CN101426894A - 用于清洁应用的包含氟化物的共沸组合物 - Google Patents
用于清洁应用的包含氟化物的共沸组合物 Download PDFInfo
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- CN101426894A CN101426894A CNA2007800070549A CN200780007054A CN101426894A CN 101426894 A CN101426894 A CN 101426894A CN A2007800070549 A CNA2007800070549 A CN A2007800070549A CN 200780007054 A CN200780007054 A CN 200780007054A CN 101426894 A CN101426894 A CN 101426894A
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- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- WAGFXJQAIZNSEQ-UHFFFAOYSA-M tetraphenylphosphonium chloride Chemical compound [Cl-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 WAGFXJQAIZNSEQ-UHFFFAOYSA-M 0.000 description 1
- 125000002221 trityl group Chemical group [H]C1=C([H])C([H])=C([H])C([H])=C1C([*])(C1=C(C(=C(C(=C1[H])[H])[H])[H])[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Abstract
本发明涉及组合物,该组合物包含全氟-1-己烯和至少一种卤代烃、氢氟烃或氟醚。在一个实施方案中,这些组合物是共沸的或类似共沸物的。在另一个实施方案中,这些组合物作为用于从表面去除油和/或其它残留物的脱脂剂或去焊药剂用于清洁应用中。
Description
相关申请交叉参考
本申请要求于2006年2月28日提交的美国临时申请60/777,350的优先权。
发明背景
技术领域
本发明涉及组合物,该组合物包含氟化烯烃或氟化酮和至少一种醇、卤代烃、氟烷基醚或氢氟烃及其组合。这些组合物是共沸的或类似共沸物的,并可作为去焊药剂用于清洁应用以及用于从表面去除油或残留物。
背景技术
焊药残留物总是存在于使用松香焊药组装的微电子部件上。由于现代电子电路板向着扩大电路和部件密度的方向发展,在焊接后整个板的清洁成为了重要的加工步骤。在焊接后,通常用有机熔剂去除焊药残留物。去焊药溶剂应当是不可燃的,具有低毒性和具有高溶解力,以便焊药和焊药残留物可以在未损害被清洁基片的情况下去除。而且,其它类型的残留物,例如油和油脂,必须有效地从这些装置中去除以在使用中获得最佳性能。
可选择地,由于作为蒙特利尔协议(Montreal Protocol)的结果,淘汰了几乎全部先前的CFCs和HCFCs,非臭氧消耗溶剂已经变得可得。虽然通常可以通过制备溶剂混合物来调节沸点、燃烧性和溶解能力特性,但这些混合物通常是不令人满意的,因为它们在使用期间分馏至不理想的程度。这种溶剂混合物还在溶剂蒸馏期间分馏,使得回收原始组合物的溶剂混合物实际上是不可能的。
共沸溶剂混合物可以具有这些去焊药、去油脂应用所需和其它清洁剂需要的性能。共沸混合物显示出或者最大或者最小的沸点并且在沸腾时不分馏。在沸腾条件下组成的内在恒定性确保混合物的各个组分的比率在使用期间不会改变且溶解性能也保持恒定。
本发明提供了用于半导体芯片和电路板清洁、去焊药和去油脂工序的共沸的和类似共沸物的组合物。本发明的组合物是不可燃的,并且由于其并不分馏而不会在使用期间产生可燃组合物。另外,所使用的共沸溶剂混合物可以再蒸馏和再使用而组成不变。
发明简述
本发明涉及组合物,该组合物包含氟化烯烃和至少一种选自卤代烃、氟烷基醚和氢氟烃的化合物,其中所述至少一种化合物不是单独的反式-1,2-二氯乙烯、单独的C4F9OCH3、单独的HFC-43-10mee、单独的HFC-365mfc、或反式-1,2-二氯乙烯与C4F9OC2H5的混合物。在一个实施方案中,所述至少一种化合物选自:
正丙基溴;
三氯乙烯;
四氯乙烯;
反式-1,2-二氯乙烯;
甲醇;
乙醇;
正丙醇;
异丙醇;
C4F9OCH3;
C4F9OC2H5;
HFC-43-10mee;
HFC-365mfc及其组合。
在一个实施方案中,所述组合物是共沸的或类似共沸物的。此外,本发明涉及清洁表面或从表面例如集成电路器件去除残留物的方法。
发明详述
发明人特别地引入了在本公开中引用的所用文件的全部内容作为参考。而且,当数量、浓度或其它值或参数以或者范围、优选范围或者一系列上限优选值和下限优选值给出时,应当理解为特别公开了由任何成对的任何上限范围限定或优选值和任何下限范围限定或优选值所形成的所有范围,无论范围是否被分别公开。当本文列出了一个数值范围,除非另外指出,所述范围拟包括其端点和该范围内的所有整数和分数。当限定一个范围时,本发明的保护范围并不拟限于所列出的具体值。
