CN102300940B - 在水中可再分散的可交联聚合物粉末化合物 - Google Patents
在水中可再分散的可交联聚合物粉末化合物 Download PDFInfo
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- CN102300940B CN102300940B CN201080006127.4A CN201080006127A CN102300940B CN 102300940 B CN102300940 B CN 102300940B CN 201080006127 A CN201080006127 A CN 201080006127A CN 102300940 B CN102300940 B CN 102300940B
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- water
- vinyl
- polymer powder
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- crosslinkable polymer
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
-
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
-
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract
本发明涉及在水中可再分散的可交联聚合物粉末组合物，其能通过以下步骤得到：选自具有1-15个碳原子的直链或支链烷基羧酸的乙烯基酯、具有1-15个碳原子的醇的甲基丙烯酸酯和丙烯酸酯、乙烯基芳族化合物、烯烃、二烯和卤乙烯的一种或多种单体在水性介质中进行自由基聚合，其中没有环氧官能共聚单体发生共聚合，然后干燥由此得到的聚合物分散体，其特征在于，在聚合之前和/或期间，以及/或者在干燥得到的聚合物分散体之前，加入环氧树脂，并且，如果合适，在干燥之后加入与环氧树脂交联的固化剂。
Description
本发明涉及在水中可再分散的可交联聚合物粉末组合物，其制备方法以及其用途。
在水中可再分散的聚合物粉末即(再)分散粉末是通过在干燥助剂(通常是保护性胶体)的存在下干燥相应的聚合物水分散体而得到的。由于保护性胶体的比例，首先防止聚合物颗粒在干燥过程中不可逆地粘着在一起，因为聚合物颗粒被水溶性保护性胶体颗粒包围。其次，该保护性胶体基体在聚合物粉末分散在水中时再次溶解，保证了水分散体中再次出现的聚合物颗粒具有起始分散体的粒径。
这种分散体粉末被用于各种应用中，例如用于涂料、各种基底的粘合剂中。最广泛的是其经常与水硬性胶结剂结合用于建筑化学产品中。所述建筑化学产品的实例有建筑粘合剂，特别是地砖粘合剂，抹灰和灰浆，涂料和填料，流平化合物，复合绝热体系和接缝灰浆。分散粉末的优点特别在于它们可以以制备好的可储存的任选与水硬性胶粘剂如水泥一起的干燥混合物的形式使用，使得它们在使用前添加水即可使用。这种干燥混合物比浆状体系更容易运输(没有水)并且在储存期间具有优势。
使用分散粉末特别是为了提高机械强度以及用其改性的灰浆在聚合物颗粒成膜时的粘合性。已知可对聚合物膜进行交联以进一步提高机械强度。
