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CN100441673C - Solvent Composition for Washing - Google Patents

Solvent Composition for Washing Download PDF

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Publication number
CN100441673C
CN100441673C CNB2005101186935A CN200510118693A CN100441673C CN 100441673 C CN100441673 C CN 100441673C CN B2005101186935 A CNB2005101186935 A CN B2005101186935A CN 200510118693 A CN200510118693 A CN 200510118693A CN 100441673 C CN100441673 C CN 100441673C
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propylene glycol
pentafluorobutane
washing
weight
365mfc
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CN1769413A (en
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金子旻又
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Kaneko Chemical Co Ltd
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Kaneko Chemical Co Ltd
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  • Detergent Compositions (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

The invention provides a solvent composition for washing, wherein a propylene glycol solvent is mixed with 1, 1, 1, 3, 3-pentafluorobutane on the premise of not generating flammability.

Description

洗涤用溶剂组合物 Solvent Composition for Washing

本申请为申请号02802396.X、申请日2002年2月14日、发明名称“洗涤用溶剂组合物”的分案申请。This application is a divisional application with the application number 02802396.X, the filing date of February 14, 2002, and the title of the invention "solvent composition for cleaning".

技术领域 technical field

本发明涉及以1,1,1,3,3-五氟丁烷为主要成分的洗涤用溶剂组合物,特别涉及提高其洗涤能力的技术。The present invention relates to a cleaning solvent composition mainly composed of 1,1,1,3,3-pentafluorobutane, and particularly relates to a technique for improving its cleaning ability.

背景技术 Background technique

氯系溶剂和氟系溶剂通常作为焊剂(flux)洗涤剂、干洗用溶剂、脱脂洗涤剂、抛光研磨洗涤剂、保护层剥离剂和除去附着水用溶剂等广泛使用。但是,考虑对环境带来的问题,氯系溶剂作为污染地下水的物质,氟系溶剂作为破坏臭氧层的物质逐渐被控制使用。因此,各方面都希望开发新型的有关溶剂。Chlorine-based solvents and fluorine-based solvents are generally used widely as flux detergents, solvents for dry cleaning, degreasing detergents, polishing and polishing detergents, protective layer stripping agents, and solvents for removing adhering water. However, in consideration of environmental problems, the use of chlorine-based solvents as substances that pollute groundwater and fluorine-based solvents as substances that destroy the ozone layer has been gradually controlled. Therefore, development of novel related solvents is desired in various quarters.

其一,有1,1,1,3,3-五氟丁烷(365mfc、化学式C4H5F5)(参考特开平5-171189号、特开平5-171190号、特开平6-322394号、特开平7-188700号等)。1,1,1,3,3-五氟丁烷由于其分子结构中不含有氯,破坏臭氧层系数(ODP)为0,毒性也小,温暖化系数(GWP)小,具有对环境有利的优良特性。One, there is 1,1,1,3,3-pentafluorobutane (365mfc, chemical formula C 4 H 5 F 5 ) (refer to JP-5-171189, JP-5-171190, JP-6-322394 No., Special Kaiping No. 7-188700, etc.). 1,1,1,3,3-Pentafluorobutane does not contain chlorine in its molecular structure, its ozone depletion coefficient (ODP) is 0, its toxicity is small, its warming coefficient (GWP) is small, and it has excellent environmental benefits. characteristic.

但是1,1,1,3,3-五氟丁烷(365mfc)的问题是KB值(贝壳杉脂丁醇)大约为14,非常低,几乎没有脱脂能力。当KB低时,作为各种洗涤剂不能显示足够的洗涤能力。But the problem with 1,1,1,3,3-pentafluorobutane (365mfc) is that the KB value (kauributanol) is about 14, which is very low and has almost no degreasing ability. When KB is low, sufficient washing power cannot be exhibited as various detergents.

有方案(参考特开平5-171185号及特开平11-152236号公报)提出在1,1,1,3,3-五氟丁烷中,混合比其KB值高具有脱脂洗涤力的二氯甲烷、或1,1-二氯-1-氟乙烷(HCFC141b),以提高洗涤能力。There are plans (refer to JP 5-171185 and JP 11-152236) to propose that in 1,1,1,3,3-pentafluorobutane, a dichloride with a degreasing degreasing power higher than its KB value is mixed. methane, or 1,1-dichloro-1-fluoroethane (HCFC141b) to increase the washing capacity.

但是,由于二氯甲烷的毒性高,操作时对人体有不好的影响,不优选使用,同时,作为今后限制的对象,恐怕难以使用。1,1-二氯-1-氟乙烷(141b)由于臭氧层破坏系数高,已经成为限制的对象。However, since dichloromethane is highly toxic and has adverse effects on the human body during handling, it is not preferable to use it, and it may be difficult to use it as an object of future restrictions. 1,1-Dichloro-1-fluoroethane (141b) has been subject to regulation due to its high ozone layer destruction coefficient.

发明内容 Contents of the invention

本发明考虑如上所述的问题,其第1目的在于得到以1,1,1,3,3-五氟丁烷为主要成分的洗涤能力,特别是洗涤脱脂能力高的洗涤用溶剂组合物。The present invention considers the above-mentioned problems, and its first object is to obtain a cleaning solvent composition containing 1,1,1,3,3-pentafluorobutane as a main component with high cleaning performance, especially high cleaning and degreasing performance.

对于上述以外的本发明的目的和特征,由本说明书所述以及附图显示清楚。The objects and features of the present invention other than those described above will be apparent from the description of this specification and the accompanying drawings.

为了实现所述目的,本发明公开如下构成。In order to achieve the object, the present invention discloses the following configurations.

本发明的第1构成的特征在于,含有(a)1,1,1,3,3-五氟丁烷和(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂,没有易燃性。The first configuration of the present invention is characterized in that it contains (a) 1,1,1,3,3-pentafluorobutane and (b) selected from nitromethane, nitroethane, d-terpene and 3 - At least one solvent of methoxy butyl acetate, which is not flammable.

硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯作为提高1,1,1,3,3-五氟丁烷洗涤能力的相应溶剂是本发明人的研究成果。在这些溶剂中具有优良的脱脂洗涤能力。Nitromethane, nitroethane, d-terpene and 3-methoxy butyl acetate are the corresponding solvents for improving the washing ability of 1,1,1,3,3-pentafluorobutane are the present invention Human research results. It has excellent degreasing and washing ability in these solvents.

本发明的第2构成的特征在于,含有30~70重量%的(a)1,1,1,3,3-五氟丁烷、30~70重量%的(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂。The second configuration of the present invention is characterized in that it contains 30 to 70% by weight of (a) 1,1,1,3,3-pentafluorobutane, and 30 to 70% by weight of (b) selected from nitromethane, At least one solvent or a mixed solvent of two or more of nitroethane, d-terpene, and 3-methoxybutyl acetate.