在一个实施方案中,本发明涉及包含具有式E-或Z-R1CH=CHR2(式I)的化合物的组合物,其中,R1和R2独立地是C1-C5全氟烷基基团和至少一种醇、卤代烃、氟烷基醚或氢氟烃及其组合。R1和R2基团的例子包括但不限于CF3、C2F5、n-C3F7、i-C3F7、n-C4F9、n-C5F11和i-C4F9。典型的,非限制性的式I的化合物列于表1。
表1
代码 | 结构 | IUPAC名称 |
F11E | CF3CH=CHCF3 | 1,1,1,4,4,4-六氟-2-丁烯 |
F12E | CF3CH=CHC2F5 | 1,1,1,4,4,5,5,5-八氟-2-戊烯 |
F13E | CF3CH=CH(n-C3F7) | 1,1,1,4,4,5,5,6,6,6-十氟-2-己烯 |
F13iE | CF3CH=CH(i-C3F7) | 1,1,1,4,4,5,5,5-七氟-4-(三氟甲基)-2-戊烯 |
F22E | C2F5CH=CHC2F5 | 1,1,1,2,2,5,5,6,6,6-十氟-3-己烯 |
F14E | CF3CH=CH(n-C4F9) | 1,1,1,4,4,5,5,6,6,7,7,7-十二氟庚-2-烯 |
F23E | C2F5CH=CH(n-C3F7) | 1,1,1,2,2,5,5,6,6,7,7,7-十二氟庚-3-烯 |
F23iE | C2F5CH=CH(i-C3F7) | 1,1,1,2,2,5,6,6,6-九氟-5-(三氟甲基)己-3-烯 |
F15E | CF3CH=CH(n-C5F11) | 1,1,1,4,4,5,5,6,6,7,7,8,8,8-十四氟辛-2-烯 |
F24E | C2F5CH=CH(n-C4F9) | 1,1,1,2,2,5,5,6,6,7,7,8,8,8-十四氟辛-3-烯 |
F33E | n-C3F7CH=CH(n-C3F7) | 1,1,1,2,2,3,3,6,6,7,7,8,8,8-十四氟辛-4-烯 |
F3i3iE | i-C3F7CH=CH(i-C3F7) | 1,1,1,2,5,6,6,6-八氟-2,5-二(三甲基氟)己-3-烯 |
F33iE | n-C3F7CH=CH(i-C3F7) | 1,1,1,2,5,5,6,6,7,7,7-十一氟-2(三氟甲基)庚-3-烯 |
F34E | n-C3F7CH=CH(n-C4F9) | 1,1,1,2,2,3,3,6,6,7,7,8,8,9,9,9-十六氟壬-4-烯 |
F3i4E | i-C3F7CH=CH(n-C4F9) | 1,1,1,2,5,5,6,6,7,7,8,8,8-十三氟-2(三氟甲基)辛-3-烯 |
F44E | n-C4F9CH=CH(n-C4F9) | 1,1,1,2,2,3,3,4,4,7,7,8,8,9,9,10,10,10-十八氟癸-5-烯 |
可以通过使式R1I的全氟烷基碘与式R2CH=CH2的全氟烷基三氢烯烃相接触以形成式R1CH2CHIR2的三氢碘全氟链烷而制备式I的化合物。然后,可以将所述三氢碘全氟链烷脱碘化氢以制备R1CH=CHR2。可选择地,可以通过式R1CHICH2R2的三氢碘全氟链烷的脱碘化氢作用制备所述烯烃R1CH=CHR2,而所述三氢碘全氟链烷反过来是通过使式R2I的全氟烷基碘与式R1CH=CH2的全氟烷基三氢烯烃反应而形成的。
全氟烷基碘与全氟烷基三氢烯烃的所述接触可以在反应温度下在反应物和生成物的自生压力下,通过在能够操作的合适的反应容器中混合反应物而以间歇方式发生。合适的反应容器包括由不锈钢制成的那些,尤其是奥氏体型的,和公知的高镍合金例如镍铜合金、镍基合金和镍铬合金。可选择地,所述反应可以以半间歇方式进行,其中通过合适的添加装置例如泵在反应温度下将全氟烷基三氢烯烃反应物加入到全氟烷基碘反应物中。
全氟烷基碘与全氟烷基三氢烯烃的比应当介于约1:1至约4:1,优选为约1.5:1至2.5:1。如Jeanneaux等在Journal of Fluorine Chemistry,Vol.4,261-270页(1974)中报告的,小于1.5:1的比率倾向于导致大量的2:1加合物。
所述全氟烷基碘与所述全氟烷基三氢烯烃的接触的温度优选在约150℃-300℃的范围内,更优选为约170℃-约250℃,并最优选为约180℃-约230℃。所述全氟烷基碘与所述全氟烷基三氢烯烃的接触的压力优选为所述反应物在反应温度下的自生压力。
全氟烷基碘与全氟烷基三氢烯烃的合适的接触时间为约0.5小时-18小时,优选为约4小时-约12小时。
通过全氟烷基碘与全氟烷基三氢烯烃的反应制备的三氢碘全氟链烷可以在脱碘化氢步骤中直接使用,或者可以优选在脱碘化氢步骤前通过蒸馏回收和纯化。
在又一实施方案中,全氟烷基碘与全氟烷基三氢烯烃的接触在催化剂存在下发生。在一个实施方案中,合适的催化剂为第VIII族过渡金属络合物。代表性的第VIII族过渡金属络合物包括但不限于零价NiL4络合物,其中配体L可以是膦配体、亚磷酸盐配体、羰基配体、异腈配体、链烯烃配体或其组合。在一个此种实施方案中,Ni(O)L4络合物是NiL2(CO)2络合物。在一个具体实施方案中,第VIII族过渡金属络合物是双(三苯基膦)镍(O)二羰基。在一个实施方案中,全氟烷基碘与全氟烷基三氢烯烃的比率介于约3:1和约8:1。在一个实施方案中,在催化剂存在下,所述全氟烷基碘与所述全氟烷基三氢烯烃的接触的温度是在约80℃-约130℃的范围内。在另一个实施方案中,所述温度为约90℃-约120℃。
在一个实施方案中,在催化剂存在下,全氟烷基碘与全氟烷基三氢烯烃的反应的接触时间为约0.5小时-18小时。在另一个实施方案中,所述接触时间为约4-约12小时。
