CN1922277A - 改进复合颗粒分散体储藏稳定性的方法 - Google Patents
改进复合颗粒分散体储藏稳定性的方法 Download PDFInfo
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- CN1922277A CN1922277A CNA2005800058497A CN200580005849A CN1922277A CN 1922277 A CN1922277 A CN 1922277A CN A2005800058497 A CNA2005800058497 A CN A2005800058497A CN 200580005849 A CN200580005849 A CN 200580005849A CN 1922277 A CN1922277 A CN 1922277A
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Classifications
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/34—Higher-molecular-weight carboxylic acid esters
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/42—Ethers, e.g. polyglycol ethers of alcohols or phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing agents
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/02—Emulsion paints including aerosols
- C09D5/024—Emulsion paints including aerosols characterised by the additives
Abstract
本发明涉及一种用于改进复合颗粒水分散体和含有所述复合颗粒水分散体的含水配制剂的储藏稳定性的方法。
Description
本发明涉及一种改进由加聚物和细碎无机固体组成的颗粒(复合颗粒)的水分散体的储藏稳定性的方法,其中在在水性介质中制备复合颗粒分散体(复合颗粒水分散体)之前、期间和之后向水性分散介质中加入含羟基的烷基氨基化合物。
本发明同样涉及通过本发明方法得到的复合颗粒水分散体,以及包含这种复合颗粒水分散体的含水配制剂。
复合颗粒水分散体为常识。所述分散体为流体体系,其中水性分散介质中的分散相包含聚合物线团和由细碎无机固体组成的颗粒,所述聚合物线团由多个缠绕在一起的聚合物链(已知的聚合物基体)组成,无机固体为均匀分布。复合颗粒的直径通常为10-5000nm。
复合颗粒、其以复合颗粒水分散体形式的制备以及其应用为本领域熟练技术人员所公知,并且例如公开在以下出版物中:US-A 3,544,500、US-A 4,421,660、US-A 4,608,401、US-A 4,981,882、EP-A 104 498、EP-A 505 230、EP-A 572 128、GB-A 2 227 739、WO 0118081、WO 0129106、WO 03000760;并且还公开在Long等人,天津大学学报,1991,4,第10-15页;Bourgeat-Lami等人,Die Angewandte Makromolekulare Chemie 1996,242,第105-122页;Paulke等人,Synthesis Studies of ParamagneticPolystyrene Latex Particles in Scientific and Clinical Applications ofMagnetic Carriers,第69-76页,Plenum Press,New York,1997;Armes等人,Advanced Materials 1999,11,No.5,第408-410页。
复合颗粒水分散体或包含它们的含水配制剂的缺点在于在长期储存,特别是在≥40℃的温度下长期储存时,其显示出粘度增加,甚至可能胶凝。这使得难以处理复合颗粒水分散体或包含它们的含水配制剂。在极端情况下,复合颗粒水分散体或包含它们的含水配制剂甚至可能变得不能用于加工。
本发明的目的是提供一种用于改进复合颗粒水分散体或包含它们的含水配制剂的储藏稳定性的新方法。
因此发现了开头定义的方法。
在制备复合颗粒水分散体的水分散体之后,在其水性分散介质中加入含羟基的烷基氨基化合物特别有利。显然,此处含义“制备复合颗粒水分散体之后”还包括制备含水配制剂,在含水配制剂的制备中除了加入其它配制成分外,还分别加入了复合颗粒水分散体和至少一种含羟基的烷基氨基化合物。
有利地,含有含羟基的烷基氨基化合物的复合颗粒水分散体或包含该分散体的含水配制剂的pH为≥4、≥5、≥6或≥7且≤10、≤11、≤12或≤13。通常pH设定为≥7且≤11。
作为含羟基的烷基氨基化合物,通常使用具有至少三个碳原子和至少一个羟基和至少一个氨基的水溶性非环烷基化合物。在本文中,已经证明有利的是烷基氨基化合物为伯氨。含羟基的烷基氨基化合物通常为具有至少三个碳原子的非环烷基化合物,其含有至少一个羟基和至少一个伯氨基。还可以理解的是,可以使用含羟基的氨基化合物的混合物。
作为具有至少三个碳原子和至少一个羟基和至少一个氨基的非环烷基化合物,例如使用三乙醇胺、二乙醇胺、2-氨基-2-甲基乙醇、2-氨基-2,2-二甲基乙醇、3-氨基丙-1-醇、3-氨基丙-2-醇、3-氨基丙-1,2-二醇、2-氨基-2-甲基丙-1,3-二醇、4-氨基丁-1-醇、2-氨基丁-1-醇、2-氨基-3-甲基丁-1-醇、5-氨基戊-1-醇、2-(2-氨基乙氧基)乙醇、6-氨基己-1-醇、7-氨基庚-1-醇、1-氨基丙-2-醇、3-氨基-3-甲基丙-1-醇、3-氨基-2-甲基丙-1-醇、3-氨基-3-丙基丙-1-醇、3-氨基-3-苯基丙-1-醇、3-氨基-3-环己基丙-1-醇、3-氨基-3-(环己烯-3-基)丙-1-醇、3-氨基-1-乙烯基丙-1-醇、3-氨基-3,3-二甲基丙-1-醇、3-氨基-2,2-二甲基丙-1-醇、3-氨基-1,1-二甲基丙-1-醇、3-氨基-3,3-二甲基-1-甲基丙-1-醇、3-氨基丁-1-醇、4-氨基丁-2-醇、4-氨基-2-甲基丁-1-醇、4-氨基-4,4-二甲基丁-1-醇、5-氨基-2,2-二甲基戊-1-醇、5-氨基-5-甲基-1,1-二甲基戊-1-醇、7-氨基-5-甲基-1,1-二甲基己-1-醇或2-(2-氨基乙基氨基)乙醇。
通常使用的含羟基的氨基化合物选自:2-氨基-2-甲基乙醇、2-氨基-2,2-二甲基乙醇、3-氨基丙-1-醇、3-氨基丙-2-醇、3-氨基丙-1,2-二醇、2-氨基-2-甲基丙-1,3-二醇、4-氨基丁-1-醇、2-氨基丁-1-醇、2-氨基-3-甲基丁-1-醇、5-氨基戊-1-醇、2-(2-氨基乙氧基)乙醇、6-氨基己-1-醇和7-氨基庚-1-醇。
