
た金化合物の結晶をろ取し、洗浄後乾燥することによ
り、褐色粉末状の目的物を得る方法によって製造されて
いる。2. Description of the Related Art Organic gold paste has been used as a raw material of gold solution used for coloring in the past, but is now used also as an electrode portion of a thermal head in a thermal printer (thermal printer). Conventionally, a gold compound used as a raw material of an organic gold paste is sulfur balsam (S Ba), which is obtained by boiling sulfur white with a terpene to exhibit a brown oily state.
sam) while chloroauric acid crystals (HAuCl
4 ) Ethanol was added as a solvent to dissolve, and the sulfur balsam was allowed to react with the solution while stirring. Then, ethanol was added thereto to crystallize the gold compound, and the generated gold compound crystals were collected by filtration. It is manufactured by a method of obtaining a brown powdery target by washing and drying.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、従来の
有機金ペースト用金化合物の製造方法では、原料として
高価な塩化金酸結晶とエタノールを用いているので、製
造にかかるコストが高くなる不具合がある。これに対し
て、原料として安価な塩化金酸溶液を用い、これにエタ
ノールを用いて反応させることが考えられているが、塩
酸が多く含まれているため、反応前にエタノールによっ
て塩化金酸が還元され、安定な金化合物を得ることがで
きない。そこで、本発明は、ペースト化する前段階とし
て溶剤（イソボニルアセテート）に溶かしてラスター化
した時に従来と同様に安定であり、かつ製造コストを低
減し得る有機金ペースト用金化合物の製造方法を提供す
ることを目的とする。However, in the conventional method of producing a gold compound for an organic gold paste, since expensive chloroauric acid crystals and ethanol are used as raw materials, there is a problem that the production cost is increased. . On the other hand, it is considered that an inexpensive chloroauric acid solution is used as a raw material, and the reaction is performed using ethanol.However, since a large amount of hydrochloric acid is contained, chloroauric acid is reacted with ethanol before the reaction. It cannot be reduced to obtain a stable gold compound. Therefore, the present invention provides a method for producing a gold compound for an organic gold paste, which is stable as before and can be reduced in production cost when dissolved in a solvent (isobonyl acetate) as a pre-pasting step. The purpose is to provide.
【０００４】[0004]
【課題を解決するための手段】前記課題を解決するた
め、本発明の有機金ペースト用金化合物の製造方法は、
塩化金酸溶液にイソプロピルアルコールを加えて撹拌
し、この溶液に硫黄バルサムを撹拌しながら加えて反応
させた後、これにイソプロピルアルコールを加えて金化
合物を結晶化させ、生成された金化合物の結晶をろ取
し、洗浄後乾燥することを特徴とする。前記反応は、70
〜90℃の温度で 0.5〜５時間かけるのが好ましく、特に
80℃の温度で１時間かけて行うことが好ましい。前記洗
浄は、適当量のイソプロピルアルコールを用いて行うこ
とが好ましい。又、前記乾燥は、減圧乾燥とすることが
好ましい。Means for Solving the Problems In order to solve the above problems, a method for producing a gold compound for an organic gold paste according to the present invention comprises:
Isopropyl alcohol is added to the chloroauric acid solution, and the mixture is stirred. Sulfur balsam is added to the solution with stirring, and the mixture is reacted. After that, isopropyl alcohol is added to crystallize the gold compound. Is filtered, washed and dried. The reaction is 70
It is preferable to take 0.5 to 5 hours at a temperature of ~ 90 ° C, especially
It is preferably carried out at a temperature of 80 ° C. for one hour. The washing is preferably performed using an appropriate amount of isopropyl alcohol. The drying is preferably performed under reduced pressure.
【０００５】[0005]
【作用】本発明の有機金ペースト用金化合物の製造方法
においては、溶媒としてのイソプロピルアルコールの還
元力が弱く、熱をかけても塩化金酸が還元されにくくな
り、かつ原料としての塩化金酸溶液とイソプロピルアル
コールが安価となる。反応温度が70℃未満では反応に時
間がかかりすぎ、90℃を越えると塩化金酸が還元される
可能性があり好ましくない。また反応時間は 0.5時間未
満では反応が完全に終了せず、また５時間を超えても反
応はそれ以上進まず無駄である。In the method for producing a gold compound for an organic gold paste according to the present invention, the reducing power of isopropyl alcohol as a solvent is weak, chloroauric acid is hardly reduced even when heated, and chloroauric acid as a raw material is reduced. The solution and isopropyl alcohol are cheaper. If the reaction temperature is lower than 70 ° C., the reaction takes too much time, and if it exceeds 90 ° C., chloroauric acid may be reduced, which is not preferable. If the reaction time is less than 0.5 hour, the reaction is not completed completely, and if it exceeds 5 hours, the reaction does not proceed any further and is useless.