将1,1,1,3,3-五氟丁烷设定在30~70重量%、选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂设定在30~70重量%范围,是因为当含有量过低时,不能足以提高洗涤能力,不能得到足够的洗涤效果。在含有量过高的情况下,硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯的特性充分显示,产生易燃性,成为可燃物。1,1,1,3,3-pentafluorobutane is set at 30 to 70% by weight, selected from nitromethane, nitroethane, d-terpene and 3-methoxy butyl ethyl At least one solvent or two or more mixed solvents in the acid ester is set in the range of 30 to 70% by weight because if the content is too low, the cleaning ability cannot be sufficiently improved and sufficient cleaning effect cannot be obtained. When the content is too high, the properties of nitromethane, nitroethane, d-terpene, and 3-methoxybutyl acetate are fully exhibited, flammability occurs, and they become combustibles.

本发明的第3主要构成的特征在于,含有30~60重量%的(a)1,1,1,3,3-五氟丁烷、40~70重量%的(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂。该构成足以洗涤焊剂。The third main constitution of the present invention is characterized in that it contains 30 to 60% by weight of (a) 1,1,1,3,3-pentafluorobutane, and 40 to 70% by weight of (b) selected from nitromethane , nitroethane, d-terpene and 3-methoxy butyl acetate at least one solvent or a mixed solvent of two or more. This composition is sufficient for washing flux.

本发明的第4主要构成的特征在于,含有(a)1,1,1,3,3-五氟丁烷和(c)丙二醇系溶剂,没有易燃性。The fourth main configuration of the present invention is characterized in that it contains (a) 1,1,1,3,3-pentafluorobutane and (c) a propylene glycol-based solvent, and has no flammability.

作为提高1,1,1,3,3-五氟丁烷的洗涤能力的相应溶剂,本发明人发现还有丙二醇系溶剂。丙二醇系溶剂由于具有非常强的溶解力,脱脂洗涤效果好。而且丙二醇系溶剂没有毒性、非常安全、容易操作,而且在其分子结构中不含有氯和氟,臭氧破坏系数(ODP)和温暖化系数(GWP)都小,具有不污染环境的特性。通过将这样的溶剂混合在1,1,1,3,3-五氟丁烷中,可用于大幅度提高脱脂洗涤能力,充分显示作为各种洗涤剂的性能。The present inventors have found that there is also a propylene glycol-based solvent as a corresponding solvent for improving the cleaning ability of 1,1,1,3,3-pentafluorobutane. Propylene glycol-based solvents have a very strong solvency and are effective in degreasing and washing. Moreover, the propylene glycol solvent is non-toxic, very safe, easy to handle, and does not contain chlorine and fluorine in its molecular structure. The ozone destruction coefficient (ODP) and warming coefficient (GWP) are small, and it has the characteristics of not polluting the environment. By mixing such a solvent with 1,1,1,3,3-pentafluorobutane, it can be used to greatly improve the degreasing cleaning ability, and fully demonstrate the performance as various detergents.

但是丙二醇系溶剂有易燃性,具有可燃物相应的缺点,但是因为1,1,1,3,3-五氟丁烷没有易燃性为不燃物,所以通过和这些不燃溶剂混合,可以形成没有易燃性、安全的难燃物。However, propylene glycol-based solvents are flammable and have the corresponding disadvantages of flammable substances. However, because 1,1,1,3,3-pentafluorobutane is not flammable and is non-flammable, it can be formed by mixing with these non-flammable solvents. Non-flammable, safe flame retardant.

本发明的第5主要构成的特征在于含有10~80重量%的(a)1,1,1,3,3-五氟丁烷、20~90重量%的(c)1种和2种以上的丙二醇系溶剂。The fifth main constitution of the present invention is characterized by containing 10 to 80% by weight of (a) 1,1,1,3,3-pentafluorobutane, and 20 to 90% by weight of (c) one or more types propylene glycol based solvents.

将1,1,1,3,3-五氟丁烷设定10~80重量%范围、丙二醇系溶剂设定20~90重量%范围,是因为当丙二醇系溶剂含有量过低时,不足以提高洗涤能力,不能得到足够的洗涤效果。在丙二醇系溶剂含有量过高时,担心产生易燃性,形成可燃物。通过设定如前所述的配合量,可以得到具有足够洗涤能力并且没有易燃性的洗涤用溶剂组合物。The 1,1,1,3,3-pentafluorobutane is set in the range of 10 to 80% by weight, and the propylene glycol solvent is set in the range of 20 to 90% by weight, because when the content of the propylene glycol solvent is too low, it is not enough If the washing ability is improved, a sufficient washing effect cannot be obtained. When the content of the propylene glycol-based solvent is too high, flammability may occur and combustibles may be formed. By setting the compounding quantity as mentioned above, the solvent composition for cleaning which has sufficient cleaning power and has no inflammability can be obtained.

本发明的第6主要构成的特征在于含有10~70重量%的(a)1,1,1,3,3-五氟丁烷、30~90重量%的(c)1种和2种以上的丙二醇系溶剂。这种构成可以充分洗涤焊剂。The sixth main constitution of the present invention is characterized by containing 10 to 70% by weight of (a) 1,1,1,3,3-pentafluorobutane, and 30 to 90% by weight of (c) one or more types propylene glycol based solvents. This composition can fully wash the flux.

还有,本发明的第4~6主要构成的特征在于,含有选自(d)硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇以及d-萜二烯中的至少1种溶剂。In addition, the fourth to sixth main configurations of the present invention are characterized in that they contain (d) nitromethane, nitroethane, 3-methoxybutyl acetate, 3-methoxy-1 - At least one solvent selected from butanol and d-terpene.

本发明的第4~6主要构成的特征在于,含有5重量%以上的选自(d)硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇以及d-萜二烯中的至少1种溶剂。The fourth to sixth main constitutions of the present invention are characterized in that they contain 5% by weight or more of a compound selected from (d) nitromethane, nitroethane, 3-methoxybutyl acetate, 3-methoxy - At least one solvent selected from 1-butanol and d-terpene.

如上所述通过含有硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇以及d-萜二烯,可以进一步提高溶解力,显示优异的洗涤力。As mentioned above, by containing nitromethane, nitroethane, 3-methoxy butyl acetate, 3-methoxy-1-butanol and d-terpene, the solubility can be further improved, showing Excellent detergency.

实施发明的最佳形态The best form for carrying out the invention

下面对本发明的洗涤用溶剂组合物的实施形态进行说明。本发明涉及的洗涤用溶剂组合物具有以下5个类型。Embodiments of the cleaning solvent composition of the present invention will be described below. The solvent composition for washing|cleaning which concerns on this invention has the following 5 types.

[1]洗涤用溶剂组合物,其特征在于,含有(a)1,1,1,3,3-五氟丁烷和(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂,没有易燃性。[1] A solvent composition for cleaning, characterized in that it contains (a) 1,1,1,3,3-pentafluorobutane and (b) a difluoroethylene selected from nitromethane, nitroethane, d-terpene At least one solvent among alkenes and 3-methoxy butyl acetate, no flammability.

[2]洗涤用溶剂组合物,其特征在于,含有30~70重量%的(a)1,1,1,3,3-五氟丁烷和30~70重量%的(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂。[2] A solvent composition for cleaning, characterized in that it contains 30 to 70% by weight of (a) 1,1,1,3,3-pentafluorobutane and 30 to 70% by weight of (b) selected from nitric acid At least one solvent or a mixed solvent of two or more of methyl methane, nitroethane, d-terpene, and 3-methoxy butyl acetate.

