JP3239377B2 - N-methyl-2-pyrrolidone solution - Google Patents
N-methyl-2-pyrrolidone solutionInfo
- Publication number
- JP3239377B2 JP3239377B2 JP19205991A JP19205991A JP3239377B2 JP 3239377 B2 JP3239377 B2 JP 3239377B2 JP 19205991 A JP19205991 A JP 19205991A JP 19205991 A JP19205991 A JP 19205991A JP 3239377 B2 JP3239377 B2 JP 3239377B2
- Authority
- JP
- Japan
- Prior art keywords
- methyl
- pyrrolidone
- water
- weight
- solution
- 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)
- Detergent Compositions (AREA)
Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【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℃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。
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するこ
とは一般的に好ましくない。However, the present inventors have studied the stability of N-methyl-2-pyrrolidone in the air, and found that N-methyl-2-pyrrolidone peroxide is produced. In particular, it has been found that peroxides are remarkably generated when heated to 50 to 150 ° C. as a cleaning liquid for an integrated circuit sealing element, which poses a safety problem.
To solve this problem, it is conceivable to add a reducing substance such as so-called hydroquinone to N-methyl-2-pyrrolidone, but N-methyl-2-pyrrolidone used in many applications is considered.
-It is generally not preferred to add an active substance such as a reducing substance to pyrrolidone.
【０００４】[0004]
【課題を解決する手段】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
ドンに水を特定量添加することにより、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−ピロリドン及び水からなるＮ
−メチル−２−ピロリドン溶液、またはＮ−メチル−２
−ピロリドン、水及び、Ｎ−メチル−２−ピロリドンと
水との混液に可溶性の溶媒からなるＮ−メチル−２−ピ
ロリドン溶液であって、Ｎ−メチル−２−ピロリドンを
少なくとも２５重量％含有し、水をＮ−メチル−２−ピ
ロリドン１００重量部に対して１０〜３００重量部含有
することを特徴とする溶液に存する。The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, by adding a specific amount of water to N-methyl-2-pyrrolidone, N-methyl-2-pyrrolidone was added.
-It has been found that generation of peroxide of pyrrolidone can be sufficiently suppressed, and the present invention has been completed. That is, the gist of the present invention is to provide an N-methyl-2-pyrrolidone and water comprising N-methyl-2-pyrrolidone.
-Methyl-2-pyrrolidone solution, or N-methyl-2
-Pyrrolidone, water and N-methyl-2-pyrrolidone
N-methyl-2-pi, comprising a solvent soluble in a mixture with water
What is claimed is: 1. A rolidone solution comprising at least 25% by weight of N-methyl-2-pyrrolidone and 10 to 300 parts by weight of water based on 100 parts by weight of N-methyl-2-pyrrolidone. Exist.
【０００５】以下本発明について詳細に説明する。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−ピロリドン等）はかかる範囲内であれば
本発明に影響はない。Ｎ−メチル−２−ピロリドンの製
品は、通常、窒素シール下で保存されているが、開封後
は、通常、大気中でこれを取り扱う場合、例えば、加温
して洗浄液等として使用する場合、また、通常１日から
数ヶ月保存しておきたい場合等におけるＮ−メチル−２
−ピロリドンの安定性、安全性が問題となる。Hereinafter, the present invention will be described in detail. The N-methyl-2-pyrrolidone used in the present invention may be any commercially available product, and preferably has a purity of 95% or more, particularly preferably 98% or more. Impurities (such as 2-pyrrolidone) in the product do not affect the present invention as long as they are within such a range. Products of N-methyl-2-pyrrolidone are usually stored under a nitrogen seal, but after opening, they are usually handled in the atmosphere, for example, when heated and used as a cleaning solution, etc. In addition, N-methyl-2 is usually used when it is desired to store the protein for one to several months.
-Stability and safety of pyrrolidone are problematic.
【０００６】そこで、本発明では、Ｎ−メチル−２−ピ
ロリドン１００重量部に対して水を１０〜３００重量部
の割合で添加する。水の添加量が、１０重量部に達しな
い場合は、Ｎ−メチル−２−ピロリドンの過酸化物の生
成の抑制効果が低下するので好ましくない。また、該要
件を満たす限りにおいて、Ｎ−メチル−２−ピロリドン
と水との混液に可溶性の溶媒、例えばアルコール類を添
加して取り扱い、使用してもよい。ここに、「取り扱
い、使用」とは、Ｎ−メチル−２−ピロリドンのタンク
での貯蔵方法、容器、タンクローリーなどによる輸送、
運搬方法並びに集積回路封止素子用洗浄液等への使用方
法を包含するものである。Therefore, in the present invention, water is added at a ratio of 10 to 300 parts by weight based on 100 parts by weight of N-methyl-2-pyrrolidone. If the amount of water does not reach 10 parts by weight, the effect of suppressing the production of N-methyl-2-pyrrolidone peroxide is undesirably reduced. Further, as long as the requirements are satisfied, a solvent soluble in a mixture of N-methyl-2-pyrrolidone and water, for example, alcohols, may be added for handling and use. Here, “handling and use” means a method of storing N-methyl-2-pyrrolidone in a tank, transportation by a container, a tank lorry, or the like.
It includes a transportation method and a method of using the cleaning liquid for an integrated circuit sealing element.