含羟基的氨基化合物的量为0.01-10重量%,通常为0.05-5重量%,经常为0.1-3重量%,在每种情况下基于复合颗粒水分散体的总量。可在复合颗粒制备之前将全部含羟基的氨基化合物加入到水性分散介质中。还可以在复合颗粒制备之前向水性介质中加入至少一部分含羟基的氨基化合物,并在复合颗粒制备期间或之后向水性介质中加入剩余部分。然而有利的是将全部含羟基的氨基化合物加入到复合颗粒水分散体或包含它们的含水配制剂中。然而,还可以将部分含羟基的氨基化合物加入到复合颗粒水分散体中,并将其余部分含羟基的氨基化合物加入到含有复合颗粒水分散体的含水配制剂中。
本发明方法有利地适于通过WO 03000760公开的程序制备的那类复合颗粒水分散体,并将其引用到本说明书中作为参考。该方法的特征在于:将至少一种烯属不饱和单体分散分布在水性介质中,并且在至少一种分散分布的细碎无机固体和至少一种分散剂的存在下借助于至少一种自由基聚合引发剂通过自由基水乳液聚合方法聚合,其中:
a)使用所述至少一种无机固体的稳定的水分散体,所述分散体特征在于,在基于所述至少一种无机固体的水分散体为≥1重量%的初始固体浓度下,在其制备1小时后其仍含有分散形式的超过90重量%的初始分散固体,并且分散的固体颗粒具有≤100nm的重均直径,
b)所述至少一种无机固体的分散颗粒在标准氯化钾水溶液中,在对应于开始加入分散剂之前的水性分散介质pH的pH下显示出非零电泳淌度,
c)在开始加入所述至少一种烯属不饱和单体之前,将至少一种阴离子、阳离子和非离子分散剂加入到固体颗粒水分散体中,
d)然后,将总量的0.01-30重量%的所述至少一种单体加入到固体颗粒水分散体中,并聚合至至少90%的转化率,和
e)然后在聚合条件下以其消耗速率连续加入所述至少一种单体的其余部分。
适于该方法的细碎无机固体为形成稳定的如下水分散体的所有那些,其中所述水分散体在基于所述至少一种无机固体的水分散体为≥1重量%的初始固体浓度下,在其制备1小时后不经搅拌或振荡仍然含有分散形式的超过90重量%的初始分散固体,且分散的固体颗粒具有≤100nm的直径,并且所述水分散体在对应于开始加入分散剂之前的水性反应介质pH的pH值下显示出非零电泳淌度。
初始固体浓度和1小时后的固体浓度的定量测定以及粒径的测定通过分析超速离心方法进行(参见S.E.Harding等人,AnalyticalUltracentrifugation in Biochemistry and Polymer Science,Royal Society ofChemistry,Cambridge,Great Britain 1992,第10章,Analysis of PolymerDispersions with an Eight-Cell AUC Multiplexer:High Resolution ParticleSize Distribution and Density Gradient Techniques,W.Michtle,第147-175页)。所述粒径为已知为D50值的那些。
电泳淌度的测定方法为本领域熟练技术人员所公知(例如参见R.J.Hunter,Introduction to Modern Colloid Science,Section 8.4,第241-248页,Oxford University Press,Oxford,1993,和K.Oka和K.Furusawa,Electrical Phenomena at Interfaces,Surfactant Science Series,第76卷,第8章,第151-232页,Marcel Dekker,New York,1998)。分散在水性反应介质中的固体颗粒的电泳淌度使用市售电泳仪在20℃和1巴(绝对)测定,电泳仪的实例为得自Malvern Instruments Ltd.的Zetasizer 3000。为此,将固体颗粒的水分散体用pH中性的10毫摩尔(mM)氯化钾水溶液(标准氯化钾溶液)稀释,直到固体颗粒的浓度约为50-100毫克/升。使用常规无机酸或碱将样品的pH调节到开始加入分散剂之前的水性反应介质所具有的pH,无机酸例如为稀盐酸或硝酸,碱例如为稀氢氧化钠溶液或氢氧化钾溶液。分散的固体颗粒在电场中的迁移可通过所谓的电泳光散射检测(例如参见B.R.Ware和W.H.Flygare,Chem.Phys.Lett.12(1971),第81-85页)。在此方法中,电泳淌度的标记通过分散的固体颗粒的迁移方向限定;换句话说,如果分散的固体颗粒向阴极迁移,其电泳淌度为正,如果向阳极迁移,电泳淌度为负。
将分散的固体颗粒的电泳淌度影响或调节到一定程度上的合适参数为水性反应介质的pH。分散的固体颗粒在酸性pH范围(pH<7)内的质子化和在碱性pH范围(pH>7)内的去质子化分别将电泳淌度改变为正或负。适于WO 03000760公开的方法的pH范围为可以进行自由基引发的水乳液聚合的范围。该pH范围通常为1-12,经常为1.5-11,并且往往为2-10。
水性反应介质的pH可使用市售常规酸或碱调节,酸例如为稀盐酸、硝酸或硫酸,碱例如为稀氢氧化钠或氢氧化钾溶液。通常有利的是在加入所述至少一种细碎无机固体之前,将用于调节pH的部分或全部酸或碱加入水性反应介质中。
对于WO 03000760公开的方法而言,有利的是,在上述pH条件下:
-当分散的固体颗粒具有负电泳淌度时,对于每100重量份所述至少一种烯属不饱和单体,使用0.01-10重量份、优选0.05-5重量份、特别优选0.1-3重量份的至少一种阳离子分散剂,0.01-100重量份、优选0.05-50重量份、特别优选0.1-20重量份的至少一种非离子分散剂,和至少一种阴离子分散剂,阴离子分散剂的量应使阴离子分散剂与阳离子分散剂的当量比大于1,或
-当分散的固体颗粒具有正电泳淌度时,对于每100重量份所述至少一种烯属不饱和单体,使用0.01-10重量份、优选0.05-5重量份、特别优选0.1-3重量份的至少一种阴离子分散剂,0.01-100重量份、优选0.05-50重量份、特别优选0.1-20重量份的至少一种非离子分散剂,和至少一种阳离子分散剂,阳离子分散剂的量应使阳离子分散剂与阴离子分散剂的当量比大于1。
阴离子分散剂和阳离子分散剂的当量比指的是使用的阴离子分散剂的摩尔数与每摩尔阴离子分散剂中存在的阴离子基团数的乘积,除以使用的阳离子分散剂的摩尔数与每摩尔阳离子分散剂中存在的阳离子基团数的乘积。相应地定义阳离子分散剂和阴离子分散剂的当量比。
