CN106133010B - 粘合剂组合物 - Google Patents
粘合剂组合物 Download PDFInfo
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- CN106133010B CN106133010B CN201580015175.2A CN201580015175A CN106133010B CN 106133010 B CN106133010 B CN 106133010B CN 201580015175 A CN201580015175 A CN 201580015175A CN 106133010 B CN106133010 B CN 106133010B
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本文公开了一种特征在于固化后具有低的VOC排放的粘合剂组合物,其包含作为主要组分的至少一种分散聚合物P和至少一种矿物粘合剂M,所述分散聚合物P的玻璃化转变温度≤20℃并包含共聚形式的丙烯酸乙酯。
Description
本发明涉及粘合剂组合物,其包含以下物质作为主要组分:
a)至少一种分散聚合物P,其玻璃化转变温度≤20℃并包含共聚形式的丙烯酸乙酯,和
b)至少一种矿物粘合剂M,其含量为≥1重量份且≤10 000重量份每100重量份分散聚合物P。
本发明还涉及用上述粘合剂组合物涂覆基材的方法,并且还涉及经涂覆的基材本身。
用于本发明目的的矿物粘合剂M为粉末形式的无机粘合剂,其在与水接触后,并且在自身被置于大气条件下的空气中或在水下的其他一些情况中时,能够进行随时间变化的岩石状(stonelike)固化。本领域技术人员所熟知的这种矿物粘合剂M为,如煅石灰、石膏、炉渣砂、粉煤灰、硅尘、偏高岭土、天然火山灰或煅油页岩(burnt oil shales),以及,特别是水泥(在这方面,参见,例如,EN 197-1),如波特兰水泥、白水泥、Thurament、Celitement、高铝水泥、膨胀水泥、高炉水泥,以及与下述物质混合的水泥:例如,炉渣砂、粉煤灰、硅尘、偏高岭土、天然火山灰或煅油页岩混合。
通过与水接触和混合使得矿物粘合剂M——通常也与作为集料的砂、砾石或碎石以及其他常规填料或添加剂混合——转化为它们的即用(ready-to-use)形式,例如称作砂浆或混凝土(下文中称为“水硬性粘合剂配制料”),然后以常规方式对其进行处理。
为了改善用于加工的水硬性粘合剂配制料的机械特性或由它们获得的固化或硬化材料的机械特性(实例为弯拉强度、基材粘附力、柔性等),将水硬性粘合剂配制料与细碎的聚合物(数均粒径≥10且≤1000nm)混合,所述细碎的聚合物为水性聚合物分散体的形式或可由它们(分散聚合物)获得的聚合物粉末的形式(参见,例如,DE-AS 1669903、DE-A2837898、DE-A 4206429、DE-A 4217035、DE-A 4317036、DE-A 4320220、US-A 3043790、US-A3196122、DE-A 3220384、US-A 3239479、US-A 3232899、US-A 4225496、US-A 4340510、BE-A8454499、GB-PS 1505558、JP-A 54/43285、JP-A 91/131533、EP-A 537411、EP-A 770639或EP-A 812872)。
尽管从待处理的水硬性粘合剂配制料的机械特性,以及由它们获得的固化或硬化材料的机械特性来看,要求通常得以充分满足,但是所获得的固化或硬化材料并不总是能够充分满足关于排放挥发性有机化合物(简称为VOCs)的要求,尤其在使用基于丙烯酸烷基酯和/或甲基丙烯酸烷基酯的分散聚合物时。对于这类固化或硬化材料的分级由用于控制地板安装、粘合剂和建筑材料产品中排放的协会(Association for the Control ofEmissions in Products for Floor Installation,Adhesives and BuildingMaterials)(GEV)在1997年引入,其中用于“非常低VOCs”的质量标志EC1以GEV给予那些在3天后表现出≤1000μg/m3的总VOC且28天后表现出≤100μg/m3的总VOC的固化或硬化材料。迄今为止,并没有公开基于矿物粘合剂(更具体为水泥)且基于包含丙烯酸烷基酯和/或甲基丙烯酸烷基酯的分散聚合物的任何矿物防水配制料(称为矿物防水浆料),所述矿物防水配制料的硬化防水涂层满足EC1质量分级所要求的低VOC排放水平。
因此,本发明的目的为提供粘合剂组合物,其基于矿物粘合剂(尤其是水泥),并且基于包含丙烯酸烷基酯和/或甲基丙烯酸烷基酯的分散聚合物,通过与水反应,所述粘合剂组合物材料的硬化或固化表现出极低的VOC排放,尤其是符合GEV
这一目的已由开始时定义的粘合剂组合物实现。
所述粘合剂组合物的主要成分为分散聚合物P,其玻璃化转变温度≤20℃并包含共聚形式的丙烯酸乙酯。
用于本说明书目的的分散聚合物P为细碎的聚合物,其数均粒径≥10且≤1000nm,其形式为水性聚合物分散体或可由所述水性聚合物分散体获得的聚合物粉末。
特别有利地,用于本发明粘合剂组合物的分散聚合物P包含共聚形式的以下物质:
并且单体A至G的量合计达100重量%。
只使用丙烯酸乙酯作为单体A。
本发明的分散聚合物P有利地包含≥35且≤65重量%,尤其有利地≥40且≤55重量%,且特别有利地≥40且≤50重量%的共聚形式的丙烯酸乙酯。
作为单体B,可以考虑所有的单烯键式不饱和化合物,其具有至少一个含硅基团、一个环氧基、N-羟甲基或羰基基团。
作为单体B,可以考虑所有的具有至少一个含硅基团的单烯键式不饱和化合物。特别有利地,含有硅基团的单体B具有可水解的含硅基团。可水解的含硅基团有利地包含至少一个烷氧基团或一个卤素原子,例如氯。根据本发明可有利地使用的单体B公开于WO 2008/150647,第9页,第5至25行。通过引用其表述,这些含硅基团的单体B被视为本说明书的一部分。然而,特别有利地,含有硅基团的单体B选自乙烯基三乙酰氧基硅烷、3-甲基丙烯酰基氧基丙基三甲基硅烷和乙烯基三乙氧基硅烷。
作为单体B,还可以考虑所有的具有至少一个环氧基团的单烯键式不饱和化合物,例如,如丙烯酸缩水甘油酯和/或甲基丙烯酸缩水甘油酯,特别优选甲基丙烯酸缩水甘油酯。
作为单体B,还可以考虑所有的具有至少一个N-羟甲基基团的单烯键式不饱和化合物,如基于α,β-单烯键式不饱和C3至C6单羧酸酰胺或二羧酸酰胺的N-羟甲基酰胺化合物,尤其是,如N-羟甲基丙烯酰胺和/或N-羟甲基甲基丙烯酰胺。
作为单体B,也可以考虑所有的具有至少一个羰基基团的单烯键式不饱和化合物,如乙烯基羰基化合物,如苯基乙烯基酮;或例如二羰基化合物,如二丙酮丙烯酰胺以及尤其是丙烯酸乙酰基乙酰氧基乙酯和甲基丙烯酸乙酰基乙酰氧基乙酯。
特别有利地,作为单体B,使用乙烯基三乙酰氧基硅烷、3-甲基丙烯酰基氧基丙基三甲基硅烷、乙烯基三乙氧基硅烷、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、苯基乙烯基酮、二丙酮丙烯酰胺、丙烯酸乙酰基乙酰氧基乙酯和/或甲基丙烯酸乙酰基乙酰氧基乙酯,尤其优选甲基丙烯酸缩水甘油酯。
本发明的分散聚合物P有利地包含≥0且≤5重量%,尤其有利地≥0.5且≤4重量%,且特别有利地≥1且≤3重量%的共聚形式的单体B。
作为单体C,可以考虑所有的具有至少一个羟烷基基团的单烯键式不饱和化合物。