US-A 4028294公开了通过在乳液聚合中使用环氧树脂与单体的混合物来制备可交联聚合物胶乳。而且，为了获得可交联体系，在带有与环氧树脂交联的基团的环氧反应性共聚单体的存在下进行聚合。据说在所选的聚合温度下没有发生早期交联。其中没有描述在水中可再分散的聚合物粉末组合物的制备。US-A 4108819描述了在环氧树脂的存在下乙酸乙烯酯与乙烯的共聚合。为了防止早期交联，在聚合期间将pH保持在3-7。然后在制备的分散体中加入氨基固化剂。这些过程的一个缺点是有早期交联的危险，因为环氧基团和氨基固化剂均存在于水分散体中，因此在储存期间至少部分交联。其中没有描述在水中可再分散的聚合物粉末组合物的制备。在US6235811B1中，通过将乙酸乙烯酯(共)聚合物胶乳与液体环氧树脂或环氧树脂的水溶液混合，然后加入液体异佛尔酮二胺，来制备环氧改性的乙酸乙烯酯(共)聚合物的水分散体。这里，环氧树脂和胺交联剂也同时存在于液相中，这导致在长期储存时发生早期交联。DE 2601200描述了乙酸乙烯酯-乙烯共聚物水分散体，其是通过在环氧树脂存在下的聚合而得到的，其中添加胺交联剂。因为活性组分同时存在于水相中，这种体系容易发生早期交联。在US-A 4690988中，通过首先将聚环氧化物与烯键式不饱和羧酸反应，在乙烯化环氧树脂的存在下进一步聚合单体(乙烯基官能的增链单体)来得到聚合物改性的乙烯化环氧树脂。由此得到的聚合物的交联通过添加(氢)过氧化物来实现。在这种体系中难以排除早期交联。
根据US 2001/0024644A1，可交联分散粉末是通过烯键式不饱和单体与环氧官能单体在水性介质中进行共聚合，干燥分散体然后添加聚过氧化物而得到。缺点是交联效率较低。EP 0896029A1描述了一种方法，其中烯键式不饱和单体与含有可交联基团的共聚单体共聚合，干燥分散体，然后混入带有能与共聚物的可交联基团交联的官能团的固体颗粒。EP-A 723975A1公开了一种分散体粉末，其是通过苯乙烯和/或(甲基)丙烯酸酯与环氧官能共聚单体的共聚合而得到的。这个方法的缺点是在可交联的共聚单体的存在下聚合期间有早期交联的危险。EP 721004A2公开了聚合物粉末组合物，其包含聚合物粉末和多个粉末状交联组分，所述粉末状交联组分是通过将相应的液体施加到粉末状载体上而得到。然后粉末状交联组分彼此混合。其缺点是这种3组分体系的处理和这种混合物差的再分散性。
因此，本发明的目的是提供一种聚合物组合物，其尤其是在用于建筑化学产品中时产生防水膜，即使在不添加无机粘合剂的情况下，并且，在制备和储存期间有效防止早期交联。
本发明涉及在水中可再分散的可交联聚合物粉末组合物，其能通过以下步骤得到：选自具有1-15个碳原子的直链或支链烷基羧酸的乙烯基酯、具有1-15个碳原子的醇的甲基丙烯酸酯和丙烯酸酯、乙烯基芳族化合物、烯烃、二烯和卤乙烯的一种或多种单体在水性介质中进行自由基聚合，其中没有环氧官能共聚单体发生共聚合，然后干燥由此得到的聚合物分散体，其特征在于，在聚合之前和/或期间，以及/或者在干燥得到的聚合物分散体之前，加入环氧树脂，并且，如果合适，在干燥之后加入与环氧树脂交联的固化剂。
环氧树脂应理解为不能进行自由基聚合并且每分子具有至少两个环氧基团的环氧化合物。所述环氧化合物可以是脂肪族、芳代脂肪族或芳族的，例如双酚A型环氧化合物，即双酚A与表氯醇或甲基表氯醇的缩合物。通常含有双缩水甘油氧基苯基甲烷的混合物的基于双酚F的环氧树脂也是适合的。其它实例为脂肪族环氧化合物，例如脂肪族多元醇的缩水甘油醚，特别是丁基二缩水甘油醚；脂环族环氧树脂，例如乙烯基环己烷二氧化物、二环戊二烯二氧化物和3，4-环氧-6-甲基环己基甲基；和杂环环氧化合物，例如异氰尿酸三缩水甘油酯。这些环氧树脂是可商购的，例如双酚A和双酚F型的Epilox