根据WO 03000760使用的所述至少一种阴离子、阳离子和非离子分散剂的总量可以包括在固体水分散体的初始进料中。然而,还可以在固体水分散体的初始进料中仅仅包括部分所述分散剂,而其余分散剂在自由基乳液聚合期间连续或非连续加入。然而对于本发明来说关键的是,在自由基引发的乳液聚合之前或期间,上述阴离子分散剂和阳离子分散剂的当量比保持为细碎固体的电泳标记的函数。因此,当使用在上述pH条件下的无机固体颗粒具有负的电泳淌度时,在乳液聚合期间阴离子分散剂和阳离子分散剂的当量比必须大于1。类似地,在无机固体颗粒具有带有正的电泳淌度时,在乳液聚合期间阳离子分散剂和阴离子分散剂的当量比必须大于1。有利的是当量比≥2、≥3、≥4、≥5、≥6、≥7或≥10,特别有利的是当量比为2-5之间。
可用于WO 03000760公开的方法并且通常用于制备复合颗粒的合适的细碎无机固体包括金属,金属化合物如金属氧化物和金属盐,以及半金属化合物和非金属化合物。可以使用的细碎金属粉末为贵金属胶体,例如钯、银、钌、铂、金和铑,以及其合金。对于细碎金属氧化物,可以提及的实例包括二氧化钛(例如可以从Sachtleben Chemie GmbH以Hombitec购得)、氧化锆(IV)、氧化锡(II)、氧化锡(IV)(例如可以从Akzo-Nobel以NyacolSN品级购得)、氧化铝(例如可以从Akzo-Nobel以NyacolAl品级购得)、氧化钡、氧化镁、各种铁氧化物如氧化铁(II)(方铁矿(wuestite))、氧化铁(III)(赤铁矿)和氧化铁(II/III)(磁铁矿)、氧化铬(III)、氧化锑(III)、氧化铋(III)、氧化锌(例如可以从Sachtleben Chemie GmbH以Sachtotec品级购得)、氧化镍(II)、氧化镍(III)、氧化钴(II)、氧化钴(III)、氧化铜(II)、氧化钇(III)(例如可以从Akzo-Nobel以NyacolYTTRIA品级购得)、氧化铈(IV)(例如可以从Akzo-Nobel以NyacolCEO2品级购得),上述氧化物可以呈非晶和/或其不同的晶型,还包括其羟基氧化物,例如羟基钛(IV)氧化物、羟基锆(IV)氧化物、羟基铝氧化物(例如可以从Condea-ChemieGmbH以Disperal品级购得)和羟基铁(III)氧化物,上述羟基氧化物呈非晶和/或其不同的晶型。下列非晶和/或不同晶体结构的金属盐原则上可用于本发明方法:硫化物,如硫化铁(II)、硫化铁(III)、二硫化铁(II)(黄铁矿)、硫化锡(II)、硫化锡(IV)、硫化汞(II)、硫化镉(II)、硫化锌、硫化铜(II)、硫化银、硫化镍(II)、硫化钴(II)、硫化钴(III)、硫化锰(II)、硫化铬(III)、硫化钛(II)、硫化钛(III)、硫化钛(IV)、硫化锆(IV)、硫化锑(III)和硫化铋(III);氢氧化物,如氢氧化锡(II)、氢氧化铝、氢氧化镁、氢氧化钙、氢氧化钡、氢氧化锌、氢氧化铁(II)和氢氧化铁(III);硫酸盐,如硫酸钙、硫酸锶、硫酸钡和硫酸铅(IV);碳酸盐,如碳酸锂、碳酸镁、碳酸钙、碳酸锌、碳酸锆(IV)、碳酸铁(II)和碳酸铁(III);正磷酸盐,如正磷酸锂、正磷酸钙、正磷酸锌、正磷酸镁、正磷酸铝、正磷酸锡(III)、正磷酸铁(II)和正磷酸铁(III);偏磷酸盐,如偏磷酸锂、偏磷酸钙和偏磷酸铝;焦磷酸盐,如焦磷酸镁、焦磷酸钙、焦磷酸锌、焦磷酸铁(III)和焦磷酸锡(II);铵的磷酸盐,如磷酸铵镁、磷酸铵锌、羟基磷灰石[Ca5{(PO4)3OH}];原硅酸盐,如原硅酸锂、原硅酸钙/镁、原硅酸铝、原硅酸铁(II)、原硅酸铁(III)、原硅酸镁、原硅酸锌、原硅酸锆(III)和原硅酸锆(IV);偏硅酸盐,如偏硅酸锂、偏硅酸镁/钙、偏硅酸钙、偏硅酸镁和偏硅酸锌;页硅酸盐,例如硅酸钠铝和硅酸钠镁,特别是天然分层形式的那些,例如OptigelSH(Südchemie AG的商标)、SaponitSKS-20和HektoritSKS 21(Hoechst AG的商标)、LaponiteRD和LaponiteGS(Laporte Industries Ltd的商标);铝酸盐,如铝酸锂、铝酸钙和铝酸锌;硼酸盐,如偏硼酸镁和原硼酸镁;草酸盐,如草酸钙、草酸锆(IV)、草酸镁、草酸锌和草酸铝;酒石酸盐,如酒石酸钙;乙酰丙酮化物,如乙酰丙酮铝和乙酰丙酮铁(III);水杨酸盐,如水杨酸铝;柠檬酸盐,如柠檬酸钙、柠檬酸铁(II)和柠檬酸锌;棕榈酸盐,如棕榈酸铝、棕榈酸钙和棕榈酸镁;硬脂酸盐,如硬脂酸铝、硬脂酸钙、硬脂酸镁和硬脂酸锌;月桂酸盐,如月桂酸钙;亚油酸盐,如亚油酸钙;以及油酸盐,如油酸钙、油酸铁(II)和油酸锌。
作为根据本发明可以使用的半金属化合物,可以提及的是非晶二氧化硅和/或以不同晶体结构存在的二氧化硅。根据本发明合适的二氧化硅可以市购并且例如可以Aerosil(Degussa AG的商标)、Levasil(Bayer AG的商标)、Ludox(DuPont的商标)、Nyacol和Bindzil(Akzo-Nobel的商标)和Snowtex(Nissan Chemical Industries,Ltd的商标)得到。根据本发明合适的非金属化合物例如为胶态石磨和金刚石。
特别合适的细碎无机固体为在20℃和1巴(绝对)下在水中溶解度为≤1克/升,优选≤0.1克/升,特别是≤0.01克/升的那些。特别优选的化合物选自:二氧化硅,氧化铝,氧化锡(IV),氧化钇(III),氧化铈(IV),羟基铝氧化物,碳酸钙,碳酸镁,正磷酸钙,正磷酸镁,偏磷酸钙,偏磷酸镁,焦磷酸钙,焦磷酸镁,原硅酸盐如原硅酸锂、原硅酸钙/镁、原硅酸铝、原硅酸铁(II)、原硅酸铁(III)、原硅酸镁、原硅酸锌、原硅酸锆(III)、原硅酸锆(IV),偏硅酸盐如偏硅酸锂、偏硅酸钙/镁、偏硅酸钙、偏硅酸镁、偏硅酸锌,页硅酸盐如硅酸钠铝和硅酸钠镁,特别是天然分层形式的那些,如OptigelSH、SaponitSKS-20和HektoritSKS 21、以及LaponiteRD、LaponiteGS,氧化铁(II),氧化铁(III),氧化铁(II/III),二氧化钛,羟基磷灰石,氧化锌和硫化锌。特别优选硅化合物,例如热解法二氧化硅和/或胶态二氧化硅、二氧化硅溶胶和/或页硅酸盐。硅化合物通常具有负的电泳淌度。
在本发明方法中,还可有利地使用市售化合物Aerosil、Levasil、Ludox、Nyacol和bindzil品级(二氧化硅)、Disperal品级(羟基铝氧化物)、NyacolAL品级(氧化铝)、Hombitec品级(二氧化钛)、NyacolSN品级(氧化锡(IV))、NyacolYTTRIA品级(氧化钇(III))、NyacolCEO2品级(氧化铈(IV))和Sachtotec品级(氧化锌)。
可用于制备复合颗粒的细碎无机固体具有的颗粒在分散在水性反应介质中时粒径≤100nm。成功使用的细碎无机固体为其分散的颗粒具有>0nm且≤90nm、≤80nm、≤70nm、≤60nm、≤50nm、≤40nm、≤30nm、≤20nm或≤10nm和所有中间值的直径的那些。有利地使用粒径≤50nm的细碎无机固体。粒径通过AUC方法测定。