作为单体C,有利地是,可以考虑丙烯酸羟基-C2-C10-烷基酯和/或甲基丙烯酸羟基-C2-C10-烷基酯,优选丙烯酸羟基-C2-C4-烷基酯和/或甲基丙烯酸羟基-C2-C4-烷基酯,且特别有利地是丙烯酸羟基-C2-C3-烷基酯和/或甲基丙烯酸羟基-C2-C3-烷基酯,并且对于本说明书的目的,烷氧基化丙烯酸羟烷基酯和/或甲基丙烯酸羟烷基酯,即与环氧烷(主要是环氧乙烷和环氧丙烷)反应的那些,也被视为单体C。有利地,含羟烷基基团的单体C选自单丙烯酸二乙二醇酯、丙烯酸4-羟丁酯、丙烯酸3-羟丙酯、丙烯酸2-羟丙酯、丙烯酸2-羟乙酯、单甲基丙烯酸二乙二醇酯、甲基丙烯酸4-羟丁酯、甲基丙烯酸3-羟丙酯、甲基丙烯酸2-羟丙酯和甲基丙烯酸2-羟乙酯。尤其优选丙烯酸2-羟乙酯和/或甲基丙烯酸2-羟乙酯,特别优选甲基丙烯酸2-羟乙酯。
本发明的分散聚合物P有利地包含≥0且≤7重量%,尤其有利地≥1且≤6重量%,且特别有利地≥2且≤5重量%的共聚形式的单体C。
作为单体D,可以考虑所有的单烯键式不饱和C3至C6一元羧酸和/或C4-C6二羧酸。
作为单体D,有利地是,可以考虑丙烯酸、甲基丙烯酸、乙基丙烯酸、衣康酸、烯丙基乙酸、巴豆酸、乙烯基乙酸、富马酸、马来酸或2-甲基马来酸。然而,单体D还包括相应α,β-单烯键式不饱和二羧酸的酸酐,如马来酸酐或2-甲基马来酸酐。单体D优选地选自丙烯酸、甲基丙烯酸、巴豆酸、富马酸、马来酸、马来酸酐、2-甲基马来酸和衣康酸,特别优选丙烯酸和/或甲基丙烯酸。当然,单体D还包括完全或部分中和的水溶性盐,尤其是上述酸的碱金属盐。
本发明的分散聚合物P有利地包含≥0且≤5重量%,尤其有利地≥0.1且≤3重量%,且特别有利地≥0.1且≤2重量%的聚合形式的单体D。
作为单体E,可以考虑所有的具有至少两个非共轭烯键式不饱和基团(例如尤其是乙烯基、亚乙烯基或烯基基团)的化合物。
作为单体E,特别有利的是二元醇与α,β-单烯键式不饱和一元羧酸(优选丙烯酸和甲基丙烯酸)的二酯。这类具有两个非共轭烯键式不饱和双键的单体的实例为二丙烯酸亚烷基二醇酯和二甲基丙烯酸亚烷基二醇酯,如二丙烯酸乙二醇酯、二丙烯酸1,2-丙二醇酯、二丙烯酸1,3-丙二醇酯、二丙烯酸1,3-丁二醇酯、二丙烯酸1,4-丁二醇酯和二甲基丙烯酸乙二醇酯、二甲基丙烯酸1,2-丙二醇酯、二甲基丙烯酸1,3-丙二醇酯、二甲基丙烯酸1,3-丁二醇酯、二甲基丙烯酸1,4-丁二醇酯;三元醇与α,β-单烯键式不饱和一元羧酸的三酯,如三丙烯酸甘油酯、三甲基丙烯酸甘油酯、三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯,以及二乙烯基苯、甲基丙烯酸乙烯酯、丙烯酸乙烯酯、甲基丙烯酸烯丙酯、丙烯酸烯丙酯、马来酸二烯丙酯、富马酸二烯丙酯、亚甲基双丙烯酰胺、丙烯酸环戊二烯酯、氰脲酸三烯丙酯或异氰脲酸三烯丙酯。尤其优选二丙烯酸1,4-丁二醇酯、甲基丙烯酸烯丙酯和/或二乙烯基苯,其中对于本说明书的目的,二乙烯基苯应理解为意指1,2-二乙烯基苯、1,3-二乙烯基苯和/或1,4-二乙烯基苯。
本发明的分散聚合物P有利地包含≥0且≤5重量%,尤其有利地≥0且≤3重量%,且特别有利地≥0且≤2重量%的共聚形式的单体E。尤其有利地,所述分散聚合物P包含≤1重量%的共聚形式的单体E或根本不包含共聚形式的单体E。
作为单体F,可以考虑所有的烯键式不饱和化合物,其不同于单体A至E但可与单体A至E共聚,并且为此,仅仅由各个以共聚形式的单体F所合成的均聚物的玻璃化转变温度在≤30℃范围内。
单体F的实例为共轭的脂族C4至C9二烯化合物、乙烯醇和C1至C10一元羧酸的酯、丙烯酸C1至C10烷基酯、甲基丙烯酸C5至C10烷基酯、丙烯酸C5至C10环烷基酯和甲基丙烯酸C5至C10环烷基酯、马来酸C1至C10二烷基酯和/或富马酸C1至C10二烷基酯、C3至C10烷醇的乙烯基醚、以及支化和未支化的C3至C10烯烃。有利的单体F为其均聚物的玻璃化转变温度Tg≤0℃且尤其有利地≤-10℃的那些。
在本说明书的上下文中,C1至C10烷基基团为具有1至10个碳原子的直链或支链烷基基团,实例为甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、正戊基、异戊基、叔戊基、正己基、2-乙基-己基、正壬基或正癸基。C5至C10环烷基基团优选为环戊基或环己基基团,其可任选地被1、2或3个C1至C4烷基基团取代。
尤其适合作为单体F的是乙酸乙烯酯、丙烯酸甲酯、丙烯酸正丙酯、丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸仲丁酯、丙烯酸异丁酯、丙烯酸正己酯、甲基丙烯酸正辛酯、丙烯酸2-乙基己酯、甲基丙烯酸正己酯、甲基丙烯酸2-乙基己酯、丙烯酸2-丙基庚酯、丙烯酸异癸酯、丙烯酸正十二烷酯、甲基丙烯酸正十二烷酯、丙烯酸苄酯、丙烯酸乙基二甘醇酯、马来酸二正丁酯和/或富马酸二正丁酯,尤其优选丙烯酸甲酯、丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸仲丁酯、丙烯酸异丁酯、丙烯酸正己酯、甲基丙烯酸正己酯、甲基丙烯酸正辛酯、丙烯酸2-乙基己酯、甲基丙烯酸2-乙基己酯、丙烯酸2-丙基庚酯、丙烯酸异癸酯、丙烯酸正十二烷酯、甲基丙烯酸正十二烷酯、丙烯酸苄酯和丙烯酸乙基二甘醇酯,但特别有利地是丙烯酸2-乙基己酯。
本发明的分散聚合物P有利地包含≥15且≤45重量%,尤其有利地≥20且≤35重量%,且特别有利地≥25且≤30重量%的共聚形式的单体F。
作为单体G,可以考虑所有的烯键式不饱和化合物,其不同于单体A至E但可与单体A至E共聚,并且为此仅仅由各个以共聚形式的单体G所合成的均聚物的玻璃化转变温度在≥50℃范围内。有利的单体G为其均聚物的玻璃化转变温度Tg≥80℃且尤其有利地≥100℃的那些。
单体G的实例为乙烯基芳族单体、甲基丙烯酸C2至C4烷基酯和烯键式不饱和腈化合物。乙烯基芳族单体应理解为包括,特别是其中苯环任选地被1、2或3个取代基取代的苯乙烯或α-甲基苯乙烯衍生物,所述取代基为C1至C4烷基基团、卤素,尤其是溴或氯,和/或甲氧基基团。所述烯键式不饱和腈化合物主要为衍生自上述α,β-单烯键式不饱和一元羧酸或二羧酸,尤其是C3至C6一元羧酸或二羧酸,优选C3或C4一元羧酸或二羧酸的腈类,例如,丙烯腈、甲基丙烯腈、顺丁烯二腈和/或反丁烯二腈,特别优选丙烯腈和/或甲基丙烯腈。特别优选这类单体为苯乙烯、2-甲基苯乙烯、3-甲基苯乙烯、4-甲基苯乙烯、2,4-二甲基苯乙烯、2,5-二甲基苯乙烯和3,5-二甲基苯乙烯、对乙酰氧基苯乙烯、对溴苯乙烯、对叔丁基苯乙烯、邻氯苯乙烯、间氯苯乙烯或对氯苯乙烯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸异丙酯、丙烯酸叔丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸异丁酯、丙烯酸正己酯、甲基丙烯酸环己酯、丙烯腈、甲基丙烯腈、还有叔丁基乙烯基醚或环己基乙烯基醚,但尤其优选甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸异丙酯、丙烯酸叔丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸苯酯、甲基丙烯酸环己酯、苯乙烯、3-甲基苯乙烯、4-甲基苯乙烯、2,4-二甲基苯乙烯、2,5-二甲基苯乙烯和3,5-二甲基苯乙烯。已发现使用苯乙烯特别有利。
本发明的分散聚合物P有利地包含≥10且≤30重量%,尤其有利地≥15且≤30重量%,且特别有利地≥15且≤25重量%的共聚形式的单体F。
