JPS6372656A - Perfluorotripentylamine for vapor phase soldering liquid medium - Google Patents
Perfluorotripentylamine for vapor phase soldering liquid mediumInfo
- Publication number
- JPS6372656A JPS6372656A JP61215949A JP21594986A JPS6372656A JP S6372656 A JPS6372656 A JP S6372656A JP 61215949 A JP61215949 A JP 61215949A JP 21594986 A JP21594986 A JP 21594986A JP S6372656 A JPS6372656 A JP S6372656A
- Authority
- JP
- Japan
- Prior art keywords
- vapor phase
- perfluorotripentylamine
- liquid medium
- phase soldering
- solder
- 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.)
- Granted
Links
- 238000005476 soldering Methods 0.000 title claims abstract description 21
- 239000012808 vapor phase Substances 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 title claims abstract description 14
- AQZYBQIAUSKCCS-UHFFFAOYSA-N perfluorotripentylamine Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)N(C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AQZYBQIAUSKCCS-UHFFFAOYSA-N 0.000 title claims description 23
- -1 perfluoro-2-methylbutyl group Chemical group 0.000 claims abstract description 22
- 125000005008 perfluoropentyl group Chemical group FC(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)* 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- DAFIBNSJXIGBQB-UHFFFAOYSA-N perfluoroisobutene Chemical group FC(F)=C(C(F)(F)F)C(F)(F)F DAFIBNSJXIGBQB-UHFFFAOYSA-N 0.000 abstract description 11
- 229910000679 solder Inorganic materials 0.000 abstract description 10
- 230000008018 melting Effects 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 5
- OOHAUGDGCWURIT-UHFFFAOYSA-N n,n-dipentylpentan-1-amine Chemical compound CCCCCN(CCCCC)CCCCC OOHAUGDGCWURIT-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 231100000086 high toxicity Toxicity 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 125000004493 2-methylbut-1-yl group Chemical group CC(C*)CC 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、気相でハンダを溶融することによりハンダ付
けを行なう気相ハンダ付け方法の液媒体として好適に用
い得るパーフルオロトリペンチルアミンに関する。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to perfluorotripentylamine which can be suitably used as a liquid medium in a vapor phase soldering method in which soldering is performed by melting solder in a vapor phase. .
気相ハンダ付けは、ハンダの溶融温度よりも高い沸点を
もつ化学的に不活性な液体を加熱してその飽和蒸気浴を
形成し、ハンダ付けすべき部品の上に予め接合材料を載
せてそれらをその蒸気浴中に挿入し、気化潜熱を利用し
てハンダを溶融し、ハンダ付けする方法である。Vapor phase soldering involves heating a chemically inert liquid with a boiling point higher than the melting temperature of the solder to form a saturated vapor bath, and then placing the joining material on the parts to be soldered beforehand. In this method, the solder is inserted into the steam bath and the latent heat of vaporization is used to melt the solder and perform soldering.
しかし、この技術に於ける問題の１つは蒸気浴を形成さ
せるために用いる液媒体の選定に関する問題である。液
媒体としては次のような性質を具備する必要がある。However, one of the problems with this technique concerns the selection of the liquid medium used to form the steam bath. The liquid medium must have the following properties.
ａ、適当な沸点（ハンダを溶解する沸点）であること
ｂ、各種材料に対し不活性であること
Ｃ１取扱いが安全で、毒性、腐食性物質を発生しないこ
と
ｄ、難燃性であること
８９重い層を形成できる高い気体密度をもつことｆ、蒸
発後、残留物を残さないこと
パーフルオロトリペンチルアミンは、気相ハンダ付けの
液媒体として現在量もよく使用されている。しかし、市
販のパーフルオロトリペンチルアミンである［フロリナ
ートＦＣ−７０Ｊ （商品名：スリーエム社製）は、
気相ハンダ付けの際にパーフルオロイソブチレン（以下
、ＰＦＩＢと略称する。）及びフッ化水素のような酸性
物質が極く少量ではあるが生成するという問題がある。a. It must have an appropriate boiling point (boiling point to melt solder) b. It must be inert to various materials C1 It must be safe to handle and do not generate toxic or corrosive substances d. It must be flame retardant 89 Perfluorotripentylamine is often used in current quantities as a liquid medium in vapor phase soldering because it has a high gas density that allows it to form heavy layers and leaves no residue after evaporation. However, commercially available perfluorotripentylamine [Florinat FC-70J (trade name: manufactured by 3M)]
There is a problem in that acidic substances such as perfluoroisobutylene (hereinafter abbreviated as PFIB) and hydrogen fluoride are generated during vapor phase soldering, although in very small amounts.