细碎固体原则上可通过本领域熟练技术人员公知的方法得到,并且其可例如通过在气相中的沉淀反应或化学反应得到(参见E.Matijevic,Chem.Mater.5(1993),第412-426页;Ullmann’s Encyclopedia of IndustrialChemistry,第A 23卷,第583-660页,Verlag Chemie,Weinheim,1992;D.F.Evans,H.Wennerstrm in The Colloidal Domain,第363-405页,Verlag Chemie,Weinheim,1994,以及R.J.Hunter in Foundations ofColloid Science,第I卷,第10-17页,Clarendon Press,Oxford,1991)。
固体的稳定分散体通常在合成细碎无机固体期间在水性介质中直接制备,或者通过将细碎无机固体分散在水性介质中制备。根据所述固体的制备方式,这可直接进行,例如在沉淀二氧化硅或热解法二氧化硅、氧化铝等的情况下;或通过使用合适的辅助装置进行,例如分散器或超声焊极(sonotrode)。
为了制备复合颗粒水分散体,合适的细碎无机固体有利地为如下那些:其固体水分散体在基于所述固体的水分散体为≥1重量%的初始固体浓度下,在其制备或通过搅拌或振动沉积固体1小时后,不经进一步搅拌或振动仍然含有分散形式的超过90重量%的初始分散的固体,并且其分散的固体颗粒具有≤100nm直径。初始固体浓度通常≤60重量%。然而有利的是,还可使用≤55重量%、≤50重量%、≤45重量%、≤40重量%、≤35重量%、≤30重量%、≤25重量%、≤20重量%、≤15重量%、≤10重量%并且≥2重量%、≥3重量%、≥4重量%或≥5重量%以及所有其间的值的初始固体浓度,在每种情况下基于细碎无机固体水分散体。为了制备复合颗粒水分散体,对于每100重量份的所述至少一种烯属不饱和单体,通常使用1-1000、通常5-300,经常10-200重量份的所述至少一种细碎无机固体。
为了制备WO 03000760的复合颗粒水分散体,使用的分散剂包括不仅使细碎无机固体颗粒,还将单体液滴和所得复合颗粒在水相中保持分散分布,并由此确保产生的复合颗粒水分散体的稳定性的那些。合适的分散剂包括通常用于进行自由基水乳液聚合的保护性胶体和乳化剂。
合适的保护性胶体的详细描述在Houben-Weyl,Methoden derorganischen Chemie,第XIV/1卷,Makromolekulare Stoffe[Macromolecular compounds],Georg-Thieme-Verlag,Stuttgart,1961,第411-420页中给出。
合适的中性保护性胶体的实例为聚乙烯醇、聚亚烷基二醇、纤维素衍生物、淀粉衍生物和明胶衍生物。
合适的阴离子保护性胶体,亦即其分散组分具有至少一个负电荷的保护性胶体的实例为:聚丙烯酸和聚甲基丙烯酸及其碱金属盐,含有丙烯酸、甲基丙烯酸、2-丙烯酰氨基-2-甲基丙烷磺酸、4-苯乙烯磺酸和/或马来酐的共聚物,以及该类共聚物的碱金属盐,以及例如聚苯乙烯的高分子量化合物的磺酸的碱金属盐。
合适的阳离子保护性胶体,亦即其分散组分具有至少一个正电荷的保护性胶体的实例为:含有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,氨基官能的丙烯酸酯、甲基丙烯酸酯、丙烯酰胺和/或甲基丙烯酰胺的均聚物或共聚物的N-质子化和/或N-烷基化衍生物。
当然还可使用乳化剂和/或保护性胶体的混合物。作为分散剂,通常仅使用相对分子量通常低于1500的乳化剂,这与保护性胶体相对分子量不同。若使用表面活性物质混合物,各个组分当然必须彼此相容,若有相容性疑惑可通过几个预备试验进行检查。合适的乳化剂的综述在Houben-Weyl,Methoden der organischen Chemie,第XIV/1卷,Makromolekulare Stoffe[Macromolecular compounds],Georg-Thieme-Verlag,Stuttgart,1961,第192-208页给出。
常用的非离子乳化剂例如为乙氧基化单、二和三烷基酚(EO单元:3-50;烷基:C4-C12)和乙氧基化的脂肪醇(EO单元:3-80;烷基:C8-C36)。实例为购自BASF AG的LutensolA品级(C12C14脂肪醇乙氧基化物,EO单元:3-8)、LutensolAO品级(C13C15羰基合成醇乙氧基化物,EO units:3-30)、LutensolAT品级(C16C18脂肪醇乙氧基化物,EO单元:11-80)、LutensolON品级(C10羰基合成醇乙氧基化物,EO单元:3-11)和LutensolTO品级(C13羰基合成醇乙氧基化物,EO单元:3-20)。
常用的阴离子乳化剂例如为烷基硫酸酯(烷基:C8-C12)、硫酸与乙氧基化链烷醇(EO单元:3-30;烷基:C12-C18)和乙氧基化烷基酚(EO单元:3-50;烷基:C4-C12)的单酯、烷基磺酸(烷基:C12-C18)和烷基芳基磺酸(烷基:C9-C18)的碱金属盐或铵盐。
已经证明为合适的其它阴离子乳化剂的化合物为通式I化合物:
其中R1和R2为氢或C4-C24烷基但不能同时为氢,并且A和B可为碱金属离子或铵离子。在通式I中,R1和R2优选为含6-18个碳原子,尤其是含6、12或16个碳原子的直链或支链烷基或为H,R1和R2不能同时为氢。A和B优选为钠、钾或铵,特别优选钠。特别有利的化合物I为A和B为钠、R1为含12个碳原子的支链烷基并且R2为氢或R1的那些。通常,使用含有50-90重量%单烷基化产物的工业级混合物;例如Dowfax2A1(Dow Chemical Company的商标)。化合物I广泛公知,例如由US-A-4,269,749已知并可市购。
合适的阳离子活性乳化剂通常为含有C6-C18烷基、芳烷基或杂环基的伯、仲、叔或季铵盐、链烷醇铵盐、吡啶盐、咪唑啉输盐、唑啉盐、吗啉盐、噻唑啉盐,以及胺氧化物的盐、喹啉盐、异喹啉盐、盐、锍盐和盐。可以提及的实例包括:十二烷基乙酸铵或相应盐酸盐、各种链烷酸2-(N,N,N)三甲基铵乙基酯的氯化物或乙酸盐、氯化N-鲸蜡基吡啶、N-月桂基吡啶硫酸盐,以及N-鲸蜡基-N,N,N-三甲基溴化铵、N-十二烷基-N,N,N-三甲基溴化铵、N-辛基-N,N,N-三甲基溴化铵、N,N-二硬脂基二甲基氯化铵,以及双结构表面活性剂N,N′-(月桂基二甲基)乙二胺二溴化物。其它实例公开在H.Stache,Tensid-Taschenbuch,Carl-Hanser-Verlag,Munich,Vienna,1981和McCutcheon’s,Emulsifiers& Detergents,MC Publishing Company,Glen Rock,1989。
通常使用0.1-10重量%,经常0.5-7.0重量%,通常1.0-5.0重量%的分散剂制备复合颗粒水分散体,在每种情况下基于复合颗粒水分散体的总量。优选使用乳化剂。