在一个优选的实施方案中,根据本发明使用的分散聚合物P包含共聚形式的以下物质:
且在一个特别优选的形式中,
在一个有利的实施方案中,所述分散聚合物P包含共聚形式的
在一个特别有利的实施方案中,所述分散聚合物P包含共聚形式的
然而,必不可少的是分散聚合物P的玻璃化转变温度Tg在≤20℃范围内且有利地≤5℃。
根据本发明,分散聚合物P和矿物粘合剂M一起用于粘合剂组合物中。因此,如果分散聚合物P将要用于柔性矿物防水浆料(grouts),则有利的是选择分散聚合物P使得它们的玻璃化转变温度Tg在≥-40且≤5℃范围内,有利地在≥-20且≤5℃范围内,且尤其有利地在≥-15且≤0℃范围内。与之相比,如果分散聚合物P将要用于矿物修补砂浆(repairmortars),则有利的是选择分散聚合物P使得它们的玻璃化转变温度Tg在≥-10且≤20℃范围内,有利地在≥0且≤20℃范围内,且尤其有利地在≥5且≤15℃范围内。然而,如果分散聚合物P将要用于矿物灰泥(plasters),则有利的是选择分散聚合物P使得它们的玻璃化转变温度Tg在≥-10且≤20℃范围内,有利地在≥-5且≤10℃范围内,且尤其有利地在≥-5且≤5℃范围内。因此,根据本发明使用的分散聚合物P包含共聚形式的单体A至G,其种类和量使得聚合物具有上述的玻璃化转变温度Tg。
根据Fox(T.G.Fox,Bull.Am.Phys.Soc.1956[Ser.II]1,第123页并且根据Ullmann’sder technischen Chemie,第19卷,第18页,第4版,VerlagChemie,Weinheim,1980),具有不超过低水平交联的共聚物的玻璃化转变温度在良好的近似下通过下式给出:
1/Tg=x1/Tg1+x2/Tg2+....xn/Tgn,
其中x1、x2、....xn为单体1、2、....n的质量分数并且Tg1、Tg2、....Tgn为仅由单体1、2、....n中的一种所形成的各自聚合物的玻璃化转变温度,以开尔文温度计。这些大多数烯键式不饱和单体的均聚物的玻璃化转变温度是已知的(或可以本身已知的简单方式用实验方法确定)并且列于例如J.Brandrup,E.H.Immergut,Polymer Handbook第一版;J.Wiley,New York,1966,第二版;J.Wiley,New York,1975,第三版;J.Wiley,New York,1989;以及Ullmann′s Encyclopedia of Industrial Chemistry,第169页,VerlagChemie,Weinheim,1992中。
然而,在本说明书的上下文中,玻璃化转变温度的Tg的数字涉及到通过来自Mettler-Toledo的DSC 822仪器(系列TA 8000)按照DSC方法(差示扫描量热法,20K/min,中点测量,DIN 53765)测得的玻璃化转变温度。
所述分散聚合物P的制备原则上是本领域技术人员所熟知的,并且通过下述方法完成:例如通过单体A至G的自由基聚合按照本体聚合法、乳液聚合法、溶液聚合法、沉淀聚合法或悬浮聚合法,但是,尤其优选自由基引发的水性乳液聚合。
于水性介质中实施自由基引发的烯键式不饱和单体的乳液聚合在之前已被多次记载,因此对于本领域技术人员而言是充分熟知的[在这方面,参见Emulsionpolymerization in Encyclopedia of Polymer Science and Engineering,第8卷,第659页起(1987);D.C.Blackley,in High Polymer Latices,第1卷,第35页起(1966);H.Warson,The Applications of Synthetic Resin Emulsions,第5章,第246页起(1972);D.Diederich,Chemie in unserer Zeit 24,第135至142页(1990);EmulsionPolymerization,Interscience Publishers,New York(1965);DE-A 40 03 422;和Dispersionen synthetischer Hochpolymerer,F.Springer-Verlag,Berlin(1969)]。自由基引发的水性乳液聚合通常使得烯键式不饱和单体分散于水性介质中(通常额外地使用分散助剂),并且通过至少一种水溶性自由基聚合引发剂聚合而进行,所述分散助剂如乳化剂和/或保护胶体。通过同样为本领域技术人员已知的化学和/或物理方法,在合成的水性聚合物分散体中,未反应的烯键式不饱和单体的残留水平得以特别有利地降低[参见例如EP-A 771328、DE-A 19624299、DE-A 19621027、DE-A 19741184、DE-A 19741187、DE-A 19805122、DE-A 19828183、DE-A 19839199、DE-A 19840586和19847115];通过稀释或浓缩、或者将其他常规助剂添加到水性聚合物分散体,而使聚合物固体含量调节至所需的水平,所述常规助剂如杀菌剂、泡沫改性添加剂或粘度改性添加剂。分散聚合物P的水性分散体的制备与这类通用方法的区别仅在于特定使用了上述的单体A至G。此处这是显然的,关于本说明书的上下文中分散聚合物P的制备,还旨在也包括为本领域技术人员所熟知的晶种操作模式、分级操作模式和梯度操作模式。
因此,在本说明书的上下文中,用于制备分散聚合物P的单体A至G的量旨在对应以共聚形式存在于分散聚合物P中的单体A至G的量。
对于制备本发明的或根据本发明使用的分散聚合物P,以其水性聚合物分散体的形式(分散聚合物P分散体),可在引发聚合反应之前,将全部量的单体A至G(全部单体量)作为初始进料引入到水性反应介质中。然而,也可在引发聚合反应前,任选地仅将一部分单体A至G作为初始进料引入到水性反应介质中,然后,在引发聚合后,在聚合条件下,于自由基乳液聚合过程中,根据消耗速率以恒定或变化的体积流速连续地或不连续地加入全部量或任选地剩余量。在此情况下,单体A至G的计量可以分离的单个料流的形式作为不均匀的或均匀的(亚)混合物进行或作为单体乳液进行。单体A至G有利地以单体混合物的形式计量,尤其是以水性单体乳液的形式计量。
对于制备本发明的分散聚合物P分散体,所使用的助剂包括分散助剂,所述分散助剂使得单体液滴和所合成的聚合物颗粒在水性介质中保持分散分布状态,从而确保所制备的水性聚合物分散体的稳定性。考虑的分散助剂不仅包括通常用于实施自由基水性乳液聚合的保护胶体,而且包括乳化剂。
合适的保护胶体的实例为聚乙烯醇、聚亚烷基二醇、聚丙烯酸和聚甲基丙烯酸的碱金属盐、明胶衍生物或丙烯酸、甲基丙烯酸、马来酸酐、2-丙烯酰胺基-2-甲基丙烷磺酸和/或4-苯乙烯磺酸共聚物及其碱金属盐,以及N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、N-乙烯基咔唑、1-乙烯基咪唑、2-乙烯基咪唑、2-乙烯基吡啶、4-乙烯基吡啶、丙烯酰胺、甲基丙烯酰胺、具有氨基的丙烯酸酯、甲基丙烯酸酯、丙烯酰胺和/或甲基丙烯酰胺的均聚物和共聚物。其他合适的保护胶体的详细描述见于Houben-Weyl,Methoden der organischenChemie,第XIV/1卷,Makromolekulare Stoffe[Macromolecular compounds],Georg-Thieme-Verlag,Stuttgart,1961,第411至420页。
