JP3582168B2 - Azeotropic cleaning composition - Google Patents

Description

【００４４】
表１の結果より、本発明の組成物は、蒸発中に大きな組成変化を起こさず、共沸様の性質を有していることが明らかになった。
【００４５】
実施例３〜実施例８、比較例１〜比較例１４
試験１（マシン油の除去試験）
予め一定量のマシン油を注入したＳＵＳパイプ（１ｍｍφ×６０ｍｍＬ）を、試験溶剤５００ｍｌを入れ、２５℃に保持したビーカー中に、水平にして浸漬した。
【００４６】
４０分後にＳＵＳパイプを引き上げ、ＳＵＳパイプ中のマシン油の除去率を測定し、下記の評価基準で脱脂力評価を行なった。
【００４７】
（評価基準）
マシン油の除去率を以下のごとく表示する。
【００４８】
○：９０％以上
◇：７０〜８９％
△：５０〜６９％
×：５０％以下
試験１の結果を表２に示す。
【００４９】
【表２】

【００５０】
試験２（フラックスの除去試験）
フラックス溶液にプリント基板を浸漬後、取り出し、３０分間風乾し、２３０℃で２分間リフローした。
【００５１】
室温に冷却したプリント基板を、４０℃に保持した超音波洗浄機で、６分間洗浄した。
【００５２】
洗浄後のプリント基板を、８０℃で１０分間乾燥し、純水中に残存フラックスを抽出後、導電率計で、イオン性残渣を測定した。
【００５３】
これらの結果を表２にあわせて示す。
【００５４】
（評価基準）
イオン性残渣を以下のごとく表示する。
【００５５】
○：１０μｇ／ｉｎ^２ ａｓ ＮａＣｌ 以下
△：１０〜１４μｇ／ｉｎ^２ ａｓ ＮａＣｌ
×：１４μｇ／ｉｎ^２ ａｓ ＮａＣｌ 以上
表２から明らかなように、本発明の共沸様洗浄剤組成物は、マシン油、フラックス、いずれの汚れに対しても、十分な洗浄効果が得られ、また、繰り返し蒸留再生を行っても、特性を維持できることが明らかになった。
【００５６】
【発明の効果】
本発明の共沸様洗浄剤組成物は、機器等の加工部品に付着する機械油やプリント基板等に付着するフラックス等のいずれの汚れに対しても、十分な除去能力を持ち、且つ繰り返し蒸留回収使用が可能であり、オゾン層破壊といった環境汚染の心配もないため、従来から使用されてきた塩素系及びフロン系溶剤の代替洗浄剤として極めて有効である。
【図面の簡単な説明】
【図１】実施例１より得られたノルマルデカンと３−メトキシ−３−メチル−１−ブタノールとの混合組成物の気液平衡曲線である。[0001]
[Industrial applications]
The present invention relates to a non-aqueous azeotropic detergent composition comprising normal decane and 3-methoxy-3-methyl-1-butanol.
[0002]
More specifically, it has excellent detergency against machine oils, greases, fluxes, waxes, and other oils adhering to processed parts such as automobiles, electric appliances, electronics, machinery, precision equipment, etc., and requires no rinsing and is repeatedly distilled and collected. The present invention relates to an azeotropic detergent composition that can be used under conditions and can substitute for detergents such as 1,1,1-trichloroethane and Freon 113.
[0003]
[Prior art]
Degreasing detergents used in various industrial fields are roughly classified into non-aqueous detergents and aqueous detergents. Non-aqueous detergents conventionally used include 1,1,1-trichloroethane, Freon 113, trichloroethylene and the like. , Tetrachloroethylene, halogen solvents such as methylene chloride, petroleum solvents such as gasoline and kerosene, alcohol solvents such as methyl alcohol and isopropyl alcohol, etc. Examples of aqueous detergents include various acids, alkalis and surfactants Etc. are blended.
[0004]
These cleaning agents are used in various fields, especially in a wide variety of cleaning fields, processed parts with a large amount of mineral oils and fats, precision parts, metal parts that are prone to stains and rust, and cleaning. As for degreasing cleaning of small parts handled by putting a large number of parts in a basket, halogens such as 1,1,1-trichloroethane, non-aqueous, high-defining power, non-flammable, etc. System solvents have been mainly used.
[0005]
However, in recent years, 1,1,1-trichloroethane and chlorofluorocarbon 113, which have been used in large quantities as excellent degreasing agents due to global environmental problems, have been regulated as substances that destroy the stratospheric ozone layer. They must be completely eliminated by the end of the year, and the switch to alternative detergents is urgent.
[0006]
Other halogenated solvents such as trichlorethylene and perchlorethylene also have serious environmental problems such as toxicity problems and groundwater pollution, and their future is concerned.
[0007]
Thus, as alternative cleaning agent candidates, in addition to petroleum solvents, alcohol solvents, and aqueous cleaning agents that have been used in some fields, HCFC-141b, HCFC-225 and other hydrochlorofluorocarbons, terpenes, Various solvents such as glycol ethers and N-methylpyrrolidone have been studied.
[0008]
However, these alternative cleaning agent candidates all have major drawbacks, and none of them satisfy all the required items such as detergency, safety, and economy.
[0009]
That is, hydrochlorofluorocarbons such as HCFC-225 can be treated as a non-aqueous nonflammable solvent, but they are additionally specified as ozone depleting substances and cannot be used as a substitute in the future.
[0010]
In addition, other non-aqueous solvents such as petroleum solvents and alcohol solvents have a danger of ignition, and further include any problem factors such as degreasing power, stability, toxicity and odor.
[0011]
Further, although the water-based cleaning agent has the advantage of not being flammable, it has a weak degreasing power, and is liable to cause stains and corrosion problems on metal parts. There are many problems, such as the need for
[0012]