烯属不饱和并且适于制备复合颗粒的单体特别包括:易于自由基聚合的单体,例如乙烯,乙烯基芳族单体如苯乙烯、α-甲基苯乙烯、邻氯苯乙烯或乙烯基甲苯,乙烯醇和C1-C18单羧酸的酯如乙酸乙烯酯、丙酸乙烯酯、正丁酸乙烯酯、月桂酸乙烯酯和硬脂酸乙烯酯,优选C3-C6α,β-单烯属不饱和单羧酸和二羧酸如尤其是丙烯酸、甲基丙烯酸、马来酸、富马酸和衣康酸与通常C1-C12,优选C1-C8,尤其是C1-C4链烷醇的酯,例如丙烯酸和甲基丙烯酸的甲酯、乙酯、正丁酯、异丁酯和2-乙基己酯,马来酸二甲酯或马来酸二正丁酯,α,β-单烯属不饱和羧酸的腈如丙烯腈,以及C4-C8共轭二烯如1,3-丁二烯和异戊二烯。这些单体通常构成主要单体,基于待通过本发明方法聚合的单体的总量,其通常占≥50重量%,≥80重量%或≥90重量%的比例。通常,这些单体在标准条件下[20℃,1巴(绝对)]仅仅具有中等至较差的溶解性。
通常增加聚合物基体膜的内部强度的单体通常含有至少一个环氧基、羟基、N-羟甲基或羰基,或含有至少两个非共轭烯属不饱和双键。其实例为具有两个乙烯基的单体、具有两个亚乙烯基的单体和具有两个链烯基的单体。在本文中特别有利的是二元醇与α,β-单乙烯不饱和单羧酸的二酯,其中优选丙烯酸和甲基丙烯酸的二酯。这种具有两个非共轭烯属不饱和双键的单体的实例为二丙烯酸和二甲基丙烯酸的亚烷基二醇酯,例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、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,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、氰脲酸三烯丙酯和异氰脲酸三烯丙酯。其中特别重要的是甲基丙烯酸和丙烯酸的C1-C8羟烷基酯,例如丙烯酸和甲基丙烯酸的正羟乙酯、正羟丙酯或正羟丁酯,以及诸如双丙酮丙烯酰胺、丙烯酸和甲基丙烯酸的乙酰乙酰氧基乙酯的化合物。根据本发明,基于待聚合单体的总量,上述单体以至多5重量%的量共聚。
还可任选使用含有硅氧烷基的单体,例如乙烯基三烷氧基硅烷如乙烯基三甲氧基硅烷,烷基乙烯基二烷氧基硅烷,丙烯酰氧基烷基三烷氧基硅烷,或甲基丙烯酰氧基烷基三烷氧基硅烷,例如丙烯酰氧基乙基三甲氧基硅烷、甲基丙烯酰氧基乙基三甲氧基硅烷、丙烯酰氧基丙基三甲氧基硅烷或甲基丙烯酰氧基丙基三甲氧基硅烷。这些单体以至多2重量%,通常0.01-1重量%,经常0.05-0.5重量%的量使用,在每种情况下基于单体总量。
除此之外,含有至少一个酸基和/或其相应阴离子的烯属不饱和单体A或含有至少一个氨基、酰氨基、脲基或N-杂环基和/或其N-质子化或N-烷基化铵衍生物的烯属不饱和单体B也可用作单体。基于单体总量,单体A或单体B的量分别至多为10重量%,通常0.1-7重量%,经常0.2-5重量%。
所用单体A为含有至少一个酸基的烯属不饱和单体。酸基例如可为羧酸、磺酸、硫酸、磷酸和/或膦酸基团。单体A的实例为丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸、巴豆酸、4-苯乙烯磺酸、2-甲基丙烯酰氧基乙磺酸、乙烯基磺酸和乙烯基膦酸,以及正羟基烷基丙烯酸酯和正羟基烷基甲基丙烯酸酯的磷酸单酯如丙烯酸羟乙酯、丙烯酸正羟丙酯、丙烯酸正羟丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸正羟丙酯、甲基丙烯酸正羟丁酯的磷酸单酯。然而根据本发明还可使用上述含有至少一个酸基的烯属不饱和单体的铵盐和碱金属盐。特别优选的碱金属为钠和钾。这种化合物的实例为丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸、巴豆酸、4-苯乙烯磺酸、2-甲基丙烯酰氧基乙磺酸、乙烯基磺酸和乙烯基膦酸的铵盐、钠盐和钾盐,以及丙烯酸羟乙酯、丙烯酸正羟丙酯、丙烯酸正羟丁酯和甲基丙烯酸羟乙酯、甲基丙烯酸正羟丙酯或甲基丙烯酸正羟丁酯的单和二铵盐、钠盐和钾盐。
优选使用丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸、巴豆酸、4-苯乙烯磺酸、2-甲基丙烯酰氧基乙磺酸、乙烯基磺酸和乙烯基膦酸。
作为单体B,使用含有至少一个氨基、酰氨基、脲基或N-杂环基和/或其N-质子化或N-烷基化铵衍生物的烯属不饱和单体。
含有至少一个氨基的单体B的实例为丙烯酸2-氨基乙酯、甲基丙烯酸2-氨基乙酯、丙烯酸3-氨基丙酯、甲基丙烯酸3-氨基丙酯、丙烯酸4-氨基正丁酯、甲基丙烯酸4-氨基正丁酯、丙烯酸2-(N-甲基氨基)乙酯、甲基丙烯酸2-(N-甲基氨基)乙酯、丙烯酸2-(N-乙基氨基)乙酯、甲基丙烯酸2-(N-乙基氨基)乙酯、丙烯酸2-(N-正丙基氨基)乙酯、甲基丙烯酸2-(N-正丙基氨基)乙酯、丙烯酸2-(N-异丙基氨基)乙酯、甲基丙烯酸2-(N-异丙基氨基)乙酯、丙烯酸2-(N-叔丁基氨基)乙酯、甲基丙烯酸2-(N-叔丁基氨基)乙酯(例如可以从Elf Atochem以NorsocrylTBAEMA购得)、丙烯酸2-(N,N-二甲基氨基)乙酯(例如可以从Elf Atochem以NorsocrylADAME购得)、甲基丙烯酸2-(N,N-二甲基氨基)乙酯(例如可以从Elf Atochem以NorsocrylMADAME购得)、丙烯酸2-(N,N-二乙基氨基)乙酯、甲基丙烯酸2-(N,N-二乙基氨基)乙酯、丙烯酸2-(N,N-二正丙基氨基)乙酯、甲基丙烯酸2-(N,N-二正丙基氨基)乙酯、丙烯酸2-(N,N-二异丙基氨基)乙酯、甲基丙烯酸2-(N,N-二异丙基氨基)乙酯、丙烯酸3-(N-甲基氨基)丙酯、甲基丙烯酸3-(N-甲基氨基)丙酯、丙烯酸3-(N-乙基氨基)丙酯、甲基丙烯酸3-(N-乙基氨基)丙酯、丙烯酸3-(N-正丙基氨基)丙酯、甲基丙烯酸3-(N-正丙基氨基)丙酯、丙烯酸3-(N-异丙基氨基)丙酯、甲基丙烯酸3-(N-异丙基氨基)丙酯、丙烯酸3-(N-叔丁基氨基)丙酯、甲基丙烯酸3-(N-叔丁基氨基)丙酯、丙烯酸3-(N,N-二甲基氨基)丙酯、甲基丙烯酸3-(N,N-二甲基氨基)丙酯、丙烯酸3-(N,N-二乙基氨基)丙酯、甲基丙烯酸3-(N,N-二乙基氨基)丙酯、丙烯酸3-(N,N-二正丙基氨基)丙酯、甲基丙烯酸3-(N,N-二正丙基氨基)丙酯、丙烯酸3-(N,N-二异丙基氨基)丙酯和甲基丙烯酸3-(N,N-二异丙基氨基)丙酯。
含有至少一个酰氨基的单体B的实例为丙烯酰胺、甲基丙烯酰胺、N-甲基丙烯酰胺、N-甲基甲基丙烯酰胺、N-乙基丙烯酰胺、N-乙基甲基丙烯酰胺、N-正丙基丙烯酰胺、N-正丙基甲基丙烯酰胺、N-异丙基丙烯酰胺、N-异丙基甲基丙烯酰胺、N-叔丁基丙烯酰胺、N-叔丁基甲基丙烯酰胺、N,N-二甲基丙烯酰胺、N,N-二甲基甲基丙烯酰胺、N,N-二乙基丙烯酰胺、N,N-二乙基甲基丙烯酰胺、N,N-二正丙基丙烯酰胺、N,N-二正丙基甲基丙烯酰胺、N,N-二异丙基丙烯酰胺、N,N-二异丙基甲基丙烯酰胺、N,N-二正丁基丙烯酰胺、N,N-二正丁基甲基丙烯酰胺、N-(3-N′,N′-二甲基氨基丙基)甲基丙烯酰胺、双丙酮丙烯酰胺、N,N’-亚甲基双丙烯酰胺、N-(二苯甲基)丙烯酰胺、N-环己基丙烯酰胺和N-乙烯基吡咯烷酮和N-乙烯基己内酰胺。