[3]洗涤用溶剂组合物,其特征在于,含有30~60重量%的(a)1,1,1,3,3-五氟丁烷和40~70重量%的(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂。[3] A solvent composition for cleaning, characterized in that it contains 30 to 60% by weight of (a) 1,1,1,3,3-pentafluorobutane and 40 to 70% by weight of (b) selected from nitric acid At least one solvent or a mixed solvent of two or more of methyl methane, nitroethane, d-terpene, and 3-methoxy butyl acetate.

[4]洗涤用溶剂组合物,其特征在于,含有(a)1,1,1,3,3-五氟丁烷和(c)丙二醇系溶剂,没有易燃性。[4] A cleaning solvent composition comprising (a) 1,1,1,3,3-pentafluorobutane and (c) a propylene glycol-based solvent, and having no inflammability.

[5]洗涤用溶剂组合物,其特征在于,含有10~80重量%的(a)1,1,1,3,3-五氟丁烷和20~90重量%的(c)1种或2种以上的丙二醇系溶剂。[5] A cleaning solvent composition characterized by containing 10 to 80% by weight of (a) 1,1,1,3,3-pentafluorobutane and 20 to 90% by weight of (c) one or more Two or more kinds of propylene glycol-based solvents.

[6]洗涤用溶剂组合物,其特征在于,含有10~70重量%的(a)1,1,1,3,3-五氟丁烷和30~90重量%的(c)1种或2种以上的丙二醇系溶剂。[6] A cleaning solvent composition comprising 10 to 70% by weight of (a) 1,1,1,3,3-pentafluorobutane and 30 to 90% by weight of (c) one or more of Two or more kinds of propylene glycol-based solvents.

[7]洗涤用溶剂组合物,其特征在于,在[4]-[6]中涉及的洗涤用溶剂组合物中,含有选自(d)硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇和d-萜二烯中的至少1种溶剂。[7] The cleaning solvent composition is characterized in that, in the cleaning solvent composition mentioned in [4]-[6], it contains At least one solvent selected from butyl butyl acetate, 3-methoxy-1-butanol and d-terpene.

在[1]-[3]、[6]、[7]中涉及的洗涤用溶剂组合物中,可以混合硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯或3-甲氧基-1-丁醇和d-萜二烯中的至少1种溶剂,当然也可以从中选出2种以上混合。In the cleaning solvent composition mentioned in [1]-[3], [6], [7], nitromethane, nitroethane, d-terpene, 3-methoxy-butane can be mixed At least one solvent selected from acetyl acetate or 3-methoxy-1-butanol and d-terpene, of course, two or more solvents selected from them may be mixed.

[7]中涉及的洗涤用溶剂组合物,硝基甲烷、硝基乙烷、d-萜二烯、以及3-甲氧基·丁基乙酸酯的混合量过少,也不能充分提高洗涤能力,所以其下限值优选设定5重量%以上。由于这些溶剂的混合量过大时,担心产生易燃性,所以优选适当混合至不产生易燃性的程度。另外由于这些溶剂与丙二醇系溶剂相比,稍贵一点,所以优选尽可能控制其使用量。The cleaning solvent composition involved in [7], the mixing amount of nitromethane, nitroethane, d-terpene, and 3-methoxy butyl acetate is too small, and the cleaning effect cannot be sufficiently improved. capacity, the lower limit thereof is preferably set at 5% by weight or more. Since there is a fear of flammability when the mixing amount of these solvents is too large, it is preferable to mix them appropriately to the extent that flammability does not occur. In addition, since these solvents are slightly more expensive than propylene glycol-based solvents, it is preferable to control the usage amount thereof as much as possible.

作为[4]-[7]中涉及的洗涤用溶剂组合物中使用的丙二醇系溶剂,具体如下:丙二醇甲基醚[PM](沸点:120℃,闪点:34℃)、二·丙二醇甲基醚[DPM](沸点:188℃,闪点:79℃)、三·丙二醇甲基醚[TPM](沸点:242℃,闪点:122℃)、丙二醇-n-丁基醚[PnB](沸点:170℃,闪点:62℃)、二·丙二醇-n-丁基醚[DPnB](沸点:229℃,闪点:106℃)、三·丙二醇-n-丁基醚(沸点:274℃,闪点:138℃)、丙二醇甲基醚乙酸酯[PMA](沸点:146℃,闪点:46.5℃)、丙二醇二乙酸酯[PGDA](沸点:190℃,闪点:93℃)、丙二醇苯基醚[PPh](沸点:243℃,闪点:121℃)以及丙二醇单乙醇醚乙酸酯(沸点:158℃,闪点:53℃)等。这些丙二醇系溶剂可以单独混合1种,也可以复合混合使用。As the propylene glycol-based solvent used in the cleaning solvent composition referred to in [4]-[7], specifically, the following: propylene glycol methyl ether [PM] (boiling point: 120°C, flash point: 34°C), dipropylene glycol methyl ether Base ether [DPM] (boiling point: 188°C, flash point: 79°C), tripropylene glycol methyl ether [TPM] (boiling point: 242°C, flash point: 122°C), propylene glycol-n-butyl ether [PnB] (boiling point: 170°C, flash point: 62°C), dipropylene glycol-n-butyl ether [DPnB] (boiling point: 229°C, flash point: 106°C), tripropylene glycol-n-butyl ether (boiling point: 274°C, flash point: 138°C), propylene glycol methyl ether acetate [PMA] (boiling point: 146°C, flash point: 46.5°C), propylene glycol diacetate [PGDA] (boiling point: 190°C, flash point: 93°C), propylene glycol phenyl ether [PPh] (boiling point: 243°C, flash point: 121°C), propylene glycol monoethyl ether acetate (boiling point: 158°C, flash point: 53°C), etc. These propylene glycol-based solvents may be mixed alone or in combination.