树脂。
双酚A型环氧树脂和双酚F型环氧树脂是优选的。环氧树脂的用量，基于用于聚合的单体的总重量，为1-50重量％，优选5-30重量％。
合适的与环氧树脂交联的固化剂为在建筑化学产品的加工温度下，通常是环境温度下，一般为0-40℃下与环氧树脂交联的那些。优选与环氧树脂交联的胺。特别优选的胺为具有两个或更多个氨基的那些，例如脂肪族聚胺、聚氧化烯基胺、聚乙烯亚胺、氨基硅烷和其缩合物、氨基官能聚乙烯醇。最优选的是脂肪族聚胺，其可购的商品名为Anquamine
或Epilink
或Epilox
固化剂；或聚氧化烯基胺，其可购的商品名为Jeffamine
；或聚乙烯亚胺，其可购的商品名为Polyimin。最优选的还有氨基硅烷和其缩合物。合适的氨基硅烷为例如商品名为Geniosil
的那些，例如，N-(2-氨乙基)(3-氨丙基)三甲氧基硅烷(Geniosil GF 91)、(3-氨丙基)三乙氧基硅烷(GeniosilGF 93)、N-(2-氨乙基)(3-氨丙基)甲基二甲氧基硅烷(Geniosil GF 95)。
所述交联固化剂可以液体形式加入到在水中可再分散的用环氧树脂改性的聚合物粉末组合物中；优选交联固化剂以粉末形式使用。如果固化剂在标准条件下(DIN 50014 23/50)以液体形式存在，优选将固化剂施加到粉末状载体材料上或用保护性胶体例如聚乙烯醇封装，并以此形式使用。
合适的粉末状载体材料是本领域技术人员已知的，例如氧化硅，如硅胶或硅石(例如Sipernat
22)，粘土，二氧化钛，碳酸钙，合成树脂，如硅树脂。可通过已知方法来施用：可将液体固化剂与粉末状载体混合，然后得到用固化剂涂覆的粉末状载体颗粒。高粘性固化剂可在剪切下，例如在Retsch磨机中，与粉末状载体材料混合，以得到用固化剂涂覆的粉末状载体。
为了用保护性胶体微型封装，将固化剂与保护性胶体的水溶液混合，然后去除水，例如通过转鼓式干燥或喷雾干燥。
与环氧树脂交联的固化剂的用量取决于在聚合物粉末组合物中环氧基团对固化剂的官能团，优选氨基，的摩尔比。通常，使用的含环氧化物的粉末与固化剂的比例使得环氧基团对固化剂的官能团的摩尔比为0.5-2.0。
为了制备在水中可再分散的可交联聚合物粉末组合物的基础聚合物，合适的乙烯基酯为具有1-15个碳原子的羧酸的乙烯基酯。优选的乙烯基酯为乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、2-乙基己酸乙烯酯、月桂酸乙烯酯、1-甲基乙烯基乙酸酯、新戊酸乙烯酯、和具有9-13个碳原子的α-支链一元羧酸的乙烯酯(叔烷烃一元羧酸乙烯酯(vinyl versatate))例如VeoVa9或VeoVa10
(Resolution的商品名)。乙酸乙烯酯是特别优选的。合适的甲基丙烯酸酯或丙烯酸酯为具有1-15个碳原子的直链或支链醇的酯，例如丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸(正、异和叔)丁酯、甲基丙烯酸正丁酯、2-乙基己基丙烯酸酯、降冰片丙烯酸酯。丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸丁酯、2-乙基己基丙烯酸酯是优选的。烯烃和二烯的实例为乙烯、丙烯和1，3-丁二烯。合适的乙烯基芳族化合物为苯乙烯和乙烯基甲苯。合适的卤乙烯为氯乙烯。