As described above, each of the alternative cleaning agent candidates has various problems, but there is no possibility that a desirable alternative product will be developed in the near future, and there is a situation that it is necessary to immediately switch to any of the alternative cleaning agent candidates. .
[0013]
In addition, the cleaning process is extremely important because it affects the quality and life of the final product of the object to be cleaned, and 1,1,1-trichloroethane is often used for cleaning metal parts in small and medium-sized enterprises. Water-based cleaning agents that involve a large amount of capital investment, including expansion of the cleaning process and wastewater treatment equipment, are often avoided.
[0014]
Therefore, attention has been paid to non-aqueous cleaning agents that are naturally non-corrosive, and relatively safe hydrocarbon solvents that do not deplete the ozone layer, have high degreasing power, have low toxicity, and are not flammable at room temperature are being reviewed.
[0015]
However, these hydrocarbon solvents are required to minimize the liquid volume of the washing tank as much as possible due to restrictions on the specified quantity of hazardous materials and safety issues, and therefore, a sufficient amount of A large liquid volume cannot be obtained, frequent liquid exchange is required, and in consideration of work efficiency and economy, distillation and recovery are indispensable in order to forcibly remove oil mixed in the cleaning liquid.
[0016]
However, the conventional hydrocarbon-based detergents are mainly composed of petroleum fractions or compositions in which various substances are blended with these components. It was found that the properties of the object could not be maintained, causing poor cleaning of the object to be cleaned and a problem of corrosion.
[0017]
Therefore, the present inventors have proposed a detergent composition using normal decane, normal undecane and the like in JP-A-6-220494 to solve the above-mentioned problems. However, it was found that the effect of removing flux was not sufficient.
[0018]
Further, various glycol ether compounds proposed as detergents such as fluxes are mixed with water or a surfactant, and are used as aqueous or semi-aqueous detergents. Also has the problem that it cannot be recovered by distillation.
[0019]
As described above, non-aqueous materials that satisfy the detergency of all dirt such as machine oil, flux, wax, grease, etc., do not require rinsing, and can satisfy the overall required performance such as repeated distillation and recovery. At present, cleaning agents have not been developed yet.
[0020]
[Problems to be solved by the invention]
The present invention has been made in view of the above problems, and an object of the present invention is to provide an excellent detergency for machine oil, flux, wax, and the like adhering to a machined part such as equipment, without the need for a rinse agent, and for cleaning. An object of the present invention is to provide a non-aqueous azeotropic cleaning composition which has good drying properties, can be repeatedly recovered by distillation, and has no problem of destruction of the ozone layer.
[0021]
[Means for Solving the Problems]
In view of such circumstances, the present inventors have conducted various studies in order to solve the above-mentioned problems, and as a result, have found a desired azeotropic detergent composition, and have completed the present invention.
[0022]
That is, the present invention is a two-component azeotropic cleaning composition comprising 50 to 90% by weight of normal decane and 10 to 50% by weight of 3-methoxy-3-methyl-1-butanol.
[0023]
In the present invention, the azeotropic detergent composition is a detergent having a high removal ability against machine oil, flux, and the like, and is composed of normal decane and 3-methoxy-3-methyl-1-butanol. It is a component-based composition having a boiling point lower than each of these two components, and its composition and properties hardly change even when washing and distillation operations are repeated.
[0024]
The composition ratio of the azeotropic cleaning composition of the present invention is such that normal decane is 50 to 90% by weight, 3-methoxy-3-methyl-1-butanol is 10 to 50% by weight, More preferably, the composition ratio of the azeotrope-like cleaning composition as a stain remover is 70 to 85% by weight of normal decane and 15 to 30% by weight of 3-methoxy-3-methyl-1-butanol.
[0025]