对于1,1,1,3,3-五氟丁烷,在加热状态和蒸汽下洗涤使用时,当被洗涤物为铁、锌、铝、铜、黄铜等时,有时因金属影响而不稳定,所以优选添加选自硝基化合物类、酚类、胺类、醚类、戊烯类、环氧化合物类、或三唑类的1种以上的化合物作为稳定剂。作为稳定剂具体如下。环氧丙烷、1,2-环氧丁烷、缩水甘油等的环氧类;二甲基磷酸盐、二异丙基磷酸盐、二苯基磷酸盐等的磷酸盐类;三硫代亚磷酸三月桂酯等硫代亚磷酸盐类;三苯氧基膦亚硫酸盐、三甲基膦亚硫酸盐等的膦亚硫酸盐类;硼酸、三乙基硼酸盐、三苯基硼酸盐、苯基硼酸、二苯基硼酸等的硼化合物;2,6-二叔丁基对位甲酚等的酚类;硝基甲烷、硝基乙烷等的硝基烷烃类;丙烯酸甲酯、丙烯酸乙酯等的丙烯酸酯类;其他的二噁烷、叔丁醇、季戊四醇、对异丙烯基甲苯。对这些稳定剂的添加量没有特别限定,但优选设定在洗涤用溶剂组合物整体量的0.01~5.00重量%范围。For 1,1,1,3,3-pentafluorobutane, when it is used for washing under heating and steam, when the object to be washed is iron, zinc, aluminum, copper, brass, etc., sometimes it will not be affected by the metal Therefore, it is preferable to add at least one compound selected from nitro compounds, phenols, amines, ethers, pentenes, epoxy compounds, or triazoles as a stabilizer. The stabilizer is specifically as follows. Epoxides such as propylene oxide, 1,2-butylene oxide, and glycidol; phosphates such as dimethyl phosphate, diisopropyl phosphate, and diphenyl phosphate; trithiophosphorous acid Thiophosphites such as trilauryl ester; phosphine sulfites such as triphenoxyphosphine sulfite and trimethylphosphine sulfite; boric acid, triethyl borate, triphenyl borate , phenylboronic acid, diphenylboronic acid and other boron compounds; phenols such as 2,6-di-tert-butyl-p-cresol; nitroalkanes such as nitromethane and nitroethane; methyl acrylate, Acrylates such as ethyl acrylate; other dioxane, tert-butanol, pentaerythritol, p-isopropenyltoluene. The addition amount of these stabilizers is not particularly limited, but is preferably in the range of 0.01 to 5.00% by weight of the entire cleaning solvent composition.

本发明涉及的洗涤用溶剂组合物的主要用途例如有:保护膜剥离剂和焊剂洗涤剂·油脂类等脱脂洗涤剂、抛光研磨洗涤剂、粘接剂(氨基甲酸乙脂或环氧、硅等)的溶解剂、干洗用溶剂、润滑脂·油·石蜡·墨水等的去除剂、塑料用溶剂、萃取剂、玻璃·陶瓷·橡胶·金属制各种物品、特别是IC部件、电器、精密机器、光学透镜等的洗涤剂和除水剂等。The main applications of the cleaning solvent composition related to the present invention are, for example, degreasing detergents such as protective film stripping agents and flux detergents, greases, polishing and grinding detergents, adhesives (urethane or epoxy, silicon, etc.) ), solvents for dry cleaning, removers for grease, oil, paraffin, ink, etc., solvents for plastics, extractants, various items made of glass, ceramics, rubber, and metal, especially IC parts, electric appliances, and precision equipment , Detergents and water removers for optical lenses, etc.

另外,作为本发明涉及的可使用洗涤用溶剂组合物的洗涤方法,主要为手擦、浸渍、喷雾、超声波洗涤、蒸汽洗涤、粘接剂(氨基甲酸乙酯或环氧、硅等)的充填装置喷嘴洗涤,可适用在其他的一般洗涤中。In addition, as the cleaning method that can use the solvent composition for cleaning according to the present invention, there are mainly hand rubbing, dipping, spraying, ultrasonic cleaning, steam cleaning, and filling of adhesives (urethane, epoxy, silicon, etc.) The device is equipped with nozzle washing, which can be applied to other general washing.

《机械油的洗涤试验1》"Machine Oil Washing Test 1"

在本试验中,准备SUS-304试验片(长25mm×宽30mm×高2mm),将该试验片浸渍在机械油(CQ-30:日本石油株式会社制)中,之后在各洗涤液中浸渍约3分钟,其后干燥处理试验片,然后考察试验片的洗涤状况。作为洗涤用溶剂,使用在1,1,1,3,3-五氟丁烷(365mfc),分别混合硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯(3-MBA)。下面表1显示洗涤液的组成和洗涤效果。In this test, a SUS-304 test piece (length 25 mm x width 30 mm x height 2 mm) was prepared, and the test piece was immersed in machine oil (CQ-30: manufactured by Nippon Oil Corporation) and then immersed in each cleaning solution. After about 3 minutes, the test piece was dried, and then the washing condition of the test piece was inspected. As a washing solvent, use 1,1,1,3,3-pentafluorobutane (365mfc), mix nitromethane, nitroethane, d-terpene and 3-methoxy butyl Acetate (3-MBA). Table 1 below shows the composition of the washing liquid and the washing effect.

表1Table 1

机械油的洗涤试验1(365mfc、硝基乙烷、硝基甲烷、d-萜二烯、3-MBA)Machine oil washing test 1 (365mfc, nitroethane, nitromethane, d-terpene, 3-MBA)

Figure C20051011869300091
Figure C20051011869300091

○:良好×:洗涤效果差○: Good ×: Poor washing effect

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

分别研究在1,1,1,3,3-五氟丁烷(365mfc)中,作为丙二醇系溶剂混合有丙二醇甲基醚[PM]的混合液、混合有丙二醇-n-丁基醚[PnB]的混合液、和混合有二丙二醇-n-丁基醚[DPnB]的混合液,试验结果示于下面的表2~表4中。In 1,1,1,3,3-pentafluorobutane (365mfc), a mixture of propylene glycol methyl ether [PM] as a propylene glycol solvent, a mixture of propylene glycol-n-butyl ether [PnB ] and the mixed solution containing dipropylene glycol-n-butyl ether [DPnB], the test results are shown in Tables 2 to 4 below.

表2Table 2

机械油洗涤试验2(365mfc·PM)Mechanical oil washing test 2 (365mfc·PM)

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PM:丙二醇甲基醚PM: Propylene Glycol Methyl Ether

表3table 3

机械油洗涤试验3(365mfc·PnB)Mechanical oil washing test 3 (365mfc PnB)

Figure C20051011869300102
Figure C20051011869300102

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PnB:丙二醇-n-丁基醚PnB: Propylene glycol-n-butyl ether

表4Table 4

机械油洗涤试验4(365mfc·DPnB)Mechanical oil washing test 4 (365mfc·DPnB)

Figure C20051011869300103
Figure C20051011869300103

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

由试验结果可以看出,通过在1,1,1,3,3-五氟丁烷(365mfc)中,混合硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯或丙二醇系溶剂,可以提高洗涤能力,可洗涤机械油。而且在这种情况下,硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯的混合量需要设定在30重量%以上。对于丙二醇系溶剂的混合量需要设定在20重量%以上。As can be seen from the test results, in 1,1,1,3,3-pentafluorobutane (365mfc), mixed nitromethane, nitroethane, d-terpene, 3-methoxyl Butyl acetate or propylene glycol solvents can improve the cleaning ability and can wash machine oil. Furthermore, in this case, the mixing amount of nitromethane, nitroethane, d-terpene, and 3-methoxybutyl acetate needs to be set at 30% by weight or more. It is necessary to set the compounding quantity of a propylene glycol-type solvent to 20 weight% or more.