如果合适，基于基础聚合物的总重量，也可共聚合0.05-10重量％，优选0.05至＜2重量％，特别优选0.05-1重量％的辅助单体。最优选不共聚合下述辅助单体，特别是不共聚合烯键式不饱和一元或二元羧酸。重要的是在制备基础聚合物时不共聚合环氧官能共聚单体。
辅助单体的实例为烯键式不饱和一元和二元羧酸，烯键式不饱和羧酰胺和腈，富马酸和马来酸的单酯和二酯，和马来酸酐，烯键式不饱和磺酸如乙烯基磺酸、2-丙烯酰胺基-2-甲基丙烷磺酸。其它实例为预交联共聚单体，例如多烯键式不饱和共聚单体，例如己二酸二乙烯酯、马来酸二烯丙基酯、甲基丙烯酸烯丙基酯或氰尿酸三烯丙基酯；或后交联共聚单体，例如丙烯酰胺基乙醇酸(AGA)、甲基丙烯酰胺基乙醇酸甲酯(MAGME)、N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺(NMMA)、N-羟甲基烯丙基氨基甲酸酯，N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺和N-羟甲基烯丙基氨基甲酸酯的烷基醚如异丁氧基醚或酯。其它实例为硅官能共聚单体，例如丙烯酰氧丙基三烷氧基硅烷和甲基丙烯酰氧丙基三烷氧基硅烷、乙烯基三烷氧基硅烷和乙烯基甲基二烷氧基硅烷。
在水中可再分散的可交联聚合物粉末组合物的合适的基础聚合物的实例为通过乙酸乙烯酯的聚合、乙酸乙烯酯与乙烯的共聚合、乙酸乙烯酯与乙烯和一种或多种其它乙烯基酯如叔烷烃一元羧酸乙烯酯或月桂酸乙烯酯的共聚合、氯乙烯与乙烯的共聚合、氯乙烯与乙烯和一种或多种乙烯基酯如乙酸乙烯酯和月桂酸乙烯酯的共聚合、乙酸乙烯酯与乙烯和一种或多种丙烯酸酯的共聚合、(甲基)丙烯酸酯的均聚和共聚、苯乙烯与一种或多种丙烯酸酯的共聚合、苯乙烯与1，3-丁二烯的共聚合得到的聚合物，如果合适，在这每种情况下还可共聚合辅助单体。
优选的是乙酸乙烯酯与1-40重量％的乙烯的共聚物；乙酸乙烯酯与1-40重量％的乙烯和1-50重量％的一种或多种选自以下组中的其它共聚单体的共聚物：在羧基中具有1-12个碳原子的乙烯基酯如丙酸乙烯酯、月桂酸乙烯酯，具有9-13个碳原子的α-支链羧酸的乙烯基酯(叔烷烃一元羧酸乙烯酯)如VeoVa9
、VeoVa10
、VeoVa11
；乙酸乙烯酯、1-40重量％的乙烯和优选1-60重量％的具有1-15个碳原子的直链或支链醇的(甲基)丙烯酸酯，特别是丙烯酸丁酯或丙烯酸2-乙基己酯的共聚物；包含30-75重量％的乙酸乙烯酯、1-30重量％的月桂酸乙烯酯或具有9-13个碳原子的α-支链羧酸的乙烯基酯、和1-30重量％的具有1-15个碳原子的直链或支链醇的(甲基)丙烯酸酯，特别是甲基丙烯酸甲酯、丙烯酸丁酯或丙烯酸2-乙基己酯的共聚物，其还包含1-40重量％的乙烯；包含乙酸乙烯酯和/或一种或多种选自羧基中具有1-12个碳原子的乙烯基酯的其它共聚单体、1-40重量％的乙烯和1-60重量的％氯乙烯的共聚物，这些共聚物也可含有所述量的所述辅助单体，并且以重量％表示的数据总和为100重量％。
还优选的是(甲基)丙烯酸酯聚合物，例如丙烯酸丁酯或丙烯酸2-乙基己酯或甲基丙烯酸甲酯与丙烯酸丁酯和/或丙烯酸2-乙基己酯和任选存在的乙烯的共聚物；包含苯乙烯和一种或多种选自以下组中的单体的苯乙烯-丙烯酸酯共聚物：丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸2-乙基己酯；包含一种或多种选自以下组中的单体和任选存在的乙烯的乙酸乙烯酯-丙烯酸酯共聚物：丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸2-乙基己酯；苯乙烯-1，3-丁二烯共聚物，这些共聚物也可含有所述量的所述辅助单体，并且以重量％表示的数据总和为100重量％。