应理解,也可以使用保护胶体和/或乳化剂的混合物。通常只使用乳化剂作为分散剂,其相对分子量——与保护胶体不同——通常小于1000。它们在种类上可为阴离子型、阳离子型或非离子型。应理解,当使用表面活性物质的混合物时,各组分必须彼此相容,在存在疑问时可以通过一些预试验确定。一般而言,阴离子乳化剂彼此相容且与非离子乳化剂相容。阳离子乳化剂也是如此,而阴离子乳化剂和阳离子乳化剂通常彼此不相容。合适的乳化剂的综述见于Houben-Weyl,Methoden der organischen Chemie,第XIV/1卷,Makromolekulare Stoffe[Macromolecular compounds],Georg-Thieme-Verlag,Stuttgart,1961,第192至208页。
然而,特别使用乳化剂作为分散助剂。
常规非离子乳化剂的实例包括乙氧基化单烷基酚、二烷基酚和三烷基酚(EO度:3至50,烷基基团:C4至C12)以及乙氧基化脂肪醇(EO度:3至80,烷基基团:C8至C36)。其实例为A级(C12C14脂肪醇乙氧基化物,EO度:3至8)、AO级(C13C15羰基合成醇乙氧基化物,EO度:3至30)、AT级(C16C18脂肪醇乙氧基化物,EO度:11至80)、ON级(C10羰基合成醇乙氧基化物,EO度:3至11)以及TO级(C13羰基合成醇乙氧基化物,EO度:3至20),以上均来自BASF SE。
常规阴离子乳化剂的实例包括以下物质的碱金属盐和铵盐:烷基硫酸酯(烷基基团:C8至C12)、乙氧基化烷醇(EO度:4至30,烷基基团:C12至C18)和乙氧基化烷基酚(EO度:3至50,烷基基团:C4至C12)的硫酸单酯、烷基磺酸(烷基基团:C12至C18)以及烷基芳基磺酸(烷基基团:C9至C18)。
此外,被证实适合作为其他阴离子乳化剂的为通式(I)的化合物
其中,R1和R2为H原子或C4至C24烷基,且不同时为H原子,并且M1和M2可为碱金属离子和/或铵离子。在通式(I)中,R1和R2优选具有6至18个碳原子,特别是具有6、12和16个碳原子的直链或支链烷基,或氢;R1和R2两者不同时为H原子。M1和M2优选钠、钾或铵,特别优选钠。特别有利的化合物(I)为那些化合物,其中M1和M2为钠,R1为具有12个碳原子的支链烷基基团并且R2为H原子或R1。通常使用包含50重量%至90重量%的单烷基化产品馏分的工业级混合物,如2A1(Dow Chemical Company的商标)。化合物(I)为公知常识(例如已知于US-A 4269749),且市售可得。
适合的阳离子活性乳化剂通常为含有C6至C18烷基、C6至C18烷基芳基或杂环基的伯、仲、叔或季铵盐,烷醇铵盐,吡啶鎓盐,咪唑鎓盐,噁唑鎓盐,吗啉鎓盐,噻唑鎓盐以及氧化胺的盐,喹啉鎓盐,异喹啉鎓盐,鎓盐,锍盐和鏻盐。通过举例的方式可提及十二烷基乙酸铵或相应的硫酸盐、多种2-(N,N,N-三甲铵)乙基链烷烃(paraffin)酯的硫酸盐或乙酸盐、N-十六烷基吡啶硫酸盐、N-十二烷基吡啶硫酸盐,以及N-十六烷基-N,N,N-三甲基硫酸铵、N-十二烷基-N,N,N-三甲基硫酸铵、N-辛基-N,N,N-三甲基硫酸铵、N,N-双十八烷基-N,N-二甲基硫酸铵,以及双子型表面活性剂N,N’-(十二烷基二甲基)乙二胺二硫酸盐、乙氧基化牛油烷基N-甲基硫酸铵和乙氧基化油胺(例如,来自BASF SE的AC,约11个氧化乙烯单元)。许多其他实例见于H.Stache,Tensid-Taschenbuch,Carl-Hanser-Verlag,Munich,Vienna,1981和McCutcheon’s,Emulsifiers&Detergents,MC PublishingCompany,Glen Rock,1989。阴离子抗衡基团(counter-groups)中极低的亲核性是有利的,适合的实例为高氯酸根;硫酸根;磷酸根;硝酸根;和羧酸根,如乙酸根、三氟乙酸根、三氯乙酸根、丙酸根、草酸根、柠檬酸根、和苯甲酸根;以及有机磺酸的共轭阴离子,例如,如甲基磺酸根、三氟甲基磺酸根和对甲苯磺酸根;以及四氟硼酸根、四苯基硼酸根、四(五氟苯基)硼酸根、四[双(3,5-三氟甲基)苯基]硼酸根、六氟磷酸根、六氟砷酸根或六氟锑酸根。
优选用作分散助剂的乳化剂有利地以总量的≥0.005重量%且≤10重量%、优选≥0.01重量%且≤5重量%,特别是≥0.1重量%且≤3重量%使用,各自基于单体的总量计。
除乳化剂外或代替乳化剂用作分散助剂的保护胶体的总量常常为≥0.1重量%且≤40重量%且通常为≥0.2重量%且≤25重量%,各自基于单体的总量计。
然而,优选使用阴离子乳化剂和/或非离子乳化剂作为分散助剂。
对于制备本发明的分散聚合物P分散体,可以在引发聚合反应之前,将全部量的分散助剂作为初始进料引入到水性反应介质中。然而,也可以在引发聚合反应前,任选地仅将一部分分散助剂作为初始进料引入到水性反应介质中,然后,在聚合条件下,于自由基乳液聚合过程中,连续地或不连续地加入全部量或任选地剩余量的分散助剂。大部分量或全部量的分散助剂优选以水性单体乳液的形式加入。
自由基引发的水性乳液聚合通过自由基聚合引发剂(自由基引发剂)引发。原则上,这类引发剂可以是过氧化物以及偶氮化合物。应理解,还考虑氧化还原引发剂体系。所使用的过氧化物原则上可为无机过氧化物,如过氧化氢或过二硫酸盐,如过二硫酸的单碱金属盐或二碱金属盐或铵盐,实例为其一钠盐和二钠盐、一钾盐和二钾盐或一铵盐和二铵盐;或有机过氧化物,如烷基氢过氧化物,实例为叔丁基氢过氧化物、对甲基氢过氧化物或枯基氢过氧化物,以及二烷基过氧化物或二芳基过氧化物,如二叔丁基过氧化物或二枯基过氧化物。发现使用的偶氮化合物主要为2,2’-偶氮双(异丁腈)、2,2’-偶氮双(2,4-二甲基戊腈)和2,2’-偶氮双(脒基丙基)二盐酸盐(AIBA,相当于来自WakoChemicals的V-50)。用于氧化还原引发剂体系的适合的氧化剂主要为上述过氧化物。作为相应的还原剂,可以使用低氧化态的硫的化合物,如碱金属亚硫酸盐,实例为亚硫酸钾和/或亚硫酸钠;碱金属亚硫酸氢盐,实例为亚硫酸氢钾和/或亚硫酸氢钠;碱金属偏亚硫酸氢盐,实例为偏亚硫酸氢钾和/或偏亚硫酸氢钠;甲醛次硫酸盐,实例为甲醛次硫酸钾和/或甲醛次硫酸钠;脂族亚磺酸的碱金属盐,尤其是钾盐和/或钠盐;和碱金属硫氢化盐,如硫氢化钾和/或硫氢化钠;多价金属盐,如硫酸亚铁(II)、硫酸亚铁(II)铵、磷酸亚铁(II);烯二醇,如二羟基马来酸、安息香和/或抗坏血酸;以及还原性糖,如山梨糖、葡萄糖、果糖和/或二羟基丙酮。通常,所用的自由基引发剂的量,基于单体总量计,为0.01重量%至5重量%,优选0.1重量%至3重量%且更优选0.2重量%至1.5重量%。
对于制备本发明的分散聚合物P分散体,可以在引发聚合反应之前,将全部量的自由基引发剂作为初始进料引入到水性反应介质中。然而,也可以在引发聚合反应前,任选地仅将一部分自由基引发剂作为初始进料引入到水性反应介质中,然后,在聚合条件下,于自由基乳液聚合过程中,以消耗速率连续地或不连续地加入全部量或任选地剩余量。
引发聚合反应意指在自由基引发剂形成自由基之后,存在于聚合容器中的单体开始聚合反应。这种聚合反应的引发可以通过在聚合条件下将自由基引发剂加入至聚合容器中的水性聚合混合物中而进行。然而,也可以在不适于引发聚合反应的条件下(例如,如低温下),向聚合容器中的包含最初引入的单体的水性聚合混合物中加入部分或全部量的自由基引发剂,以及随后提供该水性聚合混合物的聚合条件。在本文中,聚合条件通常意指自由基引发的水性乳液聚合在以足够的聚合速率进行时的温度和压力。它们特别取决于所用的自由基引发剂。这是有利的,选择自由基引发剂的种类和量、聚合温度和聚合压力,使得自由基引发剂的半衰期<3小时,特别有利地<1小时且非常特别有利地<30分钟,同时连续地提供引发基至足以引发并维持聚合反应的程度。