通过使三氢碘全氟链烷与碱性物质接触进行脱碘化氢步骤。合适的碱性物质包括碱金属氢氧化物(例如氢氧化钠或氢氧化钾)、碱金属氧化物(例如氧化钠)、碱土金属氢氧化物(例如氢氧化钙)、碱土金属氧化物(例如氧化钙)、碱金属醇盐(例如甲醇钠或乙醇钠)、氨水溶液、氨基钠或碱性物质的混合物例如钠石灰。优选的碱性物质是氢氧化钠和氢氧化钾。
三氢碘全氟链烷与碱性物质的所述接触可以在液相,优选在能够溶解至少两种反应物的一部分的溶剂的存在下发生。适用于脱碘化氢步骤的溶剂包括一种或多种极性有机溶剂例如醇(例如甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇和叔丁醇)、腈(例如乙腈、丙腈、丁腈、苯甲腈或己二腈)、二甲基亚砜、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺或环丁砜。溶剂的选择取决于碱性物质的溶解度、全氟烷基碘的溶解度、和全氟烷基三氢烯烃的溶解度以及产物的沸点和在纯化过程中从产物中分离痕量溶剂的容易性。典型地,乙醇或异丙醇是所述反应的良溶剂。通过蒸馏、萃取、相分离或此三种的组合可以实现溶剂与所述产物的分离。
典型地,可以通过在合适的反应容器中将一种反应物(或者碱性物质或者三氢碘全氟链烷)加入至另一种反应物进行脱碘化氢反应。所述反应容器可以由玻璃、陶瓷或金属制得,并优选以搅拌器或其它搅拌机械搅拌。
适于脱碘化氢反应的温度为约10℃-约100℃,优选为约20℃-约70℃。脱碘化氢反应可以在环境压力或减压或升压下进行。值得注意的是脱碘化氢反应中式I的化合物随着形成被蒸馏出反应容器。
可选择地,在相转移催化剂存在下,在一种或多种较低极性溶剂例如链烷(例如己烷、庚烷或辛烷)、芳香烃(例如甲苯)、卤代烃(例如二氯甲烷、二氯乙烷、氯仿、四氯化碳或全氯乙烯)或醚(例如二***、甲基叔丁醚、四氢呋喃、2-甲基四氢呋喃、二噁烷、二甲氧基乙烷、二甘醇二甲醚或四甘醇二甲醚)中,脱碘化氢反应可以通过将所述碱性物质水溶液与三氢碘全氟链烷溶液接触而进行。合适的相转移催化剂包括季铵卤化物(例如四丁基溴化铵、四丁基硫酸氢铵、三乙基苄基氯化铵、十二基三甲基氯化铵和三辛酰基(tricaprylyl)甲基氯化铵)、季鏻卤化物(例如三苯基甲基溴化鏻和四苯基氯化鏻)、本领域已知的环醚化合物如冠醚(例如18-冠醚-6和15-冠醚-5)。
可选择地,脱碘化氢反应可以在没有溶剂的存在下通过向一种或多种固体或液体碱性物质中加入三氢碘全氟链烷进行。
脱碘化氢反应的合适的反应时间根据反应物的溶解度为约15分钟-约6小时或更长。典型地,脱碘化氢反应是快速的,并需要约30分钟-约3小时来完成。
式I的化合物可以自脱碘化氢反应混合物中通过相分离,任选地在加入水后、通过蒸馏或其组合而回收。
在另一实施方案中,本发明涉及包含全氟乙基异丙基酮(1,1,1,2,2,4,5,5,5-九氟-4-(三氟甲基)-3-戊酮)(PEIK)和至少两种选自醇、卤代烃、氟烷基醚和氢氟烃的化合物的组合物。PEIK具有CAS登记号No.756-13-8且可购自3MTM(St.Paul,MN)。
在又一实施方案中,本发明涉及包含九氟-1-己烯(3,3,4,4,5,5,6,6,6-九氟-1-己烯)(PFBE)和至少一种选自醇、卤代烃、氟烷基醚和氢氟烃的化合物的组合物。3,3,4,4,5,5,6,6,6-九氟-1-己烯,也被称为HFC-1549fz,具有CAS登记号No.19430-93-4且可购自E.I.DuPont de Nemours & Co(Wilmington,DE)。
在又一个实施方案中,本发明涉及使用共沸的或类似共沸物组合物清洁表面的方法,所述组合物包含氟化烯烃或氟化酮和至少一种选自醇、卤代烃、氟烷基醚和氢氟烃的化合物。
表1的氟化烯烃、PEIK和PFBE可以与表2中所列的化合物混合以形成本发明的组合物。所述要与PFBE混合的至少一种选自醇、卤代烃、氟烷基醚或氢氟烃的化合物不应是醇、单独的反式-1,2-二氯乙烯、单独的C4F9OCH3、单独的HFC-43-10mee、单独的HFC-365mfc、或反式-1,2-二氯乙烯与C4F9OC2H5的混合物。
表2
表2中所列的化合物可购自化学品供应公司。C4F9OCH3和C4F9OC2H5可购自3MTM(St.Paul,MN)。HFC-43-10mee可购自E.I.DuPont de Nemours & Co(Wilmington,DE)。HFC-365mfc可购自Solvay-Solexis。
本发明的组合物可以通过混合所需量的各个组分以任何方便的方法制备。优选方法为称量所需量的组分,然后在合适的容器中混合所述组分。如需要,可使用搅拌。
本发明的组合物包含共沸和类似共沸物的组合物,所述共沸和类似共沸物的组合物包括一种表1中所列的氟化烯烃、PEIK或PFBE和至少一种选自三氯乙烯、四氯乙烯、反式-1,2-二氯乙烯、正丙基溴、甲醇、乙醇、正丙醇、异丙醇、C4F9OCH3、C4F9OC2H5、HFC-43-10mee、HFC-365mfc及其组合的化合物。根据本发明的组合物,其例外在于,PFBE没有与醇、反式-1,2-二氯乙烯、单独的C4F9OCH3、单独的HFC-43-10mee、单独的HFC-365mfc、或反式-1,2-二氯乙烯与C4F9OC2H5的混合物相混合。
如本文所用,共沸组合物是两种或多种物质的恒沸液体混合物,其中所述混合物蒸馏而基本没有组成改变,并表现为恒沸组合物。与相同物质的非共沸混合物的沸点相比较,特征为共沸的恒沸组合物表现出或者最大或者最小的沸点。如本文所用的共沸组合物包括均相共沸物,其为表现为单种物质的两种或多种物质的液体混合物,即通过液体的部分蒸发或蒸馏产生的蒸汽具有与液体相同的组成。如本文所用的共沸组合物还包括非均相共沸物,其中液相分为两个或多个液相。在这些实施方案中,在共沸点,气相与两个液相达成平衡且所有三相具有不同的组成。如果混合非均相共沸物的两个平衡液相并且计算所有液相的组成,其将与气相的组成相同。