选择单体或选择共聚单体的重量比使得玻璃转变温度Tg通常为-50～+50℃，优选-30～+50℃。聚合物的玻璃转变温度Tg可通过差示扫描量热法(DSC)以已知方式测定。也可通过Fox等式预先大致计算出Tg。根据Fox T.G.，Bull.Am.Physics Soc.1，3，page 123(1956)，下面的等式是正确的：1/Tg＝x1/Tg1+x2/Tg2+...+xn/Tgn，其中xn是单体n的质量分数(重量％)以及Tgn是单体n的均聚物的玻璃转变温度，以Kelvin表示。均聚物的Tg值在Polymer Handbook 2nd Edition，J.Wiley & Sons，New York(1975)中有描述。
制备基础聚合物的聚合通过乳液聚合法或悬浮聚合法，优选通过乳液聚合法来进行，聚合温度通常为40-100℃，优选为60-90℃。在气态共聚单体如乙烯、1，3-丁二烯或氯乙烯的共聚合中，也可以在通常为5-100bar的压力下进行。
使用通常用于乳液聚合或悬浮聚合的水溶性或溶于单体的引发剂或氧化还原引发剂组合来引发聚合。水溶性引发剂的实例为过二硫酸的钠、钾和铵盐、过氧化氢、叔丁基过氧化物、叔丁基氢过氧化物、过二磷酸钾、过氧化新戊酸叔丁酯、枯基过氧氢、异丙苯甲基单过氧化氢、偶氮二异丁腈。溶于单体的引发剂的实例为过二碳酸联十六烷酯、过二碳酸二环己酯、过氧化二苯甲酰。所述引发剂的用量，基于单体的总重量，通常为0.001-0.02重量％，优选为0.001-0.01重量％。
使用的氧化还原引发剂为所述引发剂与还原剂的组合。合适的还原剂为碱金属和铵的亚硫酸盐和重亚硫酸盐，例如亚硫酸钠；次硫酸的衍生物，例如锌或碱金属甲醛化次硫酸盐，例如甲醛次硫酸氢钠；和抗坏血酸。还原剂的用量，基于单体的总重量，通常为0.001-0.03重量％，优选为0.001-0.015重量％。
为了控制分子量，聚合期间可使用调节物质。如果使用调节剂，其用量基于待聚合的单体通常为0.01-5.0重量％，并且单独计量或与反应组分预先混合。这种物质的实例为正十二烷基硫醇、叔十二烷基硫醇、巯基丙酸、巯基丙酸甲酯、异丙醇和乙醛。
适用于聚合的保护性胶体为聚乙烯醇；聚乙烯醇缩醛；聚乙烯吡咯烷酮；水溶性多糖，例如淀粉(直链和支链)、纤维素和其羧甲基、甲基、羟乙基和羟丙基衍生物、糊精和环糊精；蛋白质，例如酪蛋白或酪蛋白酸盐、大豆蛋白、明胶；木质素磺酸盐；合成聚合物，例如聚(甲基)丙烯酸、(甲基)丙烯酸酯与羧基官能共聚单体单元的共聚物、聚(甲基)丙烯酰胺、聚乙烯基磺酸和其水溶性共聚物；磺化三聚氰胺甲醛树脂、磺化萘甲醛树脂、苯乙烯-马来酸共聚物和乙烯醚-马来酸共聚物；阳离子聚合物，例如聚DADMAC。
优选水解度为80-100mol％的部分水解或完全水解的聚乙烯醇，特别是水解度为80-95mol％、在4％浓度水溶液中
粘度为1-30mPa.s(在20℃下
方法，DIN 53015)的部分水解的聚乙烯醇。还优选水解度为80-95mol％、在4％浓度水溶液中