《焊剂洗涤试验1》"Flux Washing Test 1"

该试验是将焊剂(田村F-AL-4、株式会社田村制作所制)涂敷在测试用的印刷基板整面上,在约200℃的电炉中烧结处理2分钟,之后浸渍在洗涤液中约3分钟。之后干燥处理印刷基板,然后考察洗涤状态。对在1,1,1,3,3-五氟丁烷(365mfc)中,分别混合硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯(3-MBA)的洗涤液,和作为丙二醇系溶剂分别混合丙二醇甲基醚[PM]、丙二醇-n-丁基醚[PnB],或二·丙二醇-n-丁基醚[DPnB]的洗涤液进行了研究,将试验结果示于下面的表5~表8中。In this test, flux (Tamura F-AL-4, manufactured by Tamura Manufacturing Co., Ltd.) is applied to the entire surface of the printed circuit board for testing, fired in an electric furnace at about 200°C for 2 minutes, and then immersed in a cleaning solution. about 3 minutes. After that, the printed substrate was dried, and then the state of washing was examined. In 1,1,1,3,3-pentafluorobutane (365mfc), mix nitromethane, nitroethane, d-terpene, 3-methoxy butyl acetate ( 3-MBA), and propylene glycol methyl ether [PM], propylene glycol-n-butyl ether [PnB], or dipropylene glycol-n-butyl ether [DPnB] as a propylene glycol-based solvent. The examination was conducted, and the test results are shown in Tables 5 to 8 below.

表5table 5

焊剂洗涤试验(365mfc、硝基乙烷、硝基甲烷、d-萜二烯、3-MBA)Flux wash test (365mfc, nitroethane, nitromethane, d-terpene, 3-MBA)

Figure C20051011869300121
Figure C20051011869300121

○:良好  ×:洗涤效果差○: Good ×: Poor washing effect

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

表6Table 6

焊剂洗涤试验2(365mfc·PM)Flux washing test 2 (365mfc·PM)

Figure C20051011869300131
Figure C20051011869300131

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PM:丙二醇甲基醚PM: Propylene Glycol Methyl Ether

表7Table 7

焊剂洗涤试验3(365mfc·PnB)Flux wash test 3 (365mfc·PnB)

Figure C20051011869300132
Figure C20051011869300132

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PnB:丙二醇-n-丁基醚PnB: Propylene glycol-n-butyl ether

表8Table 8

焊剂洗涤试验4(365mfc·DPnB)Flux wash test 4 (365mfc·DPnB)

Figure C20051011869300133
Figure C20051011869300133

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

从试验结果可以看出,通过混合硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯(3-MBA)或者丙二醇系溶剂,发现可提高洗涤能力,可洗涤焊剂。而且发现对硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯(3-MBA)需要混合40重量%以上,丙二醇系溶剂需要混合30重量%以上。From the test results, it can be seen that by mixing nitromethane, nitroethane, d-terpene, 3-methoxybutyl acetate (3-MBA) or propylene glycol-based solvents, it was found that the cleaning ability can be improved , Washable flux. Furthermore, it has been found that p-nitromethane, nitroethane, d-terpene, and 3-methoxybutyl acetate (3-MBA) need to be mixed at least 40% by weight, and propylene glycol-based solvents need to be mixed at least 30% by weight. .

《易燃性试验》"Flammability Test"

在本试验中,在1,1,1,3,3-五氟丁烷中分别混合硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯或者丙二醇系溶剂,考察其易燃性。1,1,1,3,3-五氟丁烷(365mfc)如前所述没有易燃性,为不燃物,与此相对,硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯或者丙二醇系溶剂具有易燃性,为可燃物,所以担心使其混合后成为可燃物。因此,为了不产生易燃性,考察了硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯或者丙二醇系溶剂适当的混合量。In this test, nitromethane, nitroethane, d-terpene, 3-methoxybutyl acetate or Propylene glycol-based solvents were investigated for their flammability. 1,1,1,3,3-Pentafluorobutane (365mfc) has no flammability as mentioned above and is a non-combustible substance. In contrast, nitromethane, nitroethane, d-terpene, 3 -Methoxy butyl acetate or propylene glycol-based solvents are flammable and combustible, so there is a concern that they may become combustible after they are mixed. Therefore, in order not to cause flammability, an appropriate mixing amount of nitromethane, nitroethane, d-terpene, 3-methoxybutyl acetate, or a propylene glycol-based solvent was considered.

准备在1,1,1,3,3-五氟丁烷(365mfc)中,分别混合硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯(3-MBA)的洗涤液,和作为丙二醇系溶剂分别混合丙二醇甲基醚[PM]、丙二醇-n-丁基醚[PnB],或二丙二醇-n-丁基醚[DPnB]的洗涤液,考察混合量和易燃性的关系。试验结果示于下面的表9~表12中。对其易燃性利用标签密闭方式考察。Prepare to mix nitromethane, nitroethane, d-terpene, 3-methoxy butyl acetate ( 3-MBA), and a propylene glycol-based solvent mixed with propylene glycol methyl ether [PM], propylene glycol-n-butyl ether [PnB], or dipropylene glycol-n-butyl ether [DPnB], Investigate the relationship between the mixing amount and flammability. The test results are shown in Tables 9 to 12 below. Its flammability was inspected by label sealing method.

表9Table 9

易燃性试验1(365mfc、硝基乙烷、硝基甲烷、d-萜二烯、3-MBA)Flammability test 1 (365mfc, nitroethane, nitromethane, d-terpene, 3-MBA)

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

表10Table 10

易燃性试验2(365mfc·PM)Flammability test 2 (365mfc·PM)

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PM:丙二醇甲基醚PM: Propylene Glycol Methyl Ether

表11Table 11

易燃性试验3(365mfc·PnB)Flammability test 3 (365mfc·PnB)

Figure C20051011869300162
Figure C20051011869300162

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PnB:丙二醇-n-丁基醚PnB: Propylene glycol-n-butyl ether

表12Table 12

易燃性试验4(365mfc·DPnB)Flammability Test 4 (365mfc·DPnB)

Figure C20051011869300163
Figure C20051011869300163

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

由试验结果可以看出,对于硝基甲烷以及硝基乙烷在80重量%以上,d-萜二烯、3-甲氧基·丁基乙酸酯(3-MBA)在95重量%以上分别显示易燃性,所以为了使其没有易燃性,需要将硝基甲烷以及硝基乙烷的含有量设定在70重量%以下,将d-萜二烯、3-甲氧基·丁基乙酸酯(3-MBA)的含有量设定在90重量%以下。As can be seen from the test results, for nitromethane and nitroethane above 80% by weight, d-terpene and 3-methoxy butyl acetate (3-MBA) above 95% by weight respectively Shows flammability, so in order to make it non-flammable, it is necessary to set the content of nitromethane and nitroethane to 70% by weight or less, and d-terpene, 3-methoxy butyl The content of acetate (3-MBA) is set at 90% by weight or less.

对于丙二醇甲基醚[PM],可知在其混合80重量%以上时产生易燃性。在丙二醇-n-丁基醚[PnB]以及二·丙二醇-n-丁基醚[DPnB]的情况下,可知在其混合95重量%以上时产生易燃性。由此可知,为了使混合丙二醇系溶剂不产生易燃性,需要控制混合量,对于丙二醇甲基醚[PM]在75重量%以下、对于丙二醇-n-丁基醚[PnB]或二·丙二醇-n-丁基醚[DPnB]在90重量%以下。Propylene glycol methyl ether [PM] was found to be inflammable when mixed at 80% by weight or more. In the case of propylene glycol-n-butyl ether [PnB] and dipropylene glycol-n-butyl ether [DPnB], it was found that flammability occurs when they are mixed at 95% by weight or more. It can be seen from this that in order to prevent the flammability of the mixed propylene glycol solvent, it is necessary to control the mixing amount. For propylene glycol methyl ether [PM], it is 75% by weight or less; for propylene glycol-n-butyl ether [PnB] or dipropylene glycol -n-butyl ether [DPnB] is at most 90% by weight.