ＰＦＩＢは高い毒性をもつ物質である。従って、パーフ
ルオロトリペンチルアミンを気相ハンダ付けの液媒体と
する場合、生成するＰＦＩＢの濃度を下げる方法が望ま
れていた。PFIB is a highly toxic substance. Therefore, when perfluorotripentylamine is used as a liquid medium for vapor phase soldering, a method has been desired to reduce the concentration of PFIB produced.
本発明者らは、上記の問題点を克服するために鋭意研究
を重ねた結果、パーフルオロトリペンチルアミンは、種
々の異性体を含んでおり、この異性体の有するパーフル
オロイソペンチル基及びパーフルオロ−２−メチルブチ
ル基がＰＦＩＢの生成量に大きな影響を与えることを見
い出し、本発明を完成させるに至った。As a result of extensive research to overcome the above problems, the present inventors found that perfluorotripentylamine contains various isomers, and that these isomers have a perfluoroisopentyl group and a perfluoroisopentyl group. It was discovered that the fluoro-2-methylbutyl group has a large effect on the amount of PFIB produced, and the present invention was completed.
即ち、本発明は、種々の異性体の混合物からなるパーフ
ルオロトリペンチルアミンに於いて、該パーフルオロト
リペンチルアミンが有する全パーフルオロペンチル基の
うち、パーフルオロイソペンチル基及びパーフルオロ−
２−メチルブチル基の占める割合が１０％以下であるこ
とを特徴とする気相ハンダ付け液媒体用パーフルオロト
リペンチルアミンである。That is, the present invention provides a perfluorotripentylamine consisting of a mixture of various isomers, in which perfluoroisopentyl groups and perfluoro-
This is perfluorotripentylamine for vapor phase soldering liquid medium, characterized in that the proportion of 2-methylbutyl groups is 10% or less.
パーフルオロトリペンチルアミンは種々の方法で製造し
得るが、最も経済的に製造する方法として電解フッ素化
がある。即ち、トリペンチルアミンを原料として無水フ
ン化水素中で電解することにより、目的のパーフルオロ
トリペンチルアミンを合成することができる。このよう
にして得られるパーフルオロトリペンチルアミンは、パ
ーフルオロトリ （ｎ−ペンチル）アミンと共に種々の
異性体を含む。Perfluorotripentylamine can be produced by various methods, but the most economical method is electrolytic fluorination. That is, by electrolyzing tripentylamine in anhydrous hydrogen fluoride using tripentylamine as a raw material, the desired perfluorotripentylamine can be synthesized. The perfluorotripentylamine thus obtained includes various isomers as well as perfluorotri(n-pentyl)amine.
例えば、
パーフルオロトリ （ｎ−ペンチル）アミンＣＦｚＣｈ
ＣＦｚＣＦｚＣｈ
パーフルオロジ（ｎ−ペンチル）−イソペンチルアミン
パーフルオロジ（イソペンチル）−ｎ−ペンチルアミン
ＣＦ ２ＣＦ ＩＣＦ ２ＣＦ ｔｃＦ ３しト３
パーフルオロジ（ｎ−ペンチル）−２−メチルブチルア
ミン
パーフルオロ−ｎ−ペンチル−イソペンチル−２−メチ
ルブチルアミン
等の異性体を挙げることができる。For example, perfluorotri(n-pentyl)amine CFzCh
CFzCFzCh Perfluorodi(n-pentyl)-isopentylamine Perfluorodi(isopentyl)-n-pentylamine CF 2CF ICF 2CF tcF 3 Shito3 Perfluorodi(n-pentyl)-2-methylbutylamine perfluoro-n-pentyl-isopentyl -2-Methylbutylamine and other isomers can be mentioned.