【０００７】本発明のＮ−メチル−２−ピロリドンと水
の混液は、特に集積回路封止素子（以下「ＩＣ封止素
子」という）用洗浄液として好適に用いられる。ＩＣ封
止素子とは、銅または銀の導体基板にＩＣ素子をセット
し、封止剤としてエポキシ樹脂を主体としたもので固定
したものである。該洗浄液は、ＩＣ封止素子のバリ取り
除去のみに限らず、封止剤のモルディングに用いられた
金型内の付着物の除去等にも使用することができる。Ｉ
Ｃ封止素子の洗浄方法は、上記ＩＣ封止素子を洗浄液と
液接触させる洗浄処理であれば特に制限はなく、例え
ば、噴霧接触、シャワー接触、浸漬接触、超音波接触等
があげられる。洗浄温度は、通常５０〜１５０℃、好ま
しくは８０〜１４０℃、洗浄時間としては、通常３０秒
〜２時間、好ましくは１〜３０分で実施される。The mixed solution of N-methyl-2-pyrrolidone and water of the present invention is suitably used particularly as a cleaning liquid for an integrated circuit sealing element (hereinafter referred to as an “IC sealing element”). The IC sealing element is one in which an IC element is set on a copper or silver conductive substrate and is fixed with a sealing agent mainly composed of epoxy resin. The cleaning liquid can be used not only for removing the deburring of the IC sealing element but also for removing the deposits in the mold used for molding the sealing agent. I
The method for cleaning the C-sealed element is not particularly limited as long as the above-mentioned IC-sealed element is brought into liquid contact with a cleaning liquid, and examples thereof include spray contact, shower contact, immersion contact, and ultrasonic contact. The washing temperature is usually 50 to 150 ° C., preferably 80 to 140 ° C., and the washing time is usually 30 seconds to 2 hours, preferably 1 to 30 minutes.
【０００８】[0008]
【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越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１ 純度９９．８重量％のＮ−メチル−２−ピロリドン（水
分０．１重量％）１００重量部に対し、水を３３重量部
添加混合し、大気中、２５℃で放置した。各日数経過後
の、上記混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。 実施例２〜６ 実施例１において水添加量又は温度を表１の条件に変え
て行なったこと以外は同様にして行った。結果を表１に
示す。 比較例１ 実施例１において、水を添加することなく表１の温度で
行なったこと以外は同様にして行った。結果を表１に示
す。EXAMPLES Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited to the following examples unless it exceeds the gist. Example 1 To 100 parts by weight of N-methyl-2-pyrrolidone (0.1% by weight of water) having a purity of 99.8% by weight, 33 parts by weight of water was added and mixed, and the mixture was allowed to stand in the air at 25 ° C. After each day, the amount of peroxide in the mixture was measured by the potassium iodide method. Table 1 shows the results. Examples 2 to 6 The same procedure as in Example 1 was carried out except that the amount of water added or the temperature was changed to the conditions shown in Table 1. Table 1 shows the results. Comparative Example 1 An experiment was performed in the same manner as in Example 1 except that the experiment was performed at the temperature shown in Table 1 without adding water. Table 1 shows the results.
【０００９】[0009]
【表１】 [Table 1]
【００１０】[0010]
【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取り扱うことができる。特にＮ
−メチル−２−ピロリドンを高温に加熱して集積回路封
止素子の洗浄液として使用する際に実用的である。ま
た、タンク、タンクローリー等による貯蔵、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 handled in the atmosphere. Especially N
-Methyl-2-pyrrolidone is practical when heated to a high temperature and used as a cleaning liquid for an integrated circuit sealing element. Further, in storage, transportation, and transportation using a tank, a tank truck, or the like, there is no practical problem without intentionally sealing the gas phase with nitrogen.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭52−27765（ＪＰ，Ａ) 特表 平５−508180（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C07D 207/267 C11D 7/50 ＣＡ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ)──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-52-27765 (JP, A) Tokuhyo Hei 5-508180 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C07D 207/267 C11D 7/50 CA (STN) REGISTRY (STN)
Claims (3)
らなるＮ−メチル−２−ピロリドン溶液、またはＮ−メ
チル−２−ピロリドン、水及び、Ｎ−メチル−２−ピロ
リドンと水との混液に可溶性の溶媒からなるＮ−メチル
−２−ピロリドン溶液であって、Ｎ−メチル−２−ピロ
リドンを少なくとも２５重量％含有し、水をＮ−メチル
−２−ピロリドン１００重量部に対して１０〜３００重
量部含有することを特徴とする溶液。1. N-methyl-2-pyrrolidone and water
N-methyl-2-pyrrolidone solution,
Tyl-2-pyrrolidone, water and N-methyl-2-pyrro
N-methyl consisting of a solvent soluble in a mixture of lidone and water
-2-pyrrolidone solution, containing at least 25% by weight of N-methyl-2-pyrrolidone and 10 to 300 parts by weight of water with respect to 100 parts by weight of N-methyl-2-pyrrolidone. Solution.
である請求項１に記載の溶液。2. The solution according to claim 1, wherein the peroxide content is 3 meq / kg or less.
２−ピロリドン溶液からなる集積回路封止素子用洗浄
液。3. N-methyl- according to claim 1 or 2.
A cleaning liquid for an integrated circuit sealing element comprising a 2-pyrrolidone solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19205991A JP3239377B2 (en) | 1991-07-31 | 1991-07-31 | N-methyl-2-pyrrolidone solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19205991A JP3239377B2 (en) | 1991-07-31 | 1991-07-31 | N-methyl-2-pyrrolidone solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0532623A JPH0532623A (en) | 1993-02-09 |
| JP3239377B2 true JP3239377B2 (en) | 2001-12-17 |
Family
ID=16284940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19205991A Expired - Fee Related JP3239377B2 (en) | 1991-07-31 | 1991-07-31 | N-methyl-2-pyrrolidone solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3239377B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5532742B2 (en) | 2009-08-20 | 2014-06-25 | 株式会社ジェイエスピー | Expandable modified resin particles, modified resin expanded particles, and modified resin expanded particle molded body |
-
1991
- 1991-07-31 JP JP19205991A patent/JP3239377B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0532623A (en) | 1993-02-09 |
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