含有至少一个脲基的单体B的实例为N,N’-二乙烯基亚乙基脲和甲基丙烯酸2-(1-咪唑啉-2-酮基)乙酯(例如可以从Elf Atochem以Norsocryl100购得)。
含有至少一个N-杂环基的单体B的实例为2-乙烯基吡啶、4-乙烯基吡啶、1-乙烯基咪唑、2-乙烯基咪唑和N-乙烯基咔唑。
优选使用下列化合物:2-乙烯基吡啶、4-乙烯基吡啶、2-乙烯基咪唑、丙烯酸2-(N,N-二甲基氨基)乙酯、甲基丙烯酸2-(N,N-二甲基氨基)乙酯、丙烯酸2-(N,N-二乙基氨基)乙酯、甲基丙烯酸2-(N,N-二乙基氨基)乙酯、甲基丙烯酸2-(N-叔丁基氨基)乙酯、N-(3-N′,N′-二甲基氨基丙基)甲基丙烯酰胺和甲基丙烯酸2-(1-咪唑啉-2-酮基)乙酯。
根据水性反应介质的pH,部分或全部上述含氮单体B还可以N-质子化的季铵形式存在。
作为氮原子上具有四烷基铵结构的单体B,可以提及的实例包括丙烯酸2-(N,N,N-三甲基铵)乙酯氯化物(例如可以从Elf Atochem以NorsocrylADAMQUAT MC 80购得)、甲基丙烯酸2-(N,N,N-三甲基铵)乙酯氯化物(例如可以从Elf Atochem以NorsocrylMADQUAT MC 75购得)、丙烯酸2-(N-甲基-N,N-二乙基铵)乙酯氯化物、甲基丙烯酸2-(N-甲基-N,N-二乙基铵)乙酯氯化物、丙烯酸2-(N-甲基-N,N-二丙基铵)乙酯氯化物、甲基丙烯酸2-(N-甲基-N,N-二丙基铵)乙酯、丙烯酸2-(N-苄基-N,N-二甲基铵)乙酯氯化物(例如可以从Elf Atochem以NorsocrylADAMQUAT BZ 80购得)、甲基丙烯酸2-(N-苄基-N,N-二甲基铵)乙酯氯化物(例如可以从Elf Atochem以NorsocrylMADQUAT BZ 75购得)、丙烯酸2-(N-苄基-N,N-二乙基铵)乙酯氯化物、甲基丙烯酸2-(N-苄基-N,N-二乙基铵)乙酯氯化物、丙烯酸2-(N-苄基-N,N-二丙基铵)乙酯氯化物、甲基丙烯酸2-(N-苄基-N,N-二丙基铵)乙酯氯化物、丙烯酸3-(N,N,N-三甲基铵)丙酯氯化物、甲基丙烯酸3-(N,N,N-三甲基铵)丙酯氯化物、丙烯酸3-(N-甲基-N,N-二乙基铵)丙酯氯化物、甲基丙烯酸3-(N-甲基-N,N-二乙基铵)丙酯氯化物、丙烯酸3-(N-甲基-N,N-二丙基铵)丙酯氯化物、甲基丙烯酸3-(N-甲基-N,N-二丙基铵)丙酯氯化物、丙烯酸3-(N-苄基-N,N-二甲基铵)丙酯氯化物、甲基丙烯酸3-(N-苄基-N,N-二甲基铵)丙酯氯化物、丙烯酸3-(N-苄基-N,N-二乙基铵)丙酯氯化物、甲基丙烯酸3-(N-苄基-N,N-二乙基铵)丙酯氯化物、丙烯酸3-(N-苄基-N,N-二丙基铵)丙酯氯化物和甲基丙烯酸3-(N-苄基-N,N-二丙基铵)丙酯氯化物。当然还可使用相应的溴化物和硫酸盐代替氯化物。
优选使用丙烯酸2-(N,N,N-三甲基铵)乙酯氯化物、甲基丙烯酸2-(N,N,N-三甲基铵)乙酯氯化物、丙烯酸2-(N-苄基-N,N-二甲基铵)乙酯氯化物和甲基丙烯酸2-(N-苄基-N,N-二甲基铵)乙酯氯化物、
当然还可使用上述烯属不饱和单体的混合物。
适于通过自由基聚合制备复合颗粒水分散体的引发剂为所有能够引发自由基水乳液聚合的聚合引发剂。引发剂原则上包括过氧化物和偶氮化合物。当然,氧化还原引发剂体系也适于使用。所用过氧化物原则上可以是无机过氧化物,例如过氧化氢或过硫酸盐,如过硫酸的单或二碱金属盐或铵盐,实例为单和二钠盐和钾盐,或铵盐;或为有机过氧化物,例如过氧化氢烷基,实例为过氧化氢叔丁基、过氧化氢对基和过氧化氢枯基,以及二烷基或二芳基过氧化物,例如过氧化二叔丁基或过氧化二枯基。使用的偶氮化合物主要为2,2’-偶氮二(异丁腈)、2,2’-偶氮二(2,4-二甲基戊腈)和2,2′-偶氮二(脒基丙基)二盐酸盐(AIBA,对应于得自Wako Chemicals的商品V-50)。氧化还原引发剂体系中合适的氧化剂基本上为上述过氧化物。相应的还原剂可为具有低氧化态的硫化合物,例如碱金属亚硫酸盐如亚硫酸钾和/或钠,碱金属亚硫酸氢盐如亚硫酸氢钾和/或钠,碱金属偏亚硫酸氢盐如偏亚硫酸氢钾和/或钠,甲醛化次硫酸盐如甲醛化次硫酸钾和/或钠,脂肪亚磺酸的碱金属盐,尤其是钾盐和/或钠盐,以及碱金属氢硫化物如氢硫化钾和/或钠,多价金属盐如硫酸铁(II)、硫酸铁(II)铵、磷酸铁(II)、烯二醇如二羟基马来酸、苯偶姻和/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。基于单体混合物的总量,自由基聚合引发剂的用量通常为0.1-5重量%。
在细碎无机固体的存在下,自由基水相聚合反应的合适反应温度包括0-170℃的全部范围。使用的反应温度通常为50-120℃,通常为60-110℃,并且经常为>70℃至100℃。自由基水乳液聚合可在低于、等于或大于1巴(绝对)的压力下进行,因此聚合温度可以超过100℃并可至多为170℃。优选在升高的压力下聚合诸如乙烯、丁二烯或氯乙烯的高挥发性单体。在这种情况下压力可为1.2、1.5、2、5、10或15巴或更高的值。当乳液聚合在低于一大气压的压力下进行时,压力通常设定在950毫巴,通常为900毫巴,并且通常设定在850毫巴(绝对)。自由基水相聚合有利地在1巴(绝对),在惰性气体气氛中进行,例如在氮气或氩气中进行。
水性反应介质原则上还可包括少量水溶性有机溶剂,例如甲醇、乙醇、异丙醇、丁醇、戊醇以及丙酮等。然而聚合反应优选在没有这种溶剂的存在下进行。
在制备复合颗粒水分散体的方法中,除了上述组分外还可任选使用自由基链转移化合物,以减小或控制聚合所得到的聚合物的分子量。此类合适的化合物基本上包括脂族和/或芳脂族卤素化合物,例如正丁基氯、正丁基溴、正丁基碘、二氯甲烷、亚乙基二氯、氯仿、三溴甲烷、三氯溴甲烷、二溴二氯甲烷、四氯化碳、四溴化碳、苄基氯、苄基溴,有机含硫化合物如脂族伯、仲或叔硫醇,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、正十一硫醇及其异构体、正十二硫醇及其异构体、正十三硫醇及其异构体,取代硫醇如2-羟基乙硫醇,芳族硫醇如苯硫醇,邻、间或对甲基苯硫醇,以及公开在Polymer Handbook,第三版,1989,J.Brandrup和E.H.Immergut,JohnWiley & Sons,Section II,第133-141页中的所有其它含硫化合物;以及脂族和/或芳族醛,例如乙醛、丙醛和/或苯甲醛;不饱和脂肪酸,例如油酸;具有非共轭双键的二烯,例如二乙烯基甲烷;或乙烯基环己烷,或具有易于失去氢原子的烃,例如甲苯。然而,还可使用上述自由基链转移化合物互相相容的混合物。基于聚合单体的总量,任选使用的自由基链转移化合物的量通常为≤5重量%,经常≤3重量%,并且通常≤1重量%。