如本文所用,术语“类似共沸物组合物”有时还称为“近共沸组合物”,是指恒沸或基本上恒沸的表现为单种物质的两种或多种物质的液体混合物。表征类似共沸物组合物的一种方法在于,通过液体的部分蒸发或蒸馏产生的蒸汽具有与被蒸发或蒸馏的液体基本上相同的组成。即,所述混合物蒸馏/回流而基本上没有组成的改变。表征类似共沸物组合物的另一种方法在于,在特定的温度下,所述组合物的始沸点蒸汽压和所述组合物的露点蒸汽压基本上是相同的。在此,如果在50wt%的所述组合物通过例如蒸发或蒸馏去除后,原始组合物和在50wt%的原始组合物经蒸发或蒸馏去除后剩下的组合物之间的蒸汽压的差异小于10%,则组合物是类似共沸物。
在清洁装置,例如蒸汽脱脂器或脱焊药器中,清洁组合物在操作期间可能通过在轴封、软管连接、焊点和折线处的泄露发生部分损失。此外,在设备维护工序期间,工作组合物可能被释放到环境中。如果组合物不是纯化合物或共沸的或类似共沸物的组合物,则当从设备泄露或排出到环境中时组成可能改变,这可能导致装置中剩下的组合物变得易燃或显示出不能接受的性能。因此,在泄露或蒸发时可忽视程度分馏的单独的氟化烃或共沸的或类似共沸物的组合物用作清洁组合物是理想的。
本发明的一种实施方案的共沸组合物列于表3。
表3
组分A 组分B wt%A wt%B T(C)
F14E 甲醇 85.1 14.9 59.1
F14E 异丙醇 87.1 12.9 66.9
F14E 乙醇 87.9 12.1 65.2
F14E t-DCE 44.3 55.7 44.0
F14E nPBr 54.4 45.6 66.6
F24E 甲醇 72.1 27.9 63.4
F24E 异丙醇 78.1 21.9 74.1
F24E 乙醇 79.2 20.8 71.8
F24E t-DCE 24.5 75.5 45
F24E nPBr 25.7 74.3 70.2
F24E PCE 85.2 14.8 89.9
F24E TCE 65.0 35.0 75.9
PEIK 甲醇 97.0 3.0 43.5
PEIK 异丙醇 96.7 3.3 45.5
PEIK 乙醇 96.8 3.2 44.7
PEIK t-DCE 72.9 27.1 34.7
PEIK 43-10mee 73.2 26.8 47.7
PEIK 365mfc 38.8 61.2 38.1
PFBE 甲醇 92.2 7.8 50.6
PFBE 异丙醇 95.2 4.8 56.3
PFBE 乙醇 94.8 5.2 55.2
PFBE t-DCE 52.8 47.2 41.3
PFBE nPBr 82.3 17.7 57.1
F22E 甲醇 95.8 4.2 43.7
F22E 异丙醇 98.0 2.0 47.2
F22E 乙醇 97.6 2.4 46.6
F22E t-DCE 71.0 29.0 33.9
F22E nPBr 87.0 13.0 43.3
F22E 43-10mee 89.8 10.2 47.9
F22E 365mfc 29.3 70.7 39.2
F13iE 甲醇 95.5 4.5 44.4
F13iE 异丙醇 97.8 2.2 48.0
F13iE 乙醇 97.4 2.6 47.5
F13iE t-DCE 70.2 29.8 34.4
F13iE nPBr 86.4 13.6 44.0
F13iE 43-10mee 95.3 4.7 48.8
F13iE 365mfc 24.6 75.4 39.5
F3i3iE 甲醇 85.0 15.0 59.8
F3i3iE 异丙醇 89.2 10.8 70.0
F3i3iE 乙醇 89.0 11.0 67.8
F3i3iE t-DCE 44.1 55.9 44.5
F3i3iE C4F9OC2H5 22.8 77.2 75.7
F3i3iE nPBr 67.4 32.6 61.3
F13E 甲醇 94.4 5.6 47.3
F13E 异丙醇 96.9 3.1 51.9
F13E 乙醇 96.5 3.5 51.1
F13E t-DCE 66.3 33.7 36.3
F13E nPBr 83.7 16.3 47.1
F13E 43-10mee 59.5 40.5 52.3
F3i4E t-DCE 7.6 92.4 47.6
F3i4E 甲醇 42.8 57.2 65.4
F3i4E 异丙醇 57.8 42.2 81.0
F3i4E 乙醇 58.7 41.3 77.3
F3i4E nPBr 31.9 68.1 69.6
F44E nPBr 8.1 91.9 70.9
此外,在另一个实施方案中,本发明的共沸组合物还包括包含表2中的化合物的三元和四元共沸组合物。这些高级共聚组合物的非限制性的例子连同所述组合物在大气压下的沸点在表4中列举出。
表4
组分A 组分B 组分C wt%A wt%B wt%C T(C)
F14E t-DCE 甲醇 34.4 59.0 6.6 39.9
F14E t-DCE 乙醇 41.9 55.1 3.0 43.2
F24E t-DCE 甲醇 10.3 80.3 9.4 41.0
F24E t-DCE 乙醇 24.8 70.9 4.3 43.0
PEIK t-DCE 甲醇 71.5 26.4 2.1 33.0
PEIK t-DCE 乙醇 73.0 25.7 1.3 34.2
PEIK t-DCE 43-10mee 57.0 26.9 16.1 34.3