粘度为1-30mPa.s的经改性具有疏水性能的部分水解的聚乙烯醇。其实例为乙酸乙烯酯与疏水共聚单体的部分水解共聚物，所述疏水共聚单体例如乙酸异丙烯酯、新戊酸乙烯酯、乙基己酸乙烯酯、具有5或9-11个碳原子的饱和α-支链一元羧酸的乙烯酯、马来酸二烷基酯和富马酸二烷基酯如马来酸二异丙基酯和富马酸二异丙基酯、氯乙烯、乙烯基烷基醚如乙烯基丁基醚、烯烃如乙烯和癸烯。疏水单元的比例，基于部分水解的聚乙烯醇的总重量，优选为0.1-10重量％。也可以使用所述聚乙烯醇的混合物。
最优选水解度为85-94mol％、在4％浓度水溶液中
粘度为3-25mPa.s(在20℃下
方法，DIN 53015)的部分水解的聚乙烯醇。还最优选具有乙烯醇单元和所述量的具有5或9-11个碳原子的α-支链羧酸的乙烯酯单元的部分水解的聚乙酸乙烯酯。所述乙烯酯的实例为商品名为VeoVa5、VeoVa
9、VeoVa
10、VeoVa
11的那些叔烷烃一元羧酸乙烯酯。最优选的其它聚乙烯醇为部分水解的疏水化聚乙酸乙烯酯，其是通过同型聚合物反应得到的，例如乙烯醇单元与C1-C4醛如丁醛的缩醛化。疏水单元的比例，基于部分水解的聚乙酸乙烯酯的总重量，优选为0.1-10重量％。水解度为80-95mol％，优选85-94mol％，以及
粘度(DIN 53015，
方法，4％浓度水溶液)为1-30mPa.s，优选为2-25mPa.s。所述保护性胶体可通过本领域技术人员已知的方法得到，在聚合期间其加入量，基于单体的总重量，通常总共为1-20重量％。
如果在乳化剂的存在下进行聚合，其量基于单体的量为1-5重量％。优选不使用乳化剂。合适的乳化剂为阴离子、阳离子以及非离子乳化剂，例如阴离子表面活性剂，如链长为8-18个碳原子的烷基硫酸盐、疏水基团中具有8-18个碳原子并且具有最多40个环氧乙烷或环氧丙烷单元的烷基或烷基芳基醚硫酸盐、具有8-18个碳原子的烷烃磺酸盐或烷基芳基磺酸盐、磺基琥珀酸与一元醇或烷基酚的酯和单酯，或非离子表面活性剂，如具有8-40个环氧乙烷单元的烷基聚乙二醇醚或烷基芳基聚乙二醇醚。
在制备分散体时可在一开始将单体都加入(分批法)，或者一开始加入部分单体，剩余部分计量加入(半分批法)。一开始可将环氧树脂完全或部分与制备水一起加入。一开始也可将环氧树脂以在单体中的溶液形式完全或部分加入。在另一个实施方案中，环氧树脂可以在引发聚合之后完全或部分计量加入。例如溶解在单体中的环氧树脂可以分散在水中或以液体形式计量加入。环氧树脂也可以在聚合结束之后完全或部分加入到由此得到的聚合物分散体中，也就是在其干燥之前。在聚合之前或期间加入是优选的，环氧树脂也可以在聚合之前完全加入，或者在聚合期间完全计量加入，或者在聚合之前部分加入，其余部分在聚合期间计量加入。
通过本发明的方法得到的水分散体的固含量为30-75重量％，优选为45-60重量％。
为了制备在水中可再分散的聚合物粉末，如果合适在加入保护性胶体作为干燥助剂之后，干燥水分散体，例如通过流化床干燥、冷冻干燥或喷雾干燥。优选对分散体进行喷雾干燥。喷雾干燥在常规的喷雾干燥装置中进行，可以通过单流体、双流体或多流体喷嘴或通过转盘进行雾化。根据装置、树脂的Tg和期望的干燥度，通常在45-120℃，优选60-90℃的范围选择出口温度。
通常，干燥助剂的总用量，基于分散体的聚合物组分，为3-30重量％。这意味着在干燥之前保护性胶体的总用量，基于聚合物的比例，应该为至少3重量％至30重量％；基于聚合物的比例，优选用量为5-20重量％。