【０００６】[0006]
【実施例】以下、本発明の実施例について従来例と共に
説明する。先ず、硫黄華 8.7ｇにα−ピネン 136ｇを加
え、 180℃の温度で９時間還流させた後、放冷し、茶褐
色オイル状を呈する硫黄バルサム約 140ｇを得た。次い
で、塩化金酸溶液（30重量％溶液）55ｇに溶媒としてイ
ソプロピルアルコール60mlを加えて撹拌し、この溶液に
上記硫黄バルサム53ｇを撹拌しながら加えて80℃の温度
で１時間かけて反応させた。放冷後、反応溶液にイソプ
ロピルアルコール 250mlを撹拌しながら加えて金化合物
を結晶化させ、生成された金化合物の結晶をろ取して適
当量のイソプロピルアルコールを用いて洗浄後、減圧乾
燥することにより、褐色粉末状の金化合物を得た（収量
約25ｇ）。DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below together with conventional examples. First, 136 g of sulfuric acid was added to 136 g of α-pinene, and the mixture was refluxed at a temperature of 180 ° C. for 9 hours, and then allowed to cool to obtain about 140 g of a brown oily sulfur balsam. Next, 60 ml of isopropyl alcohol was added as a solvent to 55 g of a chloroauric acid solution (30% by weight solution) and stirred. 53 g of the above-mentioned sulfur balsam was added to this solution with stirring, and the reaction was carried out at a temperature of 80 ° C. for 1 hour. . After allowing to cool, 250 ml of isopropyl alcohol is added to the reaction solution with stirring to crystallize the gold compound, and the crystals of the generated gold compound are collected by filtration, washed with an appropriate amount of isopropyl alcohol, and dried under reduced pressure. As a result, a brown powdery gold compound was obtained (yield: about 25 g).
【０００７】[0007]
【従来例】先ず、硫黄華 6.4ｇにα−ピネン 100ｇを加
え、 180℃の温度で６時間還流させた後、放冷し、茶褐
色オイル状を呈する硫黄バルサム約 100ｇを得た。次い
で、塩化金酸結晶15ｇにエタノール25mlを加えて溶解
し、この溶液に上記硫黄バルサム22.5ｇを撹拌しながら
加え、温度が下がり始めたら80℃の温度で１時間かけて
反応させた。放冷後、反応溶液にエタノール 120mlを撹
拌しながら加えて金化合物を結晶化させ、生成された金
化合物の結晶をろ取して適当量のエタノールを用いて洗
浄後、減圧乾燥することにより褐色粉末状の金化合物を
得た（収量約10ｇ）。Conventional Example First, 100 g of α-pinene was added to 6.4 g of sulfur flower, refluxed at a temperature of 180 ° C. for 6 hours, and then allowed to cool to obtain about 100 g of a brown oily sulfur balsam. Then, 15 g of chloroauric acid crystals were dissolved by adding 25 ml of ethanol, and 22.5 g of the above-mentioned sulfur balsam was added to this solution while stirring. When the temperature began to decrease, the reaction was carried out at 80 ° C. for 1 hour. After cooling, 120 ml of ethanol was added to the reaction solution with stirring to crystallize the gold compound.The crystals of the generated gold compound were collected by filtration, washed with an appropriate amount of ethanol, and dried under reduced pressure to brown. A powdery gold compound was obtained (yield: about 10 g).
【０００８】[0008]
【比較例】従来例において、塩化金酸結晶のかわりに、
塩化金酸溶液（30重量％）55ｇを用いたところ、エタノ
ールを加えると金が還元してしまい、反応が進行しなか
った。[Comparative Example] In the conventional example, instead of chloroauric acid crystals,
When 55 g of a chloroauric acid solution (30% by weight) was used, gold was reduced when ethanol was added, and the reaction did not proceed.