PEIK t-DCE 365mfc 43.7 24.1 32.2 32.6
PFBE t-DCE C4F9OCH3 40.1 47.5 12.4 41.3
F22E t-DCE 甲醇 67.9 29.7 2.4 32.6
F22E t-DCE 365mfc 45.4 27.2 27.4 33.0
F13iE t-DCE 甲醇 66.9 30.6 2.5 33.0
F13iE t-DCE 43-10mee 69.8 29.8 0.4 34.4
F13iE t-DCE 365mfc 41.9 27.8 30.3 33.3
F3i3iE t-DCE 甲醇 32.9 60.2 6.9 40.1
F3i3iE t-DCE 乙醇 41.1 56.3 2.6 43.8
F13E t-DCE 甲醇 62.2 34.7 3.1 34.5
F13E t-DCE 43-10mee 48.0 33.2 18.8 36.1
F13E t-DCE 365mfc 23.1 30.3 46.6 34.4
本发明的二元类似共沸物组合物列于表5。
表5
组分A 组分B wt%A wt%B T(C)
F14E 甲醇 60-99 1-40 59.1
F14E 异丙醇 70-99 1-30 66.9
F14E 乙醇 72-99 1-28 65.2
F14E t-DCE 1-75 25-99 44.0
F14E nPBr 1-99 1-99 66.6
F14E C4F9OCH3 1-99 1-99 50
F14E C4F9OC2H5 1-99 1-99 50
F14E 43-10mee 1-99 1-99 50
F24E 甲醇 1-91 9-99 63.4
F24E 异丙醇 57-91 9-43 74.1
F24E 乙醇 57-92 8-43 71.8
F24E t-DCE 1-63 37-99 46.1
F24E nPBr 1-70 30-99 70.2
F24E PCE 61-99 1-39 89.9
F24E TCE 40-84 16-60 75.9
F24E C4F9OC2H5 1-99 1-99 50
PEIK 甲醇 91-99 1-9 43.5
PEIK 异丙醇 57-99 1-16 45.5
PEIK 乙醇 85-99 1-15 44.7
PEIK t-DCE 50-88 12-50 34.7
PEIK 4310mcee 1-99 1-99 47.7
PEIK 365mfc 1-99 1-99 38.1
PEIK C4F9OCH3 1-99 1-99 50
PFBE 甲醇 80-99 1-20 50.6
PFBE 异丙醇 83-99 1-17 56.3
PFBE 乙醇 83-99 1-17 55.2
PFBE t-DCE 21-79 21-79 41.3
PFBE nPBr 44-99 1-55 57.1
PFBE C4F9OCH3 1-99 1-99 50
PFBE C4F9OC2H5 1-99 1-99 50
PFBE 43-10mee 1-99 1-99 50
PFBE 365mfc 1-99 1-99 50
F22E 甲醇 86-99 1-14 43.7
F22E 异丙醇 88-99 1-12 47.2
F22E 乙醇 88-99 1-12 46.6
F22E t-DCE 48-87 13-52 33.9
F22E nPBr 64-99 1-36 43.3
F22E 43-10mee 1-99 1-99 47.9
F22E 365mfc 1-99 1-99 39.2
F22E C4F9OCH3 1-99 1-99 50
F13iE 甲醇 86-99 1-14 44.4
F13iE 异丙醇 87-99 1-13 48.0
F13iE 乙醇 88-99 1-12 47.5
F13iE t-DCE 46-86 14-54 34.4
F13iE nPBr 64-99 1-36 44.0
F13iE 43-10mee 1-99 1-99 48.8
F13iE 365mfc 1-99 1-99 39.5
F13iE C4F9OCH3 1-99 1-99 50
F3i3iE 甲醇 57-99 1-43 59.8
F3i3iE 异丙醇 73-99 1-27 70.0
F3i3iE 乙醇 73-99 1-27 67.8
F3i3iE t-DCE 1-76 24-99 44.5
F3i3iE C4F9OC2H5 1-99 1-99 75.7
F3i3iE nPBr 43-86 14-57 61.3
F3i3iE C4F9OCH3 1-99 1-99 50
F13E 甲醇 84-99 1-16 47.3
F13E 异丙醇 86-99 1-14 51.9
F13E 乙醇 86-99 1-14 51.1
F13E t-DCE 42-84 16-58 36.3
F13E nPBr 61-99 1-39 47.1
F13E 43-10mee 1-99 1-99 52.3
F13E C4F9OCH3 1-99 1-99 50
F13E C4F9OC2H5 1-99 1-99 50
F13E 365mfc 1-99 1-99 50
F3i4E t-DCE 1-69 31-99 47.6
F3i4E 甲醇 1-89 11-99 654
F3i4E 异丙醇 1-88 12-99 81
F3i4E 乙醇 1-89 11-99 77.3
F3i4E nPBr 1-72 28-99 69.6
F44E nPBr 1-70 30-99 70.9
