JP3039019B2 - Method for storing N-methyl-2-pyrrolidone - Google Patents
Method for storing N-methyl-2-pyrrolidoneInfo
- Publication number
- JP3039019B2 JP3039019B2 JP3198054A JP19805491A JP3039019B2 JP 3039019 B2 JP3039019 B2 JP 3039019B2 JP 3198054 A JP3198054 A JP 3198054A JP 19805491 A JP19805491 A JP 19805491A JP 3039019 B2 JP3039019 B2 JP 3039019B2
- Authority
- JP
- Japan
- Prior art keywords
- pyrrolidone
- methyl
- copper
- present
- storing
- 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
Landscapes
- Pyrrole Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、Ｎ−メチル−２−ピロ
リドンを大気中で取り扱う方法に関する。The present invention relates to a method for handling N-methyl-2-pyrrolidone in the atmosphere.
【０００２】[0002]
【従来の技術】Ｎ−メチル−２−ピロリドンは、合成樹
脂の良溶剤であり、ポリマー合成用、塗料成分、洗浄液
等として広く用いられている。最近では、電子部品、特
に集積回路封止素子の封止剤のバリを除去するための洗
浄液として利用されている。2. Description of the Related Art N-methyl-2-pyrrolidone is a good solvent for synthetic resins, and is widely used for polymer synthesis, as a paint component, as a cleaning liquid, and the like. Recently, it has been used as a cleaning liquid for removing burrs of an electronic component, particularly a sealant of an integrated circuit sealing element.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、本発明
者等は、Ｎ−メチル−２−ピロリドンの大気中での安定
性を検討したところ、Ｎ−メチル−２−ピロリドンの過
酸化物が生成すること、特に集積回路封止素子用の洗浄
液として５０〜１５０°Ｃに加温した場合に、過酸化物
の生成が著しく、安全上問題があることを見い出した。However, the present inventors have studied the stability of N-methyl-2-pyrrolidone in the atmosphere, and found that N-methyl-2-pyrrolidone peroxide is produced. In particular, it has been found that when heated to 50 to 150 ° C. as a cleaning liquid for an integrated circuit sealing element, peroxide is remarkably generated, which poses a safety problem.
【０００４】この問題に対し、Ｎ−メチル−２−ピロリ
ドンにいわゆるハイドロキノンのような還元性物質を添
加することも考えられるが、多くの用途で用いられるＮ
−メチル−２−ピロリドン中に還元性物質等の活性物質
を添加溶解させることは一般的に好ましくない。To solve this problem, it is conceivable to add a reducing substance such as so-called hydroquinone to N-methyl-2-pyrrolidone.
It is generally not preferable to dissolve an active substance such as a reducing substance in -methyl-2-pyrrolidone.
【０００５】[0005]
【課題を解決するための手段】本発明者等は、上記の問
題点を解決すべく鋭意検討した結果、Ｎ−メチル−２−
ピロリドンに金属銅を接触させることにより、Ｎ−メチ
ル−２−ピロリドンの過酸化物の生成が充分に抑制でき
ることを見い出し、本発明を完成するに至った。即ち、
本発明の要旨は、Ｎ−メチル−２−ピロリドンを大気中
で取り扱う際に、Ｎ−メチル−２−ピロリドンに金属銅
を接触させることを特徴とするＮ−メチル−２−ピロリ
ドンの保存方法、に存する。以下本発明について詳細に
説明する。The present inventors have conducted intensive studies to solve the above-mentioned problems and found that N-methyl-2-
It has been found that by contacting metal copper with pyrrolidone, the production of N-methyl-2-pyrrolidone peroxide can be sufficiently suppressed, and the present invention has been completed. That is,
The gist of the present invention is a method for preserving N-methyl-2-pyrrolidone, which comprises contacting N-methyl-2-pyrrolidone with metallic copper when handling N-methyl-2-pyrrolidone in the air, Exists. Hereinafter, the present invention will be described in detail.
【０００６】本発明に用いられるＮ−メチル−２−ピロ
リドンとしては商業的に入手可能な製品であればよく、
好ましくは純度が９５％以上、特に好ましくは９８％以
上である。製品中の不純物（２−ピロリドン、水等）は
かかる範囲内であれば本発明に影響はない。The N-methyl-2-pyrrolidone used in the present invention may be any commercially available product.
Preferably, the purity is 95% or more, particularly preferably 98% or more. Impurities (2-pyrrolidone, water, etc.) in the product do not affect the present invention as long as they are within such a range.
【０００７】本発明で用いる金属銅は一般の金属加工材
料として用いられている純度（通常９９．９％以上）の
ものであればよく、不純物として微量の酸素、ビスマ
ス、鉛、ヒ素、イオウ等が含まれているものが使用され
る。また、銅以外の金属の表面を銅でメッキしたものも
使用することができる。金属銅の表面は、研磨、脱脂、
酸洗等で処理を施したものがよい。The metallic copper used in the present invention may have a purity (usually 99.9% or more) used as a general metal working material, and trace amounts of impurities such as oxygen, bismuth, lead, arsenic, sulfur, etc. Is used. Further, a material in which the surface of a metal other than copper is plated with copper can also be used. Polishing, degreasing,
What has been treated by pickling or the like is preferred.