根据本发明使用的复合颗粒水分散体通常具有1-70重量%,经常5-65重量%,并且通常10-60重量%的总固体含量。
根据本发明使用的复合颗粒通常具有>10并且≤1000nm,通常≤500nm,经常≤250nm的粒径。粒径也通过AUC方法测定。所述值为已知为d50值的那些。
根据本发明有用的复合颗粒可具有不同结构。复合颗粒可包含一种或多种细碎固体颗粒。细碎固体颗粒可完全被聚合物基体包封。或者还可能是部分细碎固体颗粒被聚合物基体包封,而其余部分在聚合物基体表面上排列。当然还可能是大多数细碎固体颗粒粘合在聚合物基体的表面。
经常使用的特别是其复合颗粒由加聚物合成的复合颗粒分散体,所述聚合物可成膜并且最小成膜温度≤150℃,优选≤100℃,更优选≤50℃。由于在低于0℃时不再可能测量最小成膜温度,最小成膜温度的下限仅仅可通过玻璃化转变温度表征。玻璃化转变温度应不低于-60℃,优选不低于-30℃。最小成膜温度根据DIN 53 787或ISO 2115测定,并且玻璃化转变温度通过DIN 53 765(差示扫描量热法,20K/min,中点测量)测定。
与不包括含羟基的烷基氨基化合物的复合颗粒水分散体相比,通过本发明方法得到的复合颗粒水分散体具有明显更高的储藏稳定性。
本发明复合颗粒的分散体尤其适于制备含水配制剂,并且还可用作制备诸如压敏粘合剂、建筑粘合剂或工业粘合剂的粘合剂的原料,例如用于纸张涂料的粘料,乳胶漆,或用于塑料薄膜印刷用印刷油墨和印刷清漆,用于生产非织造布,以及例如在底漆中用于制造保护性涂层或水蒸气屏障。此外,通过本发明方法得到的复合颗粒的分散体可用于改进水泥配方和砂浆配方。通过本发明方法得到的复合颗粒通常还可用于医学诊断和其它医学应用(例如参见K.Mosbach和L.Andersson,Nature 270(1977),第259-261页;P.L.Kronick,Science 200(1978),第1074-1076页;和US-A4,157,323)。有利地,本发明复合颗粒分散体适于制备含水涂料组合物,例如乳胶漆、油墨或底漆等。
非常明显的是,包含复合颗粒水分散体和至少一种含羟基的烷基氨基化合物的含水配制剂同样具有明显增加的储藏稳定性,并因此可以在较长时间后可靠地加工。
实施例
I.复合颗粒水分散体的制备
在20-25℃(室温)、1巴(绝对)和氮气气氛下,经5分钟向装有回流冷凝器、温度计、机械搅拌器和计量装置的2升四颈烧瓶中搅拌(200rpm)装入416.6克Nyacol2040,然后加入2.5克甲基丙烯酸与12克浓度为10重量%的氢氧化钠水溶液的混合物。然后,经15分钟向搅拌的混合物中加入10.4克浓度为20重量%的非离子表面活性剂LutensolAT 18(BASF AG的商标名,平均具有18个氧化乙烯单元的C16C18脂肪醇乙氧基化物)和108.5克去离子水的混合物。然后,经60分钟将0.83克N-鲸蜡基-N,N,N-三甲基溴化铵(CTAB)在200克去离子水中的溶液计量加入到反应混合物中。然后将反应混合物加热到80℃的反应温度。
同时制备进料流1和进料流2,进料流1为由117.5克甲基丙烯酸甲酯、130克丙烯酸正丁酯和0.5克甲基丙烯酰氧基丙基三甲氧基硅烷的单体混合物,进料流2为由2.5克过硫酸钠、7克浓度为10重量%的氢氧化钠水溶液和200克去离子水组成的引发剂溶液。
随后经5分钟,从两个单独的进料管线将21.1克进料流1和57.1克进料流2加入到反应混合物中,在反应温度下搅拌。然后将反应混合物在反应温度下搅拌1小时。然后,将0.92克浓度为45重量%的Dowfax2A1水溶液加入到反应混合物中。然后经2小时,将进料流1和的剩余部分2同时开始连续计量加入反应混合物中。然后将反应混合物在反应温度下再搅拌1小时,然后冷却至室温。
基于复合颗粒水分散体的总重量,由此得到的复合颗粒水分散体具有的固体含量为35.1重量%。
II.性能测试
a)复合颗粒水分散体的储藏稳定性
为了测试储藏稳定性,在每种情况下,将50克上述复合颗粒水分散体与0.175克(基于复合颗粒水分散体的固体含量,相当于0.5重量%)和0.35克(基于复合颗粒水分散体的固体含量,相当于1重量%)浓度为50重量%的含羟基的烷基氨基化合物水溶液混合,将组分均匀混合,然后在70℃下将混合物储存在100毫升封闭样品瓶中,并每天肉眼检查胶凝(粘性激增,“蜜状”粘度)。表1列出了不同烷基氨基化合物得到的胶凝时间。
表1:用含羟基的烷基氨基化合物稳定的复合颗粒水分散体的胶凝时间,以天计
加入量 | ||
含羟基的烷基氨基化合物 | 0.5重量% | 1.0重量% |
无 | 6 | 6 |
三乙醇胺 | 7 | 9 |
二乙醇胺 | 7 | 9 |
2-氨基-2,2-二甲基乙醇 | 14 | 23 |
3-氨基丙-1-醇 | 17 | 26 |
1-氨基丙-2-醇 | 12 | 19 |
3-氨基丙-1,2-二醇 | 11 | 14 |
2-氨基-2-甲基丙-1,2-二醇 | 7 | 10 |
4-氨基丁-1-醇 | 17 | 34 |
2-氨基丁-1-醇 | 10 | 18 |
2-氨基-3-甲基丁-1-醇 | 13 | 17 |
5-氨基戊-1-醇 | 17 | 38 |
2-(2-氨基乙氧基)乙醇 | 9 | 11 |
b)含水涂料配制剂的储藏稳定性
在使用盘式搅拌器的1000rpm搅拌和室温下,使用列于下表的组分(以克计)制备两种颜料糊P1和P2。共混物的各组分以所述顺序添加。
组分 | P1 | P2 |
去离子水 | 140 | 148 |
生物杀伤剂(ActicidMBS,Thor) | 2 | 2 |
增稠剂(CollacralDS 6256,BASF AG) | 3 | 3 |
浓度为25重量%的氨水 | 0.5 | 0.5 |
2-氨基-2,2-二甲基乙醇 | 8 | - |
分散剂(PigmentverteilerMD 20,BASF AG) | 10 | 10 |
分散剂(CollacralLR 8954,BASF AG) | 10 | 10 |
消泡剂(TegoLA-E 511,Tego Chemie Service GmbH) | 2 | 2 |
颜料(二氧化钛,Kronos2190,Kronos Titan GmbH) | 120 | 120 |
填料(Omycarb5GU,Omya GmbH) | 40 | 40 |
填料(FinntalcM15,Omya GmbH) | 20 | 20 |
添加完成后,将两种颜料糊在1000rpm继续搅拌20分钟。然后将每种颜料糊都在搅拌下与1克消泡剂(Byk022,Byk-Chemie GmbH)、20克稀释到固体含量为5重量%的增稠剂溶液(CollacralLR 8990,BASF AG)、597克上述复合颗粒水分散体和27克去离子水混合。由此得到的含水涂料组合物在500rpm搅拌20分钟。在进一步测试之前,将涂料组合物在室温放置24小时。在上述放置期间,涂料组合物P2胶凝。