除了在前表中的二元类似共沸物组合物,本发明包括高级(三元或四元)类似共沸物组合物。三元或更高级类似共沸物组合物的非限制性例子在表6中给出。
表6
组分A 组分B 组分C wt%A wt%B wt%C T(C)
F14E t-DCE C4F9OCH3 1-70 20-70 1-70 50
F14E t-DCE C4F9OC2H5 1-70 29-90 1-60 50
F14E t-DCE 43-10mee 1-80 15-60 1-80 50
F14E t-DCE 365mfc 1-70 10-60 1-80 50
F14E t-DCE 甲醇 1-70 29-98 1-30 39.9
F14E t-DCE 乙醇 1-70 29-98 1-20 43.2
F24E t-DCE C4F9OCH3 1-70 20-70 1-70 50
F24E t-DCE C4F9OC2H5 1-60 30-80 1-60 50
F24E t-DCE 甲醇 1-50 40-98 1-25 41.0
F24E t-DCE 乙醇 1-60 39-98 1-20 45.0
PEIK t-DCE C4F9OCH3 1-70 20-50 1-70 50
PEIK t-DCE 甲醇 50-85 14-49 1-9 33.0
PEIK t-DCE 乙醇 50-85 14-49 1-9 34.2
PEIK t-DCE 43-10mee 1-85 10-65 1-80 34.3
PEIK t-DCE 365mfc 1-85 1-55 1-85 32.6
PFBE t-DCE 43-10mee 1-70 20-60 1-79 50
PFBE t-DCE 365mfc 1-70 15-60 1-80 50
PFBE t-DCE C4F9OCH3 1-75 24-75 1-70 41.3
F22E t-DCE C4F9OCH3 1-70 29-70 1-70 50
F22E t-DCE 43-10mee 1-80 19-60 1-80 50
F22E t-DCE 甲醇 45-85 14-54 1-10 32.6
F22E t-DCE 365mfc 1-89 10-60 1-85 33.0
F13iE t-DCE C4F9OCH3 1-75 24-70 1-70 50
F13iE t-DCE 甲醇 45-85 14-54 1-10 33.0
F13iE t-DCE 43-10mee 1-89 10-60 1-80 34.4
F13iE t-DCE 365mfc 1-89 10-60 1-84 33.3
F3i3iE t-DCE 甲醇 1-70 29-95 1-25 40.1
F3i3iE t-DCE 乙醇 1-65 34-98 1-15 43.8
F3i3iE t-DCE C4F9OCH3 1-69 30-70 1-69 50
F3i3iE t-DCE C4F9OC2H5 1-69 30-80 1-69 50
F13E t-DCE 甲醇 45-80 19-54 1-10 34.5
F13E t-DCE 43-10mee 1-85 14-60 1-80 36.1
F13E t-DCE 365mfc 1-85 14-60 1-80 34.4
F13E t-DCE C4F9OCH3 1-80 19-70 1-70 50
F3i4E t-DCE C4F9OCH3 1-30 25-69 30-69 50
F3i4E t-DCE C4F9OC2H5 1-50 30-98 1-60 50
F44E t-DCE C4F9OC2H5 1-70 1-60 29-98 50
在本发明的又一实施方案中,本发明的组合物可以进一步包括气溶胶喷射剂。气溶胶喷射剂可以帮助本发明的组合物从存储容器中以气溶胶形式运送至表面。气溶胶喷射剂可任选地以最高达到总组合物的25wt%包含于本发明组合物中。代表性的气溶胶喷射剂包括空气、氮气、二氧化碳、二氟甲烷(HFC-32,CH2F2)、三氟甲烷(HFC-23,CHF3)、二氟乙烷(HFC-152a,CHF2CH3)、三氟乙烷(HFC-143a,CH3CF3;或HFC-143,CHF2CH2F)、四氟乙烷(HFC-134a,CF3CH2F;HFC-134,CHF2CHF2)、五氟乙烷(HFC-125,CF3CHF2)、七氟丙烷(HFC-227ea,CF3CHFCF3)、五氟丙烷(HFC-245fa,CF3CH2CHF2)、二甲醚(CH3OCH3)或其混合物。
在本发明的一个实施方案中,本发明的共沸组合物是有效的清洁剂、去焊药剂和脱脂剂。特别地,在去除具有部件如倒装片、μBGA(球栅阵列)及芯片级(Chip scale)或其它高级高密度封装部件的电路板的焊药时,本发明的共沸组合物是有用的。倒装片、μBGA及芯片级是描述用于半导体工业的高密度封装部件的术语并为本领域技术人员所熟知。
在另一实施方案中本发明涉及用于从表面或基片去除残留物的方法,包括:使表面或基片与本发明的组合物接触并从组合物中回收所述表面或基片。
在本发明的方法实施方案中,表面或基片可以是集成电路器件,在此情况下,所述残留物包含松香焊药或油。所述集成电路器件可以是具有各种类型部件例如倒装片、μBGA或芯片级封装部件的电路板。此外,所述表面或基片可以是例如不锈钢的金属表面。所述松香焊药可以是通常用于集成电路器件焊接的任何类型,包括但不限于RMA(温和活化松香)、RA(活化松香)、WS(水溶性)、OA(有机酸)。油残留物包括但不限于矿物油、机油和硅油。