《机械油的洗涤试验2》"Machine Oil Washing Test 2"

下面,对1,1,1,3,3-五氟丁烷(365mfc)和丙二醇系溶剂的混合溶剂中混合硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯(3-MBA)、3-甲氧基-1-丁醇或d-萜二烯后的机械油的洗涤性能考察的试验进行说明。在该试验中,为了显著提高这些溶剂混合的洗涤能力,对洗涤效果不太良好的丙二醇系溶剂的混合量在10重量%以下的情况进行考察。Next, nitromethane, nitroethane, 3-methoxy butyl acetate ( 3-MBA), 3-methoxy-1-butanol or d-terpene after the washing performance of the machine oil test to illustrate. In this test, in order to remarkably improve the cleaning ability of mixing these solvents, the case where the mixing amount of the propylene glycol-based solvent whose cleaning effect is not so good is 10 weight% or less was examined.

和前述的试验相同,准备SUS-304试验片(长25mm×宽30mm×高2mm),将该试验片浸渍在机械油(CQ-30:日本石油株式会社制)中,之后在各洗涤液中浸渍约3分钟,其后干燥处理试验片,然后考察试验片的洗涤状况。试验结果示于下面表13~15中。In the same manner as the previous test, a SUS-304 test piece (length 25 mm x width 30 mm x height 2 mm) was prepared, and the test piece was immersed in machine oil (CQ-30: manufactured by Nippon Oil Corporation), and then washed in each washing solution. After dipping for about 3 minutes, the test piece was dried, and then the washing condition of the test piece was examined. The test results are shown in Tables 13-15 below.

表13Table 13

机械油的洗涤试验5(365mfc、PM、硝基乙烷、硝基甲烷、3-MBA、3-M-1-B、d-萜二烯)Machine oil washing test 5 (365mfc, PM, nitroethane, nitromethane, 3-MBA, 3-M-1-B, d-terpene)

Figure C20051011869300181
Figure C20051011869300181

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PM:丙二醇甲基醚PM: Propylene Glycol Methyl Ether

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

3-M-1-B:3-甲氧基-1-丁醇3-M-1-B: 3-methoxy-1-butanol

表14Table 14

机械油的洗涤试验6(365mfc、PnB、硝基乙烷、硝基甲烷、3-MBA、3-M-1-B、d-萜二烯)Machine oil washing test 6 (365mfc, PnB, nitroethane, nitromethane, 3-MBA, 3-M-1-B, d-terpene)

Figure C20051011869300191
Figure C20051011869300191

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PnB:丙二醇-n-丁基醚PnB: Propylene glycol-n-butyl ether

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

3-M-1-B:3-甲氧基-1-丁醇3-M-1-B: 3-methoxy-1-butanol

表15Table 15

机械油的洗涤试验7(365mfc、DPnB、硝基乙烷、硝基甲烷、3-MBA、3-M-1-B、d-萜二烯)Machine oil washing test 7 (365mfc, DPnB, nitroethane, nitromethane, 3-MBA, 3-M-1-B, d-terpene)

Figure C20051011869300201
Figure C20051011869300201

×:洗涤效果差  ○:良好  ◎:非常良好×: Poor washing effect ○: Good ◎: Very good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

3-M-1-B:3-甲氧基-1-丁醇3-M-1-B: 3-methoxy-1-butanol

由试验结果可以看出,通过混合硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯(3-MBA)、3-甲氧基-1-丁醇或d-萜二烯,比只混合丙二醇系溶剂时的洗涤能力强。在1,1,1,3,3-五氟丁烷(365mfc)为85重量%时,这些溶剂的混合量优选设定在至少5重量%以上。As can be seen from the test results, by mixing nitromethane, nitroethane, 3-methoxy butyl acetate (3-MBA), 3-methoxy-1-butanol or d-terpene di Alkene, the cleaning ability is stronger than when only propylene glycol-based solvent is mixed. When 1,1,1,3,3-pentafluorobutane (365mfc) is 85% by weight, the mixing amount of these solvents is preferably set at least 5% by weight or more.

《焊剂洗涤试验2》"Flux Washing Test 2"

下面对硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯(3-MBA)、3-甲氧基-1-丁醇或d-萜二烯混合后的焊剂洗涤试验进行说明。为了明显提高混合这些溶剂的洗涤能力,对洗涤效果不太良好的丙二醇系溶剂的混合量在20重量%以下时进行考察。Flux wash after mixing nitromethane, nitroethane, 3-methoxybutyl acetate (3-MBA), 3-methoxy-1-butanol or d-terpene The test is explained. In order to remarkably improve the cleaning ability of mixing these solvents, it was considered that the mixing amount of the propylene glycol-based solvent whose cleaning effect is not so good is 20% by weight or less.

和前述试验相同,该试验是将焊剂(田村F-AL-4、株式会社田村制作所制)涂敷在测试用的印刷基板整面上,在约200℃的电炉中烧结处理2分钟,处理之后浸渍在洗涤液中约3分钟。之后干燥处理印刷基板,考察洗涤状态,试验结果示于下面的表16~18中。Similar to the previous test, in this test, flux (Tamura F-AL-4, manufactured by Tamura Manufacturing Co., Ltd.) is applied to the entire surface of the printed circuit board for testing, and it is sintered in an electric furnace at about 200°C for 2 minutes. Then soak in the washing liquid for about 3 minutes. Thereafter, the printed boards were dried, and the washing state was examined. The test results are shown in Tables 16 to 18 below.

表16Table 16

焊剂洗涤试验5(365mfc、PM、硝基乙烷、硝基甲烷、3-MBA、3-M-1-B、d-萜二烯)Flux wash test 5 (365mfc, PM, nitroethane, nitromethane, 3-MBA, 3-M-1-B, d-terpene)

Figure C20051011869300221
Figure C20051011869300221

×:洗涤效果差  ○:良好×: Poor washing effect ○: Good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PM:丙二醇甲基醚PM: Propylene Glycol Methyl Ether

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

3-M-1-B:3-甲氧基-1-丁醇3-M-1-B: 3-methoxy-1-butanol

表17Table 17

焊剂洗涤试验6(365mfc、PnB、硝基乙烷、硝基甲烷、3-MBA、3-M-1-B、d-萜二烯)Flux wash test 6 (365mfc, PnB, nitroethane, nitromethane, 3-MBA, 3-M-1-B, d-terpene)

×:洗涤效果差  ○:良好×: Poor washing effect ○: Good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PnB:丙二醇-n-丁基醚PnB: Propylene glycol-n-butyl ether

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

3-M-1-B:3-甲氧基-1-丁醇3-M-1-B: 3-methoxy-1-butanol

表18Table 18

焊剂洗涤试验7(365mfc、DPnB、硝基乙烷、硝基甲烷、3-MBA、3-M-1-B、d-萜二烯)Flux wash test 7 (365mfc, DPnB, nitroethane, nitromethane, 3-MBA, 3-M-1-B, d-terpene)