これらの異性体が有する種々のパーフルオロペンチル基
の中でも、パーフルオロイソペンチル基及びパーフルオ
ロ−２−メチルブチル基の全パーフルオロペンチル基中
に占める割合（基の個数の割合、以下同じ）が低いほど
、気相ハンダ付け工程によって生成するＰＦＩＢの量は
少ないことを本発明者らは見い出した．しかも、パーフ
ルオロイソペンチル基及びパーフルオロ−２−メチルブ
チル基の全パーフルオロペンチル基に占める割合が１０
％以下とすることによりＰＦＩＢの生成は急激に減少す
ることをも見い出した。従って、本発明に於いて用いる
パーフルオロトリペンチルアミンは、全パーフルオロペ
ンチル基のうち、パーフルオロイソペンチル基及びパー
フルオロ−２−メチルブチル基の占める割合が１０％以
下のものである。特に本発明に於いて好ましくは、上記
の割合が８％以下である。尚、前記した市販のパーフル
オロトリペンチルアミンは、上記の割合が１８％である
。Among the various perfluoropentyl groups that these isomers have, the proportion of perfluoroisopentyl groups and perfluoro-2-methylbutyl groups in the total perfluoropentyl groups (ratio of the number of groups, the same applies hereinafter) is low. The inventors have found that the amount of PFIB produced by the vapor phase soldering process is smaller. Moreover, the ratio of perfluoroisopentyl groups and perfluoro-2-methylbutyl groups to the total perfluoropentyl groups is 10.
% or less, the generation of PFIB was found to be rapidly reduced. Therefore, the perfluorotripentylamine used in the present invention is one in which perfluorisopentyl groups and perfluoro-2-methylbutyl groups account for 10% or less of all perfluoropentyl groups. Particularly in the present invention, the above ratio is preferably 8% or less. Incidentally, the above-mentioned commercially available perfluorotripentylamine has the above ratio of 18%.
本発明に於けるパーフルオロイソペンチル基、パーフル
オロ−２−メチルブチル基の全パーフルオロペンチル基
に占める割合は、１９ｐ−核磁気共鳴吸収スペクトル（
ＣＦ（Ｊ、５準）による測定で求めた。The proportion of perfluoroisopentyl groups and perfluoro-2-methylbutyl groups in the total perfluoropentyl groups in the present invention is determined by the 19p-nuclear magnetic resonance absorption spectrum (
It was determined by measurement using CF (J, 5 standard).
パーフルオロトリペンチル基のフッ素原子のケミカルシ
フトは、例えば次のとおりである。The chemical shift of the fluorine atom of the perfluorotripentyl group is, for example, as follows.
ε
Ｆ ＝８１．８ｐｐｍ
δ′
Ｆ ＝８１．８ｐｐｍ
Ｆ ＝７０ｐｐｍ Ｆ ＝８１．
８ｐｐｍそこでそれぞれの基のうちで構造的特性を示す
フッ素原子のケミカルシフトにより各基を代表させるこ
と力くできる。即ち、（１）の７−クーフルオロｎ
ｇンチル基はＦ 、（ＩＩ）のパーフルオロイ２−メ
チルブチル基はＦ のケミカルシフトによりその基の
存在を確認することができる。従って、それらの積分強
度を知ることによりその基の存在量を計算することがで
きる。ε F =81.8ppm δ′ F =81.8ppm F =70ppm F =81.
8 ppm Therefore, it is possible to represent each group by the chemical shift of the fluorine atom which exhibits structural characteristics in each group. That is, 7-coufluoro n of (1)
The presence of the gnthyl group can be confirmed by the chemical shift of F, and the perfluoro2-methylbutyl group of (II) can be confirmed by the chemical shift of F. Therefore, by knowing their integrated intensities, the abundance of that group can be calculated.
本発明で使用するハンダは、２００℃以下の融点を有す
るものであることが好ましい。通常は、スズ耐鉛が６０
対４０であるハンダが最も好適に使用される。The solder used in the present invention preferably has a melting point of 200° C. or lower. Usually the tin lead resistance is 60
Solder that is 40% is most preferably used.
気相ハンダ付けの装置及び操作方法は、公知の装置及び
操作方法が何ら制限なく採用される。As the vapor phase soldering apparatus and operating method, any known apparatus and operating method may be employed without any restriction.
（効果）
本発明によれば、パーフルオロトリペンチルアミンを液
媒体として使用する気相ハンダ付けに於いても、毒性の
強いパーフルオロイソブチレンの生成を極めてわずかに
抑制することができる。従って、気相ハンダ付けを極め
て安全に行なうことができ、本発明の人体に対する安全
性への貢献度は極めて大きいものである。(Effects) According to the present invention, even in gas phase soldering using perfluorotripentylamine as a liquid medium, the production of highly toxic perfluoroisobutylene can be suppressed to a very small extent. Therefore, vapor phase soldering can be performed extremely safely, and the contribution of the present invention to human body safety is extremely large.