在本发明方法中,用于接触表面或基片的方法并不是关键的,并可以通过下述方法实现:将所述器件浸入于包含所述组合物的浴槽中,以所述组合物喷射所述器件或以已经用所述组合物润湿的基片擦拭所述器件。可选择地,所述组合物还可以在为去除这种残留物而设计的蒸汽脱脂或脱焊药装置中使用。此种蒸汽脱脂或脱焊药装置可购自各供应商,例如其中的Forward Technology(Crest Group的子公司,Trenton,NJ)、Trek Industries(Azusa,CA)和Ultronix,Inc.(Hatfield,PA)。
用于从表面去除残留物的有效组合物具有的贝壳杉脂丁醇值(Kb)为至少约10,优选约40,更优选约100。给定组合物的贝壳杉脂丁醇值(Kb)反映所述组合物溶解各种有机残留物(例如机器和常规制冷润滑油)的能力。所述Kb值可以通过ASTM D-1133-94测定。
下面的具体实施例仅欲举例说明本发明,并不意于以任何方式进行限制。
实施例
实施例1
1,1,1,4,4,5,5,6,6,7,7,7-十二氟庚-2-烯(F14E)的合成
C4F9CH2CHICF3的合成
在400ml的HastelloyTM振荡管中加入全氟正丁基碘(180.1gm,0.52mol)和3,3,3-三氟丙烯(25.0gm,0.26mol),并且在增大到最大值428PSI的自生压力下加热至200℃8小时。将反应容器冷却至室温后,收集产物。混合并蒸馏此反应的产物和以除反应之一具有两倍量的反应物外基本上相同的方法进行反应所得的两种其它产物,以提供322.4gm的C4F9CH2CHICF3(52.2℃/35mm,70%产率)。
C4F9CH2CHICF3至F14E的转化
将异丙醇(95ml)、KOH(303.7gm,0.54mol)和水(303ml)装入装配有搅拌棒和填充蒸馏柱及蒸馏头的2升圆底烧瓶中。在室温下通过加料漏斗滴加C4F9CH2CHICF3(322.4gm,0.73mol)至KOH/IPA水溶液混合物中。然后,反应加热到65-70℃以通过蒸馏回收产物。收集蒸馏物,以偏亚硫酸氢钠和水洗涤,经MgSO4干燥,接着通过填充有玻璃螺旋管的6-英寸(15.2cm)柱蒸馏。产物F14E(173.4gm,76%产率)在78.2℃沸腾。通过NMR谱表征产物(19F:δ-66.7(CF3,m,3F),-81.7(CF3,m,3F),-124.8(CF2,m,2F),-126.4(CF2,m,2F),-114.9ppm(CF2,m,2F);1H:6.58d)。
实施例2
1,1,1,2,2,5,5,6,6,7,7,8,8,8-十四氟辛-3-烯(F24E)的合成
C4F9CHICH2C2F5的合成
在400ml的HastelloyTM振荡管中加入全氟乙基碘(220gm,0.895mol)和3,3,4,4,5,5,6,6,6-九氟己-1-烯(123gm,0.50mol),并且在自生压力下加热至200℃10小时。将此反应的产物和在基本上相似条件下进行反应所得的两种其它产物混合并以两个200mL份的10wt%亚硫酸氢钠水溶液洗涤。经氯化钙干燥有机相,接着蒸馏以提供产率为37%的277.4gm的C4F9CH2CHICF3(79-81℃/67-68mm Hg)。
C4F9CHICH2C2F5至F24E的转化
将C4F9CHICH2C2F5(277.4gm,0.56mol)和异丙醇(217.8g)装入装配有机械搅拌器、加料漏斗、冷凝器和热电偶的1升圆底烧瓶中。该加料漏斗装有溶解在83.8g水中的氢氧化钾溶液(74.5g,1.13mol)。在经过温度从21℃缓慢升高至42℃的约1小时的过程中,KOH溶液被滴加入烧瓶中并伴有快速搅拌。以水稀释反应物料,通过相分离回收产物。以50mL份的10wt%亚硫酸氢钠水溶液和水洗涤产物,经氯化钙干燥,然后在大气压下蒸馏。产物F24E(128.7gm,63%)在95.5℃沸腾,并通过NMR表征(19F:δ-81.6(CF3,m,3F),-85.4(CF3,m,3F),-114.7(CF2,m,2F),-118.1(CF2,m,2F),-124.8ppm(CF2,m,2F),-126.3ppm(CF2,m,2F);1H:δ6.48;氯仿-d溶液)。
实施例3
1,1,1,4,5,5,5-七氟-4-(三氟甲基)-戊-2-烯(F13iE)的合成
CF3CHICH2CF(CF3)2的合成
在400ml的HastelloyTM振荡管中加入(CF3)2CFI(265gm,0.9mol)和3,3,3-三氟丙烯(44.0gm,0.45mol),并且在增大到最大值585psi的自生压力下加热至200℃8小时。在室温下收集产物以提供产率为62%的110gm的(CF3)2CFCH2CHICF3(76-77℃/200mm)。
(CF3)2CFCH2CHICF3至F13iE的转化
将异丙醇(50ml)、KOH(109gm,1.96mol)和水(109ml)装入装配有搅拌棒并连接至短路蒸馏柱及干冰阱的500ml圆底烧瓶中。将混合物加热到42℃并通过加料漏斗滴加(CF3)2CFCH2CHICF3(109gm,0.28mol)。在添加过程中,温度自42℃升高至55℃。在回流30分钟后,***温度升高至62℃,并通过蒸馏收集产物。收集产物,以水洗涤,经MgSO4干燥并蒸馏。产物F13iE(41gm,55%产率)在48-50℃沸腾,并通过NMR表征(19F:δ-187.6(CF,m,1F),-77.1(CF3,m,6F),-66.3(CF3,m,3F);氯仿-d溶液)。
实施例4
C4F9CHICH2C2F5的合成