【０００９】上述した実施例及び従来例の金化合物にイ
ソボニルアセテートを溶剤として加えてラスターを調製
したところ、それぞれの経時変化は、表１に示すように
なった。Rasters were prepared by adding isobonyl acetate as a solvent to the gold compounds of the above-mentioned examples and the conventional example. The time-dependent changes were as shown in Table 1.
【００１０】[0010]
【表１】 [Table 1]
【００１１】表１からわかるように、本発明に係る金化
合物は、従来のものと、同様に約１箇月後に析出が発生
するが、その間における粘度変化はない。As can be seen from Table 1, the gold compound according to the present invention precipitates after about one month similarly to the conventional one, but there is no change in viscosity during that period.
【００１２】[0012]
【発明の効果】以上説明したように、本発明の有機金ペ
ースト用金化合物の製造方法によれば、溶媒としてのイ
ソプロピルアルコールの還元力が弱く、熱をかけても塩
化金酸が還元されにくくなるので、ペースト化の前段階
としてラスター化した後、従来と同様に約１箇月安定な
金化合物を得ることができる。又、原料としての塩化金
酸溶液とイソプロピルアルコールが、従来の原料に比し
て安価となるので、製造コストを低減することができ
る。As described above, according to the method for producing a gold compound for an organic gold paste of the present invention, the reducing power of isopropyl alcohol as a solvent is weak, and chloroauric acid is not easily reduced even when heat is applied. Therefore, after rasterization as a stage prior to pasting, a stable gold compound can be obtained for about one month as in the past. Further, since the chloroauric acid solution and isopropyl alcohol as the raw materials are less expensive than the conventional raw materials, the production cost can be reduced.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C07F 1/12 C01G 7/00 ＣＡ（ＳＴＮ) ＣＡＯＬＤ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ) ＷＰＩＤＳ（ＳＴＮ)──────────────────────────────────────────────────の Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) C07F 1/12 C01G 7/00 CA (STN) CAOLD (STN) REGISTRY (STN) WPIDS (STN)
Claims (4)
を加えて撹拌し、この溶液に硫黄バルサムを撹拌しなが
ら加えて反応させた後、これにイソプロピルアルコール
を加えて金化合物を結晶化させ、生成された金化合物の
結晶をろ取し、洗浄後乾燥することを特徴とする有機金
ペースト用金化合物の製造方法。1. An isopropyl alcohol solution is added to a chloroauric acid solution, and the mixture is stirred. A sulfur balsam is added to the solution while stirring to cause a reaction. Then, isopropyl alcohol is added to the solution to crystallize a gold compound. A method for producing a gold compound for an organic gold paste, comprising filtering a crystal of the gold compound obtained, washing and drying the crystal.
乃至５時間かけて行うことを特徴とする請求項１記載の
有機金ペースト用金化合物の製造方法。2. The reaction is carried out at a temperature of 70 ° C. to 90 ° C. for 0.5 hour.
2. The method for producing a gold compound for an organic gold paste according to claim 1, wherein the method is carried out for from 5 to 5 hours.
コールを用いて行うことを特徴とする請求項１又は２記
載の有機金ペースト用金化合物の製造方法。3. The method for producing a gold compound for an organic gold paste according to claim 1, wherein the washing is performed using an appropriate amount of isopropyl alcohol.
する請求項１、２又は３記載の有機金ペースト用金化合
物の製造方法。4. The method for producing a gold compound for an organic gold paste according to claim 1, wherein the drying is performed under reduced pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13108294A JP3164969B2 (en) | 1994-05-20 | 1994-05-20 | Method for producing gold compound for organic gold paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13108294A JP3164969B2 (en) | 1994-05-20 | 1994-05-20 | Method for producing gold compound for organic gold paste |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07309877A JPH07309877A (en) | 1995-11-28 |
| JP3164969B2 true JP3164969B2 (en) | 2001-05-14 |
Family
ID=15049574
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13108294A Expired - Lifetime JP3164969B2 (en) | 1994-05-20 | 1994-05-20 | Method for producing gold compound for organic gold paste |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3164969B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112735631B (en) * | 2020-12-21 | 2022-10-21 | 有研工程技术研究院有限公司 | Low-viscosity organic gold paste capable of being sintered on surface of circuit board substrate at low temperature |
-
1994
- 1994-05-20 JP JP13108294A patent/JP3164969B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07309877A (en) | 1995-11-28 |
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