为了测试储藏稳定性,在50℃储藏14天之前和之后,分别在23℃使用ICI锥板式粘度计(根据ASTM D4287)和Brookfield KU 1粘度计(根据ASTM D562)测定含水涂料组合物P1的粘度。几乎根本没有发现粘度变化。
Claims (15)
1.一种用于改进由加聚物和细碎无机固体组成的颗粒(复合颗粒)的水分散体的储藏稳定性的方法,其中在在水性介质中制备复合颗粒分散体(复合颗粒水分散体)之前、期间或之后向水性分散介质中加入含羟基的烷基氨基化合物。
2.根据权利要求1所述的方法,其中在复合颗粒水分散体制备之后将含羟基的烷基氨基化合物加入到水性分散介质中。
3.根据权利要求1或2所述的方法,其中含有含羟基的烷基氨基化合物的复合颗粒水分散体具有≥7且≤11的pH。
4.根据权利要求1-3中任一项所述的方法,其中作为含羟基的烷基氨基化合物,使用具有至少三个碳原子和至少一个羟基和至少一个氨基的非环烷基化合物。
5.根据权利要求1-4中任一项所述的方法,其中烷基氨基化合物为伯胺。
6.根据权利要求1-5中任一项所述的方法,其中含羟基的烷基氨基化合物为具有至少三个碳原子且含有至少一个羟基和至少一个伯氨基的非环烷基化合物。
7.根据权利要求1-6中任一项所述的方法,其中基于复合颗粒水分散体的总量,含羟基的氨基化合物的量为0.01-10重量%。
8.根据权利要求1-7中任一项所述的方法,其中复合颗粒水分散体已经通过如下方法制备:将至少一种烯属不饱和单体分散分布在水性介质中,并且在至少一种分散分布的细碎无机固体和至少一种分散剂的存在下借助于至少一种自由基聚合引发剂通过自由基水乳液聚合方法聚合,其中:
a)使用所述至少一种无机固体的稳定的水分散体,所述分散体特征在于,在基于所述至少一种无机固体的水分散体为≥1重量%的初始固体浓度下,在其制备1小时后其仍含有分散形式的超过90重量%的初始分散固体,并且分散的固体颗粒具有≤100nm的重均直径,
b)所述至少一种无机固体的分散颗粒在标准氯化钾水溶液中,在对应于开始加入分散剂之前的水性分散介质pH的pH下显示出非零电泳淌度,
c)在开始加入所述至少一种烯属不饱和单体之前,将至少一种阴离子、阳离子和非离子分散剂加入到固体颗粒水分散体中,
d)然后,将总量的0.01-30重量%的所述至少一种单体加入到固体颗粒水分散体中,并聚合至至少90%的转化率,和
e)然后在聚合条件下以其消耗速率连续加入所述至少一种单体的其余部分。
9.根据权利要求1-8中任一项所述的方法,其中细碎无机固体为硅化合物。
10.根据权利要求9所述的方法,其中细碎无机固体为热解法二氧化硅和/或胶态二氧化硅和/或页硅酸盐。
11.根据权利要求1-10中任一项所述的方法,其中含羟基的氨基化合物为选自如下的化合物:2-氨基-2-甲基乙醇、2-氨基-2,2-二甲基乙醇、3-氨基丙-1-醇、3-氨基丙-2-醇、3-氨基丙-1,2-二醇、2-氨基-2-甲基丙-1,3-二醇、4-氨基丁-1-醇、2-氨基丁-1-醇、2-氨基-3-甲基丁-1-醇、5-氨基戊-1-醇、2-(2-氨基乙氧基)乙醇、6-氨基己-1-醇和7-氨基庚-1-醇。
12.通过根据权利要求1-11中任一项所述的方法得到的复合颗粒水分散体。
13.包含根据权利要求12所述的复合颗粒水分散体的含水涂料组合物。
14.根据权利要求12所述的复合颗粒水分散体用于制备含水涂料组合物的用途。
15.一种用于改进包含至少一种复合颗粒水分散体的含水配制剂的储藏稳定性的方法,其中在含水配制剂制备之前、期间或之后向水性配制介质中加入含羟基的烷基氨基化合物。
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PCT/EP2005/001913 WO2005083015A1 (de) | 2004-02-27 | 2005-02-24 | Verfahren zur verbesserung der lagerstabilität von kompositpartikel-dispersionen |
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CN102459419A (zh) * | 2009-06-03 | 2012-05-16 | 巴斯夫欧洲公司 | 改进水性复合颗粒分散体储存稳定性的方法 |
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CN102459419A (zh) * | 2009-06-03 | 2012-05-16 | 巴斯夫欧洲公司 | 改进水性复合颗粒分散体储存稳定性的方法 |
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WO2017054156A1 (en) * | 2015-09-30 | 2017-04-06 | Dow Global Technologies Llc | Shelf-stable aqueous composition and process of making the same |
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AU2005217083A1 (en) | 2005-09-09 |
BRPI0507919A (pt) | 2007-07-10 |
US20070161740A1 (en) | 2007-07-12 |
ATE551404T1 (de) | 2012-04-15 |
US7511090B2 (en) | 2009-03-31 |
CA2555101A1 (en) | 2005-09-09 |
BRPI0507919B1 (pt) | 2019-08-20 |
WO2005083015A1 (de) | 2005-09-09 |
EP1720949B1 (de) | 2012-03-28 |
CN1922277B (zh) | 2010-12-08 |
JP2007523987A (ja) | 2007-08-23 |
CA2555101C (en) | 2013-12-10 |
AU2005217083B2 (en) | 2010-04-01 |
EP1720949A1 (de) | 2006-11-15 |
ES2382042T3 (es) | 2012-06-04 |
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JP4523635B2 (ja) | 2010-08-11 |
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