【０００８】なお、銅以外の金属を接触させても過酸化
物の生成抑制効果が認められる場合もあるが、通常、該
金属そのものが、または、それが徐々にイオン化して液
中に溶出するという別の問題があるので適当ではない。
しかしながら金属銅については、液への溶出はほとんど
認められない。[0008] In some cases, the effect of suppressing the formation of peroxide is observed even when a metal other than copper is brought into contact, but usually the metal itself or it is gradually ionized and eluted into the liquid. It is not appropriate because there is another problem.
However, elution of metallic copper in the liquid is hardly observed.
【０００９】次に、過酸化物の生成抑制効果は、主に液
（Ｎ−メチル−２−ピロリドン）に接触する銅の表面積
が大きくなるほど顕著となり、銅と液の接触面積は、液
１００ｍｌに対して通常５ｃｍ2以上、好ましくは１０
ｃｍ2以上である。従って、通常、Ｎ−メチル−２−ピ
ロリドン１００ｇに対して銅を０．１ｇ、好ましくは１
ｇ以上にを浸漬して接触させるが、銅の形状を薄板状、
ワイヤー状、リボン状、金網状、粉末状等として液との
接触表面積をより大きくするように工夫すれば、特に銅
の添加量の制限はない。また、Ｎ−メチル−２−ピロリ
ドンの保存容器の内壁に銅を内張りして用いることもで
きる。Next, the effect of suppressing the formation of peroxide becomes more remarkable as the surface area of the copper in contact with the liquid (N-methyl-2-pyrrolidone) increases, and the contact area between the copper and the liquid is reduced to 100 ml. 5 cm 2 or more, preferably 10 cm
cm 2 or more. Therefore, usually, 0.1 g of copper, preferably 1 g, is added to 100 g of N-methyl-2-pyrrolidone.
g or more and contact them, but the shape of copper is thin,
There is no particular limitation on the amount of copper to be added as long as it is devised to have a larger contact surface area with the liquid, such as a wire, a ribbon, a wire net, or a powder. Also, copper can be used by lining the inner wall of the N-methyl-2-pyrrolidone storage container.
【００１０】[0010]
【実施例】以下、実施例により本発明を更に詳細に説明
するが本発明はその要旨を超えないかぎり以下の実施例
に制限されるものではない。 実施例 純度９９．８重量％のＮ−メチル−２−ピロリドン（水
分０．１重量％）５００ｇに対し、銅板（９ｃｍ×５．
５ｃｍ×０．０８５ｍｍ、重量３．８ｇ、表面積約１０
０ｃｍ2、純度９９．９％以上）を浸漬し、大気中２５
°Ｃで放置した。各日数経過後の、上記液中の過酸化物
量をヨウ化カリウム法で測定した。結果を表１に示す。 比較例 実施例において、銅板を浸漬しなかった以外は同様にし
て行った。結果を表１に示す。The present invention will be described in more detail with reference to the following Examples, which, however, are not intended to limit the scope of the invention. Example A copper plate (9 cm × 5.10 g) was prepared for 500 g of N-methyl-2-pyrrolidone (water content: 0.1 wt%) having a purity of 99.8 wt%.
5cm x 0.085mm, weight 3.8g, surface area about 10
0 cm 2 , purity 99.9% or more)
Left at ° C. After each day, the amount of peroxide in the above solution was measured by the potassium iodide method. Table 1 shows the results. Comparative Example The same procedure was performed as in the example except that the copper plate was not immersed. Table 1 shows the results.
【００１１】[0011]
【表１】 [Table 1]
【００１２】[0012]
【発明の効果】本発明によりＮ−メチル−２−ピロリド
ンの過酸化物の生成が抑制され、Ｎ−メチル−２−ピロ
リドンを大気中で安全に保存することができる。タン
ク、タンクローリ等による貯蔵、輸送、運搬にあたって
も、あえて気相部を窒素シールしなくとも実用上支障が
ない。According to the present invention, the production of peroxide of N-methyl-2-pyrrolidone is suppressed, and N-methyl-2-pyrrolidone can be safely stored in the atmosphere. In storage, transportation, and transportation by tanks, tank lorries, etc., there is no practical problem even if the gas phase part is not intentionally sealed with nitrogen.
フロントページの続き (56)参考文献 特開 昭61−40228（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C07D 207/00 - 207/50 C11D 7/50 ＣＡ（ＳＴＮ) ＣＡＯＬＤ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ)Continuation of the front page (56) References JP-A-61-40228 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C07D 207/00-207/50 C11D 7/50 CA ( STN) CAOLD (STN) REGISTRY (STN)
Claims (1)
で保存する際に、Ｎ−メチル−２−ピロリドンに金属銅
を接触させることを特徴とするＮ−メチル−２−ピロリ
ドンの保存方法。1. A method for preserving N-methyl-2-pyrrolidone, comprising contacting N-methyl-2-pyrrolidone with metallic copper when storing N-methyl-2-pyrrolidone in the atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3198054A JP3039019B2 (en) | 1991-08-07 | 1991-08-07 | Method for storing N-methyl-2-pyrrolidone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3198054A JP3039019B2 (en) | 1991-08-07 | 1991-08-07 | Method for storing N-methyl-2-pyrrolidone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0543542A JPH0543542A (en) | 1993-02-23 |
| JP3039019B2 true JP3039019B2 (en) | 2000-05-08 |
Family
ID=16384766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3198054A Expired - Fee Related JP3039019B2 (en) | 1991-08-07 | 1991-08-07 | Method for storing N-methyl-2-pyrrolidone |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3039019B2 (en) |
-
1991
- 1991-08-07 JP JP3198054A patent/JP3039019B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0543542A (en) | 1993-02-23 |
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