Figure C20051011869300241
Figure C20051011869300241

×:洗涤效果差  ○:良好×: Poor washing effect ○: Good

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

3-M-1-B:3-甲氧基-1-丁醇3-M-1-B: 3-methoxy-1-butanol

从试验结果可以看出,混合硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇,比只混合丙二醇系溶剂(PM,PnB,DPnB)时更能提高洗涤能力。对于这些硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯或3-甲氧基-1-丁醇的混合量优选在1,1,1,3,3-五氟丁烷(365mfc)75重量%时,设定为15重量%以上。另外,对于d-萜二烯不能得到良好的结果。As can be seen from the test results, mixing nitromethane, nitroethane, 3-methoxyl butyl acetate, 3-methoxyl-1-butanol is more effective than mixing only propylene glycol solvents (PM, PnB , DPnB) can improve the washing ability. The mixing amount of these nitromethane, nitroethane, 3-methoxyl butyl acetate or 3-methoxyl-1-butanol is preferably in the range of 1,1,1,3,3-pentafluoro When butane (365mfc) is 75% by weight, it is set to 15% by weight or more. In addition, no good results were obtained for d-terpenes.

《对塑料或橡胶等的影响》"Effects on plastic or rubber, etc."

下面试验考察本发明涉及的洗涤液溶剂组合物对各种塑料或橡胶等的影响。在本试验中,塑料准备软质氯乙烯、硬质氯乙烯、聚碳酸酯(PC)、丙烯酸树脂、尼龙66(注册商标)、聚缩醛、聚氨基甲酸乙酯树脂、酚醛树脂、环氧树脂、蜜胺甲醛树脂、尿素树脂、聚乙烯、聚丙烯,橡胶准备氟橡胶、氯丁橡胶、硅橡胶、氨基甲酸乙酯橡胶、SBR、天然橡胶、丁基橡胶,分别在常温下浸渍洗涤液6小时,进行试验。其后进行干燥处理,考察有无影响。该试验结果示于下面的表19~22中。The following test investigates the impact of the detergent solvent composition involved in the present invention on various plastics or rubbers. In this test, plastics prepared soft vinyl chloride, rigid vinyl chloride, polycarbonate (PC), acrylic resin, nylon 66 (registered trademark), polyacetal, polyurethane resin, phenolic resin, epoxy Resin, melamine-formaldehyde resin, urea resin, polyethylene, polypropylene, rubber preparation Fluororubber, neoprene, silicone rubber, urethane rubber, SBR, natural rubber, butyl rubber, respectively impregnated with washing liquid at room temperature 6 hours to test. Afterwards, drying treatment was carried out, and the presence or absence of influence was examined. The test results are shown in Tables 19-22 below.

表19Table 19

对塑料·橡胶等的影响1(365mfc、硝基乙烷、硝基甲烷)Effects on plastics, rubber, etc. 1 (365mfc, nitroethane, nitromethane)

Figure C20051011869300261
Figure C20051011869300261

○:无影响  ×:有影响○: no influence ×: influence

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

表20Table 20

对塑料·橡胶等的影响2(365mfc、d-萜二烯、3-MBA)Effects on plastics, rubber, etc. 2 (365mfc, d-terpene, 3-MBA)

Figure C20051011869300271
Figure C20051011869300271

○:无影响  ×:有影响○: no influence ×: influence

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

Figure C20051011869300281
Figure C20051011869300281

表22Table 22

对塑料·橡胶等的影响4(365mfc、DPnB)Effects on plastics, rubber, etc. 4 (365mfc, DPnB)

Figure C20051011869300291
Figure C20051011869300291

○:无影响  ×:有影响○: no influence ×: influence

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

由试验结果可知,本发明涉及的洗涤用溶剂组合物对各种塑料或橡胶类不带来不良影响。From the test results, it can be seen that the solvent composition for cleaning according to the present invention does not have adverse effects on various plastics or rubbers.

《金属腐蚀试验》"Metal Corrosion Test"

本试验根据JIS-K1600,在洗涤后的洗涤液的液相部及其气相部的各处上配制铝片(JIS-H-4000、A1100P),考察约48小时后的金属腐蚀状况。将结果示于下面的表23及24中。In this test, according to JIS-K1600, aluminum sheets (JIS-H-4000, A1100P) were prepared on the liquid phase part and the gas phase part of the washing liquid after washing, and the metal corrosion state after about 48 hours was investigated. The results are shown in Tables 23 and 24 below.

表23Table 23

金属腐蚀试验1(365mfc、硝基乙烷、硝基甲烷、d-萜二烯、3-MBA)Metal corrosion test 1 (365mfc, nitroethane, nitromethane, d-terpene, 3-MBA)

Figure C20051011869300301
Figure C20051011869300301

×:有腐蚀  ○:无腐蚀×: corrosion ○: no corrosion

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

3-MBA:3-甲氧基·丁基乙酸酯3-MBA: 3-methoxybutyl acetate

表24Table 24

金属腐蚀试验2(365mfc、PM、PnB、DPnB)Metal Corrosion Test 2 (365mfc, PM, PnB, DPnB)

Figure C20051011869300311
Figure C20051011869300311

○:良好  ×:洗涤效果差○: Good ×: Poor washing effect

365mfc:1,1,1,3,3-五氟丁烷(C4H5F5)365mfc: 1,1,1,3,3-pentafluorobutane (C 4 H 5 F 5 )

PM:丙二醇甲基醚PM: Propylene Glycol Methyl Ether

PnB:丙二醇-n-丁基醚PnB: Propylene glycol-n-butyl ether

DPnB:二·丙二醇-n-丁基醚DPnB: Dipropylene glycol-n-butyl ether

由试验结果可以看出,本发明涉及的洗涤用溶剂组合物的任何一种对金属都没有不良影响。It can be seen from the test results that none of the cleaning solvent compositions of the present invention has any adverse effect on metals.

产业上利用的可能性Possibility of industrial use

本发明的第1洗涤用溶剂组合物通过在1,1,1,3,3-五氟丁烷中含有硝基甲烷、硝基乙烷、d-萜二烯、3-甲氧基·丁基乙酸酯,可以大幅度地提高洗涤能力、特别是脱脂洗涤能力,可以使其充分发挥洗涤性能。因为没有易燃性,不成为危险物,所以可安全使用,同时臭氧破坏系数(ODP)以及温暖化系数(GWP)也小,对环境有利。The first cleaning solvent composition of the present invention contains nitromethane, nitroethane, d-terpene, 3-methoxybutane in 1,1,1,3,3-pentafluorobutane Glyceryl acetate can greatly improve the washing ability, especially the degreasing washing ability, and can make it fully play the washing performance. Because it is not flammable and does not become a dangerous substance, it can be used safely. At the same time, its ozone destruction coefficient (ODP) and warming coefficient (GWP) are also small, which is beneficial to the environment.