对于自由基水性乳液聚合,所考虑的反应温度包括0至170℃的整个范围。通常使用50至120℃,优选60至110℃,且更优选70至100℃的温度。自由基水性乳液聚合可在低于、等于或高于1atm[1.013巴(绝对值),大气压]的压力下进行,以使聚合温度可以超过100℃并且可以最高达170℃。在低沸点单体A至F存在下,乳液聚合优选在加压下进行。所述压力可采用1.2巴、1.5巴、2巴、5巴、10巴、或15巴(绝对值)或甚至更高的值。当乳液聚合在低于大气压的压力下进行时,提供压力为950毫巴、通常为900毫巴、并且经常850为毫巴(绝对值)。自由基水性乳液聚合有利地在1atm下于缺氧下进行,尤其是在惰性气体气氛下,例如,如在氮气或氩气下进行。
水性反应介质原则上还可包含少量(<5重量%)的水溶性有机溶剂,如甲醇、乙醇、异丙醇、丁醇、戊醇、或者丙酮等。优选地,水性反应介质不包含这类溶剂。
除了上述组分外,还可以任选地在乳液聚合过程中使用自由基链转移化合物,以控制或降低通过聚合可得的聚合物P的分子量。在这种情况下,主要使用脂族和/或芳脂族卤素化合物,实例为正丁基氯、正丁基溴、正丁基碘、二氯甲烷、二氯乙烷、三氯甲烷、三溴甲烷、溴三氯甲烷、二溴二氯甲烷、四氯化碳、四溴化碳、苄基氯、苄基溴;有机含硫化合物,如伯、仲或叔脂族硫醇,如乙硫醇、正丙硫醇、2-丙硫醇、正丁硫醇、2-丁硫醇、2-甲基-2-丙硫醇、正戊硫醇、2-戊硫醇、3-戊硫醇、2-甲基-2-丁硫醇、3-甲基-2-丁硫醇、正己硫醇、2-己硫醇、3-己硫醇、2-甲基-2-戊硫醇、3-甲基-2-戊硫醇、4-甲基-2-戊硫醇、2-甲基-3-戊硫醇、3-甲基-3-戊硫醇、2-乙基丁硫醇、2-乙基-2-丁硫醇、正庚硫醇及其异构体、正辛硫醇及其异构体、正壬硫醇及其异构体、正癸硫醇及其异构体、正十一烷硫醇及其异构体、正十二烷硫醇及其异构体、正十三烷硫醇及其异构体,取代的硫醇,如2-羟基乙硫醇,芳族硫醇,如苯硫酚、邻甲基苯硫酚、间甲基苯硫酚或对甲基苯硫酚,以及记载于Polymer handbook第3版,1989,J.Brandrup和E.H.Immergut,John Wiley&Sons,第II部分,第133至141页中的所有其他硫化合物;以及脂族醛和/或芳族醛,如乙醛、丙醛和/或苯甲醛;不饱和脂肪酸,如油酸;具有非共轭双键的二烯,如二乙烯基甲烷或乙烯基环己烷;或含有易于被夺取的氢原子的烃,例如,如甲苯。但是还可使用不相干扰的上述自由基链转移化合物的混合物。
在乳液聚合过程中,任选使用的自由基链转移化合物的总量基于单体的总量计,一般为≤5重量%、经常≤3重量%、且常常≤1重量%。
如果在引发自由基聚合之前将任选使用的自由基链转移化合物的一部分或全部加入至水性反应介质中,则是有利的。此外,在聚合过程中,部分或全部的自由基链转移化合物也可加入至水性反应介质中,所述水性反应介质与单体A至G一起是有利的。
特别有利地,进行分散聚合物P分散体的制备以使得单体A至G在聚合条件下反应直到转化率≥95重量%,有利地≥99重量%,且特别有利地≥99.5重量%。确定单体转化率是本领域技术人员所熟知的,并且尤其是,通过反应-量热法和/或光谱法实现。如果为了降低残留单体含量的目的,对聚合结束后获得的分散聚合物P分散体进行后处理,则常常是有利的。所述后处理以化学方法和/或物理方法进行,化学方法例如通过使用更有效的自由基引发剂体系来完成聚合反应(称为后聚合),物理方法例如通过用蒸汽或惰性气体汽提分散聚合物P分散体。相应的化学和/或物理方法是本领域技术人员所熟知的[参见,例如,EP-A771328、DE-A 19624299、DE-A 19621027、DE-A 19741184、DE-A 19741187、DE-A 19805122、DE-A 19828183、DE-A 19839199、DE-A 19840586和19847115]。化学和物理后处理的组合提供以下优点,即从分散聚合物P分散体中不仅去除了未反应的单体,而且还去除了其他破坏性的挥发性有机成分(所谓的VOCs[挥发性有机化合物])。
本发明的分散聚合物P分散体的聚合物固体含量通常≥10重量%且≤70重量%,常常≥20重量%且≤65重量%,且经常≥25重量%且≤60重量%,各自基于水性聚合物分散体计。经由准弹性光散射(ISO标准13 321)所测定的数均粒径(累积z-平均值)通常在≥10且≤1000nm范围内,优选在≥50且≤600nm范围内,且有利地在≥100至≤500nm范围内。
所述分散聚合物P分散体的pH有利地在≥4.5至≤8范围内,且更特别有利地在≥5.5至≤7.5范围内,各自通过经校准过,市售常用pH计在23℃下测得。
应理解,由本发明的分散聚合物P分散体,可以通过常规干燥方法(例如,如冷冻干燥或喷雾干燥)来制备相应的分散聚合物P粉末组合物。
所述分散聚合物P粉末组合物可由分散聚合物P分散体通过本领域技术人员所熟知的特别有利的喷雾干燥方法制备。为此目的,通常将分散聚合物P分散体与0.1重量%至30重量%,常常5重量%至15重量%——基于分散聚合物P的总量计——所谓的干燥助剂混合。这种干燥助剂是本领域技术人员所熟知的并且例如公开于EP-A 812872第5页第20行至第6页第17行以及其中所述的现有技术中。
根据本发明的粘合剂组合物的目标用途,可使用具有液化或固化作用的干燥助剂来制备分散聚合物P粉末组合物。因此,如果本发明的粘合剂组合物将要用于制备矿物防水浆料,则选择具有液化作用的干燥助剂来制备相应的分散聚合物P粉末组合物是有利的,所述具有液化作用的干燥助剂如在EP-A 812872第5页第20行至38行所公开的这类聚合物或低聚物,特别是它们具有磺酸基团、磺酸酯基团、羧基基团、或羧酸酯基团。与之相比,如果本发明的粘合剂组合物将要用于制备矿物修补砂浆或制备矿物灰泥,则选择具有固化作用的干燥助剂来制备相应的分散聚合物P粉末组合物则是有利的,所述具有固化作用的干燥助剂尤其是例如在EP-A 812872第5页第38至44行所公开的这类乙烯醇的均聚物或共聚物、乙烯基吡咯烷酮的均聚物或共聚物、或纤维素衍生物。
在本文中,对本发明中含有添加剂的分散聚合物P分散体进行喷雾干燥,通常是使含有添加剂的分散聚合物P分散体在干燥塔中喷射,所述干燥塔的入口热空气流温度Ten为100至200℃,优选120至160℃,并且出口热空气流温度Tex为30至90℃,优选50至90℃。在本文中,将含有添加剂的分散聚合物P分散体喷射于热气流中可通过例如单流体或多流体喷嘴或经由转盘进行。分散聚合物P粉末组合物通常用旋风分离器或过滤分离器进行沉积。优选平行输送喷射的含有添加剂的分散聚合物P分散体和热空气流。有利的是,在干燥塔中的喷雾干燥操作期间,另外计量加入本领域技术人员所熟知的细碎的矿物防粘结剂,例如,如细碎的硅胶,其具有特别是防止通过喷雾干燥获得的聚合物粉末组合物颗粒在长时间储存过程中结块的作用。
因此,根据本发明,还包括分散聚合物P粉末组合物,其在干燥操作中形成并且包含掺入到喷雾助剂基质中的分散聚合物P颗粒。嵌入在喷雾助剂基质中的分散聚合物P颗粒的初级粒径相当于分散聚合物P分散体中分散聚合物P的数均粒径,并且通常在≥10且≤1000nm范围内,优选在≥50且≤600nm范围内,且有利地在≥100且≤500nm范围内。
本发明的粘合剂组合物包含作为主要组分的分散聚合物P和矿物粘合剂M,所述矿物粘合剂M的量为≥1且≤10 000重量份每100重量份分散聚合物P。