在210ml的HastelloyTM振荡管中加入3,3,4,4,5,5,6,6,6-九氟己-1-烯(20.5gm,0.0833mol)、双(三苯基膦)镍(0)二羰基(0.53g,0.0008mol)和全氟乙基碘(153.6gm,0.625mol)并且在自生压力下在100℃加热8小时。通过GC-MS的产物分析表明了C4F9CHICH2C2F5(64.3GC面积%)和二元加合物(3.3GC面积%)的存在;3,3,4,4,5,5,6,6,6-九氟己-1-烯的转化率为80.1%。
实施例5
去焊药
本发明的组合物对于从表面清洁离子污染(焊药)是有效的。用于确定表面清洁度的测试包括以下步骤:
1.在FR-4测试板(带有由镀锡铜制成的示踪的环氧印刷线路板)上大量涂刷松香焊药。
2.接着在约175℃的烘箱中加热这样处理的板约1-2分钟以活化松香焊药。
3.然后在约200℃将所述板浸入焊药(Sn63,63/37 Sn/铅焊药)约10秒。
4.然后通过浸入沸腾清洁组合物中约3分钟并且轻微移动所述板而清洁所述板。接着,将所述板浸入新制备的、室温下的清洁组合物浴中以清洗约2分钟。
5.然后用Omega Meter 600 SMD离子分析仪测试所述板的残留离子。
通过在沉积焊药前、沉积焊药后和接着在清洁步骤后称量所述板测定清洁性能。结果在表7中给出。
表7
实施例6
金属清洁
对经过喷砂以提供粗糙表面的不锈钢(316型)2″×3″试样进行预清洁并烘箱烘干以去除任何残留污物。每个试样的皮重测定为0.1mg。以棉签涂覆少量矿物油,然后再次称量试样以得到“加载的”重量。然后,通过浸入沸腾清洁组合物中1分钟清洁该试样,在蒸汽中停留30秒,然后风干1分钟。接着,再次对试样称重并使用三个记录的重量计算污物去除百分比。结果示于表8。
表8
结果显示通过本发明的组合物从不锈钢表面有效去除了矿物油残留物。
实施例7
金属清洁
对经过喷砂以提供粗糙表面的不锈钢(316型)2″×3″试样进行预清洁并烘箱烘干以去除任何残留污物。每个试样的皮重测定为0.1mg。以棉签涂覆少量DC200硅氧烷,然后再次称量试样以得到“加载的”重量。然后,通过浸入沸腾清洁组合物中1分钟清洁该试样,在蒸汽中停留30秒,然后风干1分钟。接着,再次对试样称重并使用三个记录的重量计算污物去除百分比。结果示于表9。
表9
结果显示通过本发明的组合物从不锈钢表面有效去除了硅氧烷残留物。
实施例8
金属清洁效力
对经过喷砂以提供粗糙表面的不锈钢(316型)2″×3″试样进行预清洁并烘箱烘干以去除任何残留污物。每个试样被称量4个位置以获得皮重。以棉签涂覆少量矿物油,然后再次称量试样以得到“加载的”重量。然后,通过浸入沸腾清洁组合物中1分钟清洁该试样,在蒸汽中停留30秒,然后风干1分钟。接着,再次对试样称重并使用三个记录的重量计算污物去除百分比。结果示于表10。
表10
结果显示通过本发明的组合物从不锈钢表面有效去除了矿物油残留物。
结果显示通过本发明的组合物从不锈钢表面有效去除了硅氧烷残留物。
Claims (10)
1.组合物,包含全氟-1-己烯(3,3,4,4,5,5,6,6,6-九氟-1-己烯(PFBE))和至少一种选自卤代烃、氟烷基醚和氢氟烃的化合物,其中所述至少一种化合物不是单独的反式-1,2-二氯乙烯、单独的C4F9OCH3、单独的HFC-43-10mee、单独的HFC-365mfc、或反式-1,2-二氯乙烯与C4F9OC2H5的混合物。
2.如权利要求1所述的组合物,其中所述组合物是共沸或类似共沸物的组合物,包含全氟-1-己烯(3,3,4,4,5,5,6,6,6-九氟-1-己烯(PFBE))和至少一种选自卤代烃、氟烷基醚和氢氟烃的化合物,其中所述至少一种化合物不是单独的反式-1,2-二氯乙烯、单独的C4F9OCH3、单独的HFC-43-10mee、单独的HFC-365mfc、或反式-1,2-二氯乙烯与C4F9OC2H5的混合物。
3.如权利要求2所述的共沸或类似共沸物的组合物,其中所述至少一种选自卤代烃和氟烷基醚的化合物是反式-1,2-二氯乙烯、三氯乙烯、四氯乙烯、正丙基溴、C4F9OCH3、C4F9OC2H5、HFC-43-10mee、HFC-365mfc或其组合。
4.如权利要求2所述的共沸或类似共沸物的组合物,其中所述共沸或类似共沸物的组合物选自以下:
约44-约99wt%的PFBE和约55-约1wt%的正丙基溴;
约1-约99wt%的PFBE和约99-约1wt%的C4F9OC2H5;
约1-约70wt%的PFBE,约20-约60wt%的反式-1,2-二氯乙烯和约1-约79wt%的HFC-43-10mee;
约1-约75wt%的PFBE,约24-约75wt%的反式-1,2-二氯乙烯和约1-约70wt%的C4F9OCH3;和
约1-约70wt%的HFC-PFBE,约15-约60wt%的反式-1,2-二氯乙烯和约1-约80wt%的HFC-365mfc。
5.如权利要求2所述的共沸或类似共沸物的组合物,其中所述共沸或类似共沸物的组合物为选自以下的共沸组合物:
在约57.1℃温度下具有约14.7psia(101kPa)蒸汽压的82.3wt%的PFBE和17.7wt%的正丙基溴;和
在约41.3℃温度下具有约14.7psia(101kPa)蒸汽压的40.1wt%的PFBE、47.5wt%的反式-1,2-二氯乙烯和12.4wt%的C4F9OCH3。
6.用于清洁的方法,包括:
a)使包含残留物的表面与权利要求1的组合物接触,并
b)从组合物中回收所述表面。
7.权利要求6的方法,其中所述残留物包含油。
8.权利要求6的方法,其中所述残留物包含松香焊药。
9.权利要求6的方法,其中所述表面是集成电路器件。
10.权利要求1的组合物,还包含气溶胶喷射剂。
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