実施例
トリペンチルアミンを電解フッ素化して、異性体組成の
異なるパーフルオロトリペンチルアミンを製造した。そ
の組成を第１表に示した。こうして得た異性体組成のパ
ーフルオロトリペンチルアミンを蒸留精製して、気相ハ
ンダ付装置に入れ、ハンダ付部品を挿入した。気相ハン
ダ付装置としては、電熱器上３ ｃｒｙの位置までパー
フルオロトリペンチルアミンで満たし、液面から１０ｃ
ｍ上に銅製冷却コイルを設け、さらにその上５０ｃｍの
所に別の冷却コイルを設けたものを用いた。Example Tripentylamine was electrolytically fluorinated to produce perfluorotripentylamine having different isomer compositions. Its composition is shown in Table 1. The thus obtained perfluorotripentylamine having an isomeric composition was purified by distillation and placed in a vapor phase soldering apparatus, into which soldered parts were inserted. As a vapor phase soldering device, fill with perfluorotripentylamine up to 3 cry above the electric heater, and 10 cry from the liquid level.
A copper cooling coil was provided above m, and another cooling coil was provided 50 cm above it.
パーフルオロイブブチレンの分析は次のようにして行な
った。Analysis of perfluorobutylene was conducted as follows.
沸とうしたパーフルオロトリペンチルアミン液面の上方
５ ｃｍの位置におけるガスをサンプラーで吸入してサ
ンプリング溜めに導入し、ガスクロマトグラフにて定量
を行なった。分析カラムは５ｍＸ３ｍのステンレスカラ
ムに珪藻土にポリエチレングリコールを担持させたもの
を充填して用いた。The gas at a position 5 cm above the boiling perfluorotripentylamine liquid level was sucked in with a sampler, introduced into a sampling reservoir, and quantitatively determined using a gas chromatograph. The analytical column used was a 5 m x 3 m stainless steel column packed with diatomaceous earth supporting polyethylene glycol.
気相ハンダ付けは良好に行なうことができた。Vapor phase soldering was successful.
また、パーフルオロイソブチレンの生成量は第１表に示
すとおりであった。Further, the amount of perfluoroisobutylene produced was as shown in Table 1.
第１図は、パーフルオロイソペンチル基及びパーフルオ
ロ−２−メチルブチル基が全パーフルオロペンチル基に
占める割合と、パーフルオロイソブチレンの生成量との
関係を示すグラフである。FIG. 1 is a graph showing the relationship between the ratio of perfluoroisopentyl groups and perfluoro-2-methylbutyl groups to the total perfluoropentyl groups and the amount of perfluoroisobutylene produced.
Claims (1)
ペンチルアミンに於いて、該パーフルオロトリペンチル
アミンが有する全パーフルオロペンチル基のうち、パー
フルオロイソペンチル基及びパーフルオロ−２−メチル
ブチル基の占める割合が１０％以下であることを特徴と
する気相ハンダ付け液媒体用パーフルオロトリペンチル
アミン。(1) In perfluorotripentylamine consisting of a mixture of various isomers, out of all the perfluoropentyl groups possessed by the perfluorotripentylamine, perfluoroisopentyl groups and perfluoro-2-methylbutyl groups are Perfluorotripentylamine for vapor phase soldering liquid medium, characterized in that the proportion thereof is 10% or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61215949A JPH0757419B2 (en) | 1986-09-16 | 1986-09-16 | Vapor-phase soldering liquid medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61215949A JPH0757419B2 (en) | 1986-09-16 | 1986-09-16 | Vapor-phase soldering liquid medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6372656A true JPS6372656A (en) | 1988-04-02 |
| JPH0757419B2 JPH0757419B2 (en) | 1995-06-21 |
Family
ID=16680922
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61215949A Expired - Fee Related JPH0757419B2 (en) | 1986-09-16 | 1986-09-16 | Vapor-phase soldering liquid medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0757419B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6389690A (en) * | 1986-10-03 | 1988-04-20 | Tokuyama Soda Co Ltd | Production of perfluorotripentylamine |
-
1986
- 1986-09-16 JP JP61215949A patent/JPH0757419B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6389690A (en) * | 1986-10-03 | 1988-04-20 | Tokuyama Soda Co Ltd | Production of perfluorotripentylamine |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0757419B2 (en) | 1995-06-21 |
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