The azeotrope-like composition of the present invention has a high degreasing power with respect to machine oil, flux and the like, and maintains the characteristics of the present composition because there is little change in components even when a distillation operation is performed in the washing step. be able to.
[0026]
Furthermore, since the azeotropic composition of the present invention has a boiling point lower than the boiling points of normal decane and 3-methoxy-3-methyl-1-butanol, the azeotropic composition has excellent properties such as an increased volatilization rate. ing.
[0027]
In the present invention, the azeotropic composition of the two components exhibits an excellent effect. Normal decane alone has an excellent ability to remove machine oil, but an insufficient ability to remove flux. .
[0028]
On the other hand, 3-methoxy-3-methyl-1-butanol alone has a large surface tension and a high viscosity, and has insufficient removal ability with respect to any of machine oil, flux and the like.
[0029]
When the mixing ratio of these two components is 50% by weight or less for normal decane and 50% by weight or more for 3-methoxy-3-methyl-1-butanol, the effect of the present invention cannot be obtained.
[0030]
Even if other saturated aliphatic hydrocarbons such as undecane, dodecane and isodecane are used in place of normal decane used in the present invention, a good cleaning effect cannot be maintained.
[0031]
Further, instead of 3-methoxy-3-methyl-1-butanol used in the present invention, other glycol ether compounds, for example, ethylene glycol, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol monoethyl ether, Similarly, even if dipropylene glycol ether is used, a good cleaning effect cannot be obtained.
[0032]
That is, the present invention provides a remarkable effect for the first time by using 50 to 90% by weight of normal decane and 10 to 50% by weight of 3-methoxy-3-methyl-1-butanol in combination. A non-aqueous azeotropic detergent composition is obtained.
[0033]
The azeotropic detergent composition of the present invention includes other hydrocarbons, esters, alcohols, ethers, phenols, surfactants, rust preventives, etc. within a range that does not impair the performance of the present composition. Can also be blended.
[0034]
The method for cleaning metals, electrons, precision parts, and the like using the azeotropic cleaning composition of the present invention is not particularly limited. For example, immersion cleaning, ultrasonic cleaning, warming cleaning, shower cleaning method, and the like. After that, it is effective to carry out hot air or vacuum drying, and to use the washing liquid while collecting it intermittently or continuously by distillation.
[0035]
【Example】
Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited thereto.
[0036]
Example 1
In a 300 ml flask equipped with a reflux condenser, 100 g of a previously prepared mixed solution of normal decane and 3-methoxy-3-methyl-1-butanol was put, and the mixture was boiled in an oil bath.
[0037]
When the temperature became constant after 30 minutes, the compositions of the liquid phase and the gas phase in the flask were analyzed by gas chromatography, and the temperatures of the gas phase and the liquid layer at that time were measured.
[0038]
FIG. 1 shows a gas-liquid equilibrium curve of the mixed composition obtained from the test results.
[0039]
As is clear from FIG. 1, the mixture of normal decane and 3-methoxy-3-methyl-1-butanol contained 50 to 90% by weight of normal decane and 10 to 90% by weight of 3-methoxy-3-methyl-1-butanol. In the range of 50% by weight, the composition of the gas phase and the liquid phase becomes almost the same, which is clearly an azeotropic composition. The boiling point was extremely low (about 164 ° C.) in the range of 54 to 58% by weight of normal decane and 42 to 46% by weight of 3-methoxy-3-methyl-1-butanol.
[0040]
Further, as is apparent from FIG. 1, when the amount of normal decane is less than 50% by weight and the amount of 3-methoxy-3-methyl-1-butanol is more than 50% by weight, the difference between the gas and liquid phases becomes large.
[0041]
Example 2
200 g of a mixture of 56.0% by weight of normal decane and 44.0% by weight of 3-methoxy-3-methyl-1-butanol was placed in a distillation flask and distilled with a distillation apparatus having 20 theoretical plates.
[0042]
An aliquot was collected while measuring the vapor temperature, and analyzed by gas chromatography. Table 1 shows the results.
[0043]
[Table 1]