所考虑的矿物粘合剂M为所有粉末形式的无机粘合剂,其在与水接触后,并且在自身被置于大气条件下的空气中或在水下的其它一些情况下中时,能够进行随时间变化的岩石状固化,所述无机粘合剂如,特别是煅石灰、石膏、炉渣砂、粉煤灰、硅尘、偏高岭土、天然火山灰或煅油页岩,以及,特别是水泥(在这方面,参见,例如,EN 197-1),如波特兰水泥、白水泥、Thurament、Celitement、高铝水泥、膨胀水泥、高炉水泥,以及与下述物质混合的水泥:例如,炉渣砂、粉煤灰、硅尘、偏高岭土、天然火山灰或煅油页岩。
如果本发明的粘合剂组合物将要用于制备矿物防水浆料,则每100重量份的分散聚合物P使用≥1且≤10 000重量份,有利地≥5且≤500重量份,且尤其有利地≥10且≤150重量份的矿物粘合剂M。与之相比,如果本发明的粘合剂组合物将要用于制备矿物瓷砖粘合剂,则每100重量份的分散聚合物P使用≥1且≤100 000重量份,有利地≥50且≤10 000重量份,且尤其有利地≥100且≤2000重量份的矿物粘合剂M。与之相比,当使用本发明的粘合剂组合物制备矿物修补砂浆或地面用配混料(flooring compound)时,每100重量份的分散聚合物P使用≥1且≤100 000重量份,有利地≥100且≤50 000重量份,且尤其有利地≥300且≤10 000重量份的矿物粘合剂M。类似地,当使用本发明的粘合剂组合物制备矿物灰泥(外墙外保温系统(thermal insulation composite system))时,每100重量份的分散聚合物P使用≥1且≤100 000重量份,有利地≥50且≤10 000重量份,且尤其有利地≥100且≤5000重量份的矿物粘合剂M。特别有利地,使用水泥作为矿物粘合剂M。
在一个有利的实施方案中,根据本发明,旨在包括矿物防水浆料配制料,其矿物粘合剂M由波特兰水泥(DIN EN 197-1,CEM I至CEM V,优选CEM I)与高铝水泥(DIN EN14647)的混合物组成。特别有利地,波特兰水泥与高铝水泥的重量比在≥0.01且≤3的范围内,尤其是≥0.1且≤1的范围内,且优选≥0.2且≤0.8。特别适合作为波特兰水泥的为来自HeidelbergCement的来自Holcim的Holcim5R、或来自Lafarge的Der同时特别适合的高铝水泥为来自Calucem的40、来自Kerneos的Ciment或或来自Ciments Molins的
根据本发明,旨在包括粉末形式和含水形式的粘合剂组合物。粉末形式的粘合剂组合物为上述分散聚合物P粉末组合物与粉末形式的矿物粘合剂M的干混合物,还包含——根据目标应用——本领域技术人员所熟知的常规量的,例如,常规粉末集料,如砂或填料,以及添加剂,如消泡剂、增稠剂、保水剂、缓凝剂和/或速凝剂。这些粉末形式的粘合剂组合物具有以下优点:在干燥状态下,它们可以长期储存并易于运输到它们的使用地点,在这里,与水以及任选地其他助剂,如砂、砾石或碎石混合后,特别是,还与其他常规添加剂混合后,它们被转化成即用型水硬性粘合剂配制料。
当然,本发明的粘合剂组合物还可包含水,得到水性粘合剂组合物。在这种情况下,水性粘合剂组合物通过将分散聚合物P分散体掺合到粉末形式的矿物粘合剂M中,或掺合到包含粉末形式的矿物粘合剂M的固体混合物中而获得,这些混合物包含,例如,填料,如砂、砾石和碎石,特别是,还有其他常规填料或添加剂,并且掺合这些组分以形成即用型水硬性粘合剂配制料。此外,水性粘合剂组合物也可通过以下方式得到:将上述粉末形式的粘合剂组合物(包含至少一种矿物粘合剂M以及至少一种分散聚合物P粉末组合物)与水掺合,任选地加入填料,如砂、砾石和碎石,特别是与其他常规填料或添加剂掺合,以形成即用型水硬性粘合剂配制料。
根据本发明,水与矿物粘合剂M的重量比——根据应用领域——在≥0.1且≤10的范围内;在矿物防水浆料情况下,水与矿物粘合剂M的重量比在≥0.4且≤1.5的范围内,且优选在≥0.6且≤1的范围内。与之相比,在矿物瓷砖粘合剂、地面用配混料、修补砂浆和灰泥的情况下,水/矿物粘合剂M的重量比在≥0.2且≤1.5的范围内,且优选在≥0.4且≤1的范围内。
在一个优选的实施方案中,旨在包括矿物防水浆料配制料,其分散聚合物P由以下物质以共聚形式合成
其中每100重量份的分散聚合物P使用≥10且≤150重量份的矿物粘合剂M,矿物粘合剂M为波特兰水泥和高铝水泥的混合物,波特兰水泥与高铝水泥的重量比在≥0.01且≤3的范围内,尤其是在≥0.1且≤1的范围内,且优选≥0.2且≤0.8。在另一个优选的实施方案中,旨在包括上述防水浆料配制料,其中水与矿物粘合剂M的重量比在≥0.6且≤1的范围内。
本发明的水性粘合剂组合物,尤其是即用型水硬性粘合剂,有利地适于基材的涂覆。因此,根据本发明,还旨在包括涂覆基材的方法,所述方法包括将本发明的水性粘合剂组合物,尤其是即用型水硬性粘合剂施用于基材表面,然后对其进行固化。在这种情况下,选择水性粘合剂组合物的量使得施用于基材的水性粘合剂组合物产生≥0.1且≤20mm的干膜厚度(即,使矿物粘合剂M固化后的膜厚度)。当水性粘合剂组合物为矿物防水浆料配制料时,选择施用率以便产生≥0.5且≤5mm且特别有利地≥1且≤3mm的干膜厚度。
所考虑的基材原则上包括所有有机和无机材料。但是,根据本发明,特别有利地,可使用具有高吸收性或“饥饿”表面的基材,所述具有高吸收性或“饥饿”表面的基材对本领域技术人员而言意指对水具有毛细管效应的多孔无机材料,例如尤其是硬化混凝土、砂浆、灰泥、或石膏板。
相应地,根据本发明,还旨在应包括涂覆有粘合剂组合物的基材。
本发明的粘合剂组合物有利地适于制备涂料,尤其适于矿物密封体系,其在固化后,展现出排放挥发性有机成分的倾向性小,从而特别满足了严格的EC1限制。
下面的非限制性实施例旨在阐明本发明。
实施例
1制备聚合物分散体
1.1制备本发明聚合物分散体P1
在聚合反应器中
在氮气气氛下,将398.4g固体含量为0.53重量%,重均粒径为30nm(d50,使用分析型超速离心机测得)的水性聚苯乙烯晶种分散体在搅拌下加热至75℃。然后加入由0.4g抗坏血酸和3.9g去离子水组成的溶液。5分钟后,在内部温度保持于75℃下,开始同时加入
a)由以下物质组成的水性单体乳液
b)28g、浓度10重量%的过氧化氢水溶液,以及
c)由3.8g抗坏血酸和34g去离子水组成的溶液,
该添加以恒定流速在3小时内连续进行。之后,将反应混合物搅拌半小时,然后冷却至70℃。在该温度下,并且内部温度保持于70℃下,在2小时内开始同时加入21g、浓度10重量%的过氧化氢水溶液和6.3g抗坏血酸于56.7g去离子水的溶液,该添加以恒定流速连续进行。之后,将反应混合物冷却至20至25℃(室温)并且用浓度10重量%的氢氧化钠水溶液调节至pH 7.5。得到聚合物分散体,其固体含量为54.9重量%,透光率为49.7%,玻璃化转变温度Tg为-11℃。
固体含量通常通过在140℃下干燥等分的(约2g)水性聚合物分散体至恒重来测定。在所有情况下都进行两次独立的测量。每一实施例中记录的数字代表两个结果的平均值。
透光率值(LD)通常在将水性聚合物分散体稀释到0.01重量%后,于20℃下,使用来自Hach的DR/2010分光光度计测定。层厚度为2.5cm。
聚合物的玻璃化转变温度通常用DSC法(差示扫描量热法,20K/min,中点测量,DIN53765)测定。
1.2制备对比分散体PC1
如聚合物分散体P1一样制备对比分散体PC1。组成仅存在下述改变:对于单体丙烯酸2-乙基己酯由420g改变为210g,对于单体苯乙烯由273g改变为133g,并且对于单体丙烯酸乙酯由630g改变为980g。