本发明的第2洗涤用溶剂组合物通过含有30~70重量%的(a)1,1,1,3,3-五氟丁烷、30~70重量%的(b)选自硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂,可以避免硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯的混合量过少难以提高洗涤能力,这些溶剂的混合量过多,可以防止产生易燃性。The second cleaning solvent composition of the present invention contains 30 to 70% by weight of (a) 1,1,1,3,3-pentafluorobutane, 30 to 70% by weight of (b) selected from nitromethane , nitroethane, d-terpene and 3-methoxy butyl acetate at least one solvent or a mixture of two or more solvents can avoid nitromethane, nitroethane, d- If the blending amount of terpene and 3-methoxybutyl acetate is too small, it will be difficult to improve the detergency, and if the blending amount of these solvents is too large, the occurrence of flammability can be prevented.

本发明的第3洗涤用溶剂组合物,在含有40~70重量%范围内的硝基甲烷、硝基乙烷、d-萜二烯以及3-甲氧基·丁基乙酸酯中的至少1种溶剂或2种以上的混合溶剂,足以洗涤焊剂。The third cleaning solvent composition of the present invention contains at least one of nitromethane, nitroethane, d-terpene and 3-methoxy butyl acetate in the range of 40 to 70% by weight. One solvent or a mixture of two or more solvents is enough to wash the flux.

本发明的第4洗涤用溶剂组合物含有1,1,1,3,3-五氟丁烷和丙二醇系溶剂,可大幅度地提高洗涤能力、特别是脱脂洗涤能力,作为各种洗涤剂发挥充分的性能。并且丙二醇系溶剂没有毒性,非常安全,容易操作,而且在其分子结构中不含有氯或氟,臭氧破坏系数(ODP)和温暖化系数(GWP)也小,所以具有环境有利的特性。而且通过和1,1,1,3,3-五氟丁烷配合,可以克服丙二醇系溶剂易燃性的缺点,制成没有易燃性,安全的阻燃物。The fourth cleaning solvent composition of the present invention contains 1,1,1,3,3-pentafluorobutane and propylene glycol-based solvents, can greatly improve the cleaning ability, especially the degreasing cleaning ability, and can be used as various detergents. full performance. Moreover, propylene glycol solvents are non-toxic, very safe, easy to handle, and do not contain chlorine or fluorine in their molecular structure, and their ozone destruction coefficient (ODP) and warming coefficient (GWP) are also small, so they have environmentally friendly characteristics. Moreover, by coordinating with 1,1,1,3,3-pentafluorobutane, the shortcoming of flammability of propylene glycol solvents can be overcome, and a safe flame retardant without flammability can be made.

本发明的第5洗涤用溶剂组合物含有10~80重量%的(a)1,1,1,3,3-五氟丁烷、20~90重量%的(d)1种和2种以上的丙二醇系溶剂,可以避免丙二醇系溶剂的混合量过低时提高洗涤能力不足,或者可以控制丙二醇系溶剂的混合量过高时产生易燃性。The fifth cleaning solvent composition of the present invention contains 10 to 80% by weight of (a) 1,1,1,3,3-pentafluorobutane, and 20 to 90% by weight of (d) one or more types Propylene glycol-based solvents can avoid insufficient washing performance when the mixing amount of propylene glycol-based solvents is too low, or can control flammability when the mixing amount of propylene glycol-based solvents is too high.

本发明的第6洗涤用溶剂组合物含有30~90重量%的1种和2种以上的丙二醇系溶剂,可以充分洗涤焊剂。The sixth cleaning solvent composition of the present invention contains 30 to 90% by weight of one or two or more propylene glycol-based solvents, and can sufficiently clean flux.

本发明的第4~6的洗涤用溶剂组合物,含有选自(b)硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇以及d-萜二烯中的至少1种溶剂,可以提高溶解力,可发挥强洗涤力。The cleaning solvent composition of the 4th to 6th of the present invention contains a solvent selected from (b) nitromethane, nitroethane, 3-methoxy butyl acetate, 3-methoxy-1-butan At least one kind of solvent among alcohol and d-terpene can improve the dissolving power and can exhibit strong detergency.

Claims (4)

1.洗涤用溶剂组合物,其特征在于,含有:1. A solvent composition for washing, characterized in that it contains: 10~80重量%的(a)1,1,1,3,3-五氟丁烷、10 to 80% by weight of (a) 1,1,1,3,3-pentafluorobutane, 20~90重量%的(c)选自丙二醇甲基醚、二·丙二醇甲基醚、三·丙二醇甲基醚、丙二醇-n-丁基醚、二·丙二醇-n-丁基醚、三·丙二醇-n-丁基醚、丙二醇甲基醚乙酸酯、丙二醇二乙酸酯、丙二醇苯基醚以及丙二醇单乙醇醚乙酸酯的1种或2种以上的溶剂。20 to 90% by weight of (c) selected from propylene glycol methyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, propylene glycol-n-butyl ether, dipropylene glycol-n-butyl ether, tripropylene glycol methyl ether, One or more solvents of propylene glycol-n-butyl ether, propylene glycol methyl ether acetate, propylene glycol diacetate, propylene glycol phenyl ether, and propylene glycol monoethyl ether acetate. 2.权利要求1所述的洗涤用溶剂组合物,其特征在于,含有:2. The solvent composition for washing according to claim 1, characterized in that it contains: 10~70重量%的上述(a)1,1,1,3,3-五氟丁烷、10 to 70% by weight of the above (a) 1,1,1,3,3-pentafluorobutane, 30~90重量%的上述(c)选自丙二醇甲基醚、二·丙二醇甲基醚、三·丙二醇甲基醚、丙二醇-n-丁基醚、二·丙二醇-n-丁基醚、三·丙二醇-n-丁基醚、丙二醇甲基醚乙酸酯、丙二醇二乙酸酯、丙二醇苯基醚以及丙二醇单乙醇醚乙酸酯的1种或2种以上的溶剂。30 to 90% by weight of the above (c) is selected from propylene glycol methyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, propylene glycol-n-butyl ether, dipropylene glycol-n-butyl ether, tripropylene glycol methyl ether, - One or more solvents of propylene glycol-n-butyl ether, propylene glycol methyl ether acetate, propylene glycol diacetate, propylene glycol phenyl ether, and propylene glycol monoethyl ether acetate. 3.如权利要求1~2任何一项中所述的洗涤用溶剂组合物,其中含有(d)选自硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇以及d-萜二烯中的至少1种溶剂。3. The washing solvent composition as described in any one of claims 1 to 2, wherein (d) is selected from the group consisting of nitromethane, nitroethane, 3-methoxy butyl acetate, 3 - at least one solvent selected from methoxy-1-butanol and d-terpene. 4.如权利要求1~2任何一项中所述的洗涤用溶剂组合物,其中含有5重量%以上的(d)选自硝基甲烷、硝基乙烷、3-甲氧基·丁基乙酸酯、3-甲氧基-1-丁醇以及d-萜二烯中的至少1种溶剂。4. The cleaning solvent composition as described in any one of claims 1 to 2, wherein more than 5% by weight of (d) is selected from the group consisting of nitromethane, nitroethane, 3-methoxy butyl At least one solvent selected from acetate, 3-methoxy-1-butanol, and d-terpene.
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