[0044]
From the results in Table 1, it was clarified that the composition of the present invention did not cause a large change in composition during evaporation and had azeotropic properties.
[0045]
Examples 3 to 8, Comparative Examples 1 to 14
Test 1 (machine oil removal test)
A SUS pipe (1 mmφ × 60 mmL) into which a predetermined amount of machine oil had been injected in advance was horizontally immersed in a beaker kept at 25 ° C., containing 500 ml of a test solvent.
[0046]
After 40 minutes, the SUS pipe was pulled up, the removal rate of machine oil in the SUS pipe was measured, and the degreasing power was evaluated according to the following evaluation criteria.
[0047]
(Evaluation criteria)
The removal rate of the machine oil is displayed as follows.
[0048]
：: 90% or more ◇: 70 to 89%
Δ: 50 to 69%
X: 50% or less The results of Test 1 are shown in Table 2.
[0049]
[Table 2]

[0050]
Test 2 (flux removal test)
The printed circuit board was immersed in the flux solution, taken out, air-dried for 30 minutes, and reflowed at 230 ° C. for 2 minutes.
[0051]
The printed circuit board cooled to room temperature was washed with an ultrasonic cleaner kept at 40 ° C. for 6 minutes.
[0052]
The washed printed circuit board was dried at 80 ° C. for 10 minutes, and after extracting residual flux in pure water, ionic residues were measured with a conductivity meter.
[0053]
The results are shown in Table 2.
[0054]
(Evaluation criteria)
The ionic residue is indicated as follows.
[0055]
：: 10 μg / in ² as NaCl or less Δ: 10 to 14 μg / in ² as NaCl
×: 14 μg / in ² as NaCl As is clear from Table 2, the azeotropic cleaning composition of the present invention can provide a sufficient cleaning effect on machine oil, flux, and any stain. It was also found that the characteristics could be maintained even after repeated distillation regeneration.
[0056]
【The invention's effect】
The azeotropic cleaning composition of the present invention has a sufficient removing ability for any dirt such as machine oil adhering to machined parts such as equipment and flux adhering to printed circuit boards and the like, and is repeatedly distilled. Since it can be recovered and used and there is no concern about environmental pollution such as destruction of the ozone layer, it is extremely effective as an alternative to the conventionally used chlorine-based and chlorofluorocarbon-based solvents.
[Brief description of the drawings]
FIG. 1 is a vapor-liquid equilibrium curve of a mixed composition of normal decane and 3-methoxy-3-methyl-1-butanol obtained from Example 1.

Claims (1)

A two-component azeotropic detergent composition comprising 50 to 90% by weight of normal decane and 10 to 50% by weight of 3-methoxy-3-methyl-1-butanol.

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