得到聚合物分散体,其固体含量为54.6重量%,透光率为50.9%,玻璃化转变温度为-11℃。
1.3制备对比分散体PC2
如聚合物分散体P1一样制备对比分散体PC2。组成仅存在下述改变:对于单体丙烯酸2-乙基己酯由420g改变为560g,对于单体苯乙烯由273g改变为357g,并且对于单体丙烯酸乙酯由630g改变为406g。
得到聚合物分散体,其固体含量为55.2重量%,透光率为46.4%,玻璃化转变温度为-7℃。
1.4制备对比PC3
在聚合反应器中
在氮气气氛下,将307.6g固体含量为0.68重量%,重均粒径为30nm(d50,使用分析型超速离心机测得)的聚苯乙烯晶种分散体在搅拌下加热至90℃。然后一次性加入由0.3g过二硫酸钠和4.2g去离子水组成的溶液。5分钟后,在内部温度保持于90℃下,开始同时加入
a)由以下物质组成的水性单体乳液C1(在3小时内加入)
b)由6.8g过二硫酸钠和89.7g去离子水组成的溶液(在3小时15分钟内连续加入),
该添加以恒定流速连续进行。在单体乳液C1进料结束后,在15分钟内连续加入30.0g丙烯酸正丁酯。之后,将反应混合物搅拌半小时,然后冷却至85℃。在该温度下,在内部温度保持于85℃下,在2小时内开始同时加入由3g叔丁基氢过氧化物和27g去离子水组成的溶液和由4.5g丙酮亚硫酸氢盐和29.8g去离子水的溶液,该添加以恒定流速连续进行。之后,将反应混合物冷却至室温并用浓度10重量%的氢氧化钠水溶液调节至pH 7.5。
得到聚合物分散体,其固体含量为56.2重量%,透光率为40.3%,玻璃化转变温度为-11℃。
随后使用去离子水,将所得到的水性聚合物分散体调节到固体含量为50重量%。
2性能研究
2.1制备用于矿物粘合剂配制料的湿组分
将32g 50%的聚合物分散体P1,以及PC1至PC3各自与0.2gSD 21(消泡剂,BASF SE)混合,并在转鼓式混合器中均匀化1分钟。
2.2制备用于矿物粘合剂配制料的本发明干组分T
如表1所指定,称取本发明干组分T的成分,如波特兰水泥、高铝水泥、硫酸钙半水合物、硅砂、碳酸锂和柠檬酸到烧杯中,并在转鼓式混合器中均匀化1分钟。
表1:矿物粘合剂配制料的本发明干组分T的组成
2.3制备用于矿物粘合剂配制料的对比干组分V
如表2所指定,称取对比干组分V的成分,如波特兰水泥、碳酸钙和硅砂到烧杯中,并在转鼓式混合器中均匀化1分钟。
表2:矿物粘合剂配制料的对比干组分V的组成
2.4矿物粘合剂配制料的制备性混合及相应膜的制备
对于本发明粘合剂配制料DS1和对比配制料DSC1至DSC4(各自的组分记录于表3),水/水泥比和聚合物/水泥比都恒定保持在0.8。为此目的,在按照DIN EN 196-1(2005-05)指定的混合器中,在300rpm搅拌下,将100g干组分T或V在30秒内掺合到32.2g湿组分。然后以600rpm继续搅拌2分钟,以确保各个矿物粘合剂配制料混合均匀并且没有团块。3分钟的静置时间后,使用纬纱刀(filling knife)在不锈钢框架(长25cm,宽15cm)的辅助下将各个矿物粘合剂配制料施用至覆盖有Teflon膜的板(长27cm,宽17cm)。在所述不锈钢框架上拖动纬纱刀以确保在所有情况下所述板覆盖有2.6mm的均匀层。在矿物粘合剂配制料的制备性混合过程中,在储存过程中及在测试过程中,温度恒定于23℃,相对湿度恒定于50%(标准条件)。
表3:矿物粘合剂配制料的组成
2.5试样的制备和储存
24小时后,从所述板上取下各干燥的粘合剂配制料,并各自冲压出6个哑铃形的试样,这些试样具有以下的尺寸:总长7.5cm;总宽1.3cm;中间宽度0.4cm;中间长度3cm。小心操作以确保每个试样都没有缺损。按照AS/NZS 4858:2004(湿区膜)的要求对各试样进行储存和测试。在标准条件下将一组为3个的试样于栅架上再储存13天,然后进行测试(“干储存”)。在标准条件下,将另一组为3个的试样在栅架上再储存6天,然后在40℃下于0.5摩尔的KOH水溶液中储存21天,随后进行干燥。
在来自Zwick,Ulm(Germany)的ProLine Z010万能试验机上对所得的哑铃试样进行机械测试。将所述试样置于夹爪中。以中间部分清楚可见的方式将它们放置于爪之间。测试以50mm/分钟的速度进行。测定了所述试样断裂时的力和伸长率。在结合所述试样厚度的情况下,可以以这种方式确定断裂力以及断裂伸长率。表4和5中记录的值代表所得结果的平均值。表4记录了干储存后的结果,表5记录了在KOH水溶液中储存后的结果。
表4:14天干储存后粘合剂配制料DS1以及DSC1至DSC3的断裂力和断裂伸长率
表5:在KOH溶液中储存后粘合剂配制料DS1以及DSC1至DSC3的断裂力和断裂伸长率
从干储存的结果可见,显然,由本发明粘合剂配制料DS1形成的膜的机械性能与对比配制料DSC2、DSC3和DSC4的膜相当。如在PC1情况下,增加分散聚合物中的丙烯酸乙酯部分超出所要求的范围,会导致DSC1的膜在KOH溶液中储存后完全失效。
3测定挥发性有机成分
3.1制备水性粘合剂配制料
将480g、50%的聚合物分散体P1,以及PC1至PC3,各自地与3gSD 21混合,并且在转鼓式混合器中各自均匀化1分钟。
3.2制备用于矿物粘合剂配制料的本发明干组分T
如表1所指定,称取本发明干组分T的成分,如波特兰水泥、高铝水泥、硫酸钙半水合物、硅砂、碳酸锂和柠檬酸到烧杯中,并在转鼓式混合器中均匀化1分钟。
3.3制备用于水性粘合剂配制料的对比干组分V
如表2所指定,称取对比干组分V的成分,如波特兰水泥、碳酸钙和硅砂到烧杯中,并在转鼓式混合器中均匀化1分钟。
3.4矿物粘合剂配制料的制备性混合及基材的涂覆
对于本发明粘合剂配制料DS1和对比配制料DSC1至DSC4,水/水泥比和聚合物/水泥比都恒定保持在0.8。为此目的,在按照DIN EN 196-1(2005-05)指定的混合器中,在300rpm搅拌下将1500g干组分在30秒内掺合到483g湿组分中。然后以600rpm继续搅拌2分钟,以确保所述水性粘合剂配制料混合均匀并且没有团块。3分钟的静置时间后,使用纬纱刀在不锈钢框架(长34cm,宽14cm)的辅助下将各个矿物粘合剂配制料施用到无油脂的玻璃板(长35cm,宽15cm)。在所述不锈钢框架上拖动纬纱刀以确保在所有情况下所述板覆盖有3mm的均匀层。所述矿物粘合剂配制料的制备性混合以及涂覆操作在标准条件下各自进行。
3.5排放测试
所述玻璃板的涂覆以及所述水性粘合剂组合物挥发性成分的测定按照GEV测试方法——在丹麦Eurofins Product Testing A/S于2013年4月15日的版本中,“测定用于表征排放受控的地板安装材料、粘合剂、建筑产品和镶木地板清漆的挥发性有机化合物(Determination of volatile organic compounds for characterizing emission-controlled floor installation materials,adhesives,construction products andparquet varnishes)”——进行。
在用特定的矿物粘合剂配制料涂覆玻璃板之后,立即将其转移到测试室,使其留在这里直到空气采样结束。除非另有说明,不锈钢测试室按照DIN EN ISO 16000-9(内部空气杂质——第9部分:测定建筑产品和配件的挥发性有机化合物排放——排放室法(interior air impurities-part 9:determination of the emission of volatileorganic compounds from construction products and fittings-emission chambermethod);2008-04)的要求进行操作。调节室内温度以及进入的空气至23±1℃,大气湿度为50±5%。将空气置换速率调节至0.5h-1,其中负载量为0.4m2/m3。所述室的体积为119升。
在施用涂料后,第一次VOCs测试的空气采样进行了3天(72±1小时)。采样和VOCs测定按照DIN EN ISO 16000-6(内部空气杂质——第6部分:测定内部空气和测试室中的VOC,经TENAX吸附柱采样,热解吸和使用MS/FID的气相色谱(interior airimpurities –part 6:determination of VOC in interior air and in test chambers,sampling on TENAXadsorption columns,thermal desorption and gaschromatography with MS/FID);2008-04)进行。由此对浓度高于1μg/m3的各物质进行检测并定量。
为此目的,所述柱——装填有TENAX60/80——用氦气流冲洗。随后通过使来自所述测试室的80ml每分的体积流,流经所述TENAX吸附柱120分钟来进行采样。通过串联两个管防止由于过载引起的低于正常的结果。在氦气流中热解吸后,使用来自Perkin-Elmer的配置有质谱仪气相色谱仪测定VOCs。使用来自Agilent的非极性柱,其具有以下特征:柱长30m;内径0.25mm;膜厚0.25μm(HP-1)。进行重复测定。
如上所述,在施用涂料后28天(672±4小时)检测长期排放。
对在LCI值((毒理学)感兴趣的最低浓度)表上的所有各物质以这种方式进行确认,各自定量,并以甲苯当量的形式进行计算。如表6中所列的检测到的所有挥发性有机化合物的总和(TVOC)通过将所列出的所有各物质的量相加而确定。
表6:3天和28天后,矿物粘合剂配制料DS1以及DSC1至DSC4的排放量
TVOC[μg/m3]
当膜在3天后的排放示出TVOC为≤1000μg/m3并且在28天后的排放示出TVOC为≤100μg/m3时,则可获得GEV体系的EC1质量标志。如由表6可见,对比配制料不能达到EC1质量标志所需的TVOC值。这只有在本发明粘合剂配制料DS1和对比配制料DSC1的情况下才是可能的,但是如表5所示对比配制料DSC1不能满足机械性能方面的要求。
Claims (17)
1.粘合剂组合物,其包含以下物质作为主要组分:
a)至少一种分散聚合物P,其玻璃化转变温度≤20℃并包含共聚形式的丙烯酸乙酯,和
b)至少一种矿物粘合剂M,其含量为≥1重量份且≤10 000重量份每100重量份分散聚合物P,所述分散聚合物P包含共聚形式的以下物质:
≥35且≤65重量%的丙烯酸乙酯(单体A),
≥0且≤5重量%的至少一种单烯键式不饱和化合物,其具有至少一个含硅基团、一个环氧基、N-羟甲基或羰基基团(单体B),
≥0且≤7重量%的至少一种单烯键式不饱和化合物,其具有至少一个羟烷基基团(单体C),
≥0且≤5重量%的至少一种单烯键式不饱和C3至C6一元羧酸和/或C4-C6二羧酸,包括其盐和酸酐(单体D),
≥0且≤5重量%的至少一种化合物,其具有至少两个非共轭烯键式不饱和基团(单体E),
≥15且≤45重量%的至少一种烯键式不饱和化合物,其不同于单体A至E但可与单体A至E共聚,为此仅由以共聚形式的该烯键式不饱和化合物合成的均聚物的玻璃化转变温度在≤30℃的范围内(单体F),和
≥10且≤30重量%的至少一种烯键式不饱和化合物,其不同于单体A至E但可与单体A至E共聚,为此仅由以共聚形式的该烯键式不饱和化合物合成的均聚物的玻璃化转变温度在≥50℃的范围内(单体G),
并且单体A至G的量合计达100重量%。
2.权利要求1的粘合剂组合物,所述分散聚合物P的玻璃化转变温度≤5℃。
3.权利要求1或2的粘合剂组合物,所述单体F选自丙烯酸甲酯、丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸仲丁酯、丙烯酸异丁酯、丙烯酸正己酯、甲基丙烯酸正己酯、甲基丙烯酸正辛酯、丙烯酸2-乙基己酯、甲基丙烯酸2-乙基己酯、丙烯酸2-丙基庚酯、丙烯酸异癸酯、丙烯酸正十二烷酯、甲基丙烯酸正十二烷酯、丙烯酸苄酯和丙烯酸乙基二甘醇酯。
4.权利要求1或2的粘合剂组合物,所述单体G选自甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸异丙酯、丙烯酸叔丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸苯酯、甲基丙烯酸环己酯、苯乙烯、3-甲基苯乙烯、4-甲基苯乙烯、2,4-二甲基苯乙烯、2,5-二甲基苯乙烯和3,5-二甲基苯乙烯。
5.权利要求1或2的粘合剂组合物,所述分散聚合物P的初级数均粒径≥100且≤500nm。
6.权利要求1或2的粘合剂组合物,所述分散聚合物P包含共聚形式的以下物质:
≥40且≤50重量% 的丙烯酸乙酯,
≥1且≤3重量% 的甲基丙烯酸缩水甘油酯,
≥2且≤5重量% 的甲基丙烯酸2-羟乙酯,
≥0.1且≤2重量% 的丙烯酸,
≥25且≤30重量% 的丙烯酸2-乙基己酯,和
≥15且≤25重量% 苯乙烯。
7.权利要求1或2的粘合剂组合物,使用水泥作为矿物粘合剂M。
8.权利要求1或2的粘合剂组合物,使用波特兰水泥和高铝水泥的混合物作为矿物粘合剂M。
9.权利要求1或2的粘合剂组合物,其包含水。
10.权利要求9的粘合剂组合物,水与矿物粘合剂M的重量比≥0.1且≤10。
11.涂覆基材的方法,所述方法包括将权利要求9或10的粘合剂组合物施用到基材表面,然后对其进行固化。
12.权利要求11的方法,其中将所述粘合剂组合物以≥0.1且≤20mm的干膜厚度施用到所述基材。
13.权利要求11和12中任一项的方法,其中使用混凝土、砂浆、灰泥、或石膏板作为基材。
14.可通过权利要求11至13中任一项的方法获得经涂覆的基材。
15.权利要求9和10中任一项的粘合剂组合物用于制备矿物防水浆料的用途。
16.分散聚合物P,其包含共聚形式的以下物质:
≥40且≤50重量% 的丙烯酸乙酯,
≥1且≤3重量% 的甲基丙烯酸缩水甘油酯,
≥2且≤5重量% 的甲基丙烯酸2-羟乙酯,
≥0.1且≤2重量% 的丙烯酸,
≥25且≤30重量% 的丙烯酸2-乙基己酯,和
≥15且≤25重量% 苯乙烯。
17.权利要求16的分散聚合物P用于制备矿物防水浆料的用途。
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WO2017093493A1 (en) * | 2015-12-04 | 2017-06-08 | Basf Se | Pulverulent primer composition |
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US11352296B2 (en) * | 2018-04-28 | 2022-06-07 | Dow Global Technologies Llc | Polymer-modified cementitious composition |
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