合适的干燥助剂为例如，部分水解的聚乙烯醇；聚乙烯吡咯烷酮；聚乙烯醇缩醛；水溶性多糖，例如淀粉(直链和支链)、纤维素和其羧甲基、甲基、羟乙基和羟丙基衍生物；蛋白质，例如酪蛋白或酪蛋白酸盐、大豆蛋白、明胶；木质素磺酸盐；合成聚合物，例如聚(甲基)丙烯酸、(甲基)丙烯酸酯与羧基官能共聚单体单元的共聚物、聚(甲基)丙烯酰胺、聚乙烯基磺酸和其水溶性共聚物；磺化三聚氰胺甲醛树脂、磺化萘甲醛树脂、苯乙烯-马来酸共聚物和乙烯醚-马来酸共聚物；阳离子聚合物，例如聚DADMAC。优选不再使用部分水解的聚乙烯醇形式的保护性胶体作为干燥助剂。
在喷雾期间，基于基础聚合物至多1.5重量％的消泡剂被证明在很多情况下是有利的。为了通过改善对结块的稳定性来提高储存性能，特别是对于具有低玻璃转变温度的粉末，可以对得到的粉末提供基于聚合物组分的总重量优选至多30重量％的防结块剂。防结块剂的实例为碳酸钙或碳酸镁、滑石、石膏、二氧化硅、高岭土、偏高岭土、粒径优选为10nm-10μm的硅酸盐。
通过固含量调整待喷雾的进料的粘度，以使其值为＜500mPa.s(在20转和23℃下的Brookfield粘度)，优选＜300mPa.s。待喷雾的分散体的固含量为＞35％，优选＞40％。
为了提高性能，可在喷雾期间加入其它添加剂。在优选的实施方案中分散体粉末组合物的其它组分为例如，颜料、填料、泡沫稳定剂和防水剂。
为了得到粉末状的可再分散交联聚合物粉末组合物，可在干燥之后将与环氧树脂交联的粉末状固化剂与分散粉末混合，优选在干燥之后立即混合。也可以采用以下程序：将在水中可再分散的可交联聚合物粉末，在使用之前，首先与粉末状的交联固化剂混合，优选就在使用之前进行混合。在水中可再分散的聚合物粉末与粉末状固化剂也可以分别单独使用。例如，在制备干灰浆组合物时，在水中可再分散的可交联聚合物粉末和粉末状固化剂可分别单独混合，任选与配制品的其它组分预先混合。
在制备糊状体系时，例如，也可以采用以下程序：将在水中可再分散的用环氧树脂改性的可交联聚合物粉末在使用之前与液体固化剂混合，优选就在使用之前进行混合。也可以将在水中可再分散的用环氧树脂改性的可交联聚合物粉末与固体或液体固化剂仅在混合水中混合：例如，将液体固化剂添加到混合水中，然后将在水中可再分散的用环氧树脂改性的可交联聚合物粉末和配制品的其它固体组分与该混合水混合。相反地，先将固体组分例如在水中可再分散的用环氧树脂改性的可交联聚合物粉末分散在混合水中，然后加入液体固化剂。
在水中可再分散的可交联聚合物粉末组合物可用于其典型的应用领域中，例如，任选与无机粘合剂如水泥(波特兰水泥、高铝水泥、粗面凝灰岩水泥、炉渣水泥、镁氧水泥或磷酸盐水泥)、石膏和水玻璃结合，用于建筑化学产品中，例如建筑粘合剂，特别是地砖粘合剂和复合绝热粘合剂，抹灰，填料，地板填料，流平化合物，浆料型密封涂料，接缝灰浆和涂料，以及用作涂料或粘合剂；或用作机织织物和无纺织物和纸张的涂料或粘合剂。
优选建筑化学产品以其干灰浆形式存在。典型的干灰浆配方是本领域技术人员已知的。基于配方的总重量，其含有0-50重量％，优选0.05-50重量％的无机粘合剂；5-80重量％的填料；0.1-10重量％的聚合物粉末组合物；0-30重量％的其它添加剂，配方中重量百分比数据总和为100重量％。合适的无机粘合剂为水泥、石膏、水玻璃或熟石灰。可使用的填料的实例为碳酸盐，例如白云石、方解石和白垩形式的碳酸钙。其它实例为硅酸盐，例如滑石形式的硅酸镁、或硅酸铝如沃土和粘土；石英粉，石英砂，细粒状二氧化硅，长石，重晶石和磨细石膏颜料。纤维填料也是合适的。在实践中，经常使用不同填料的混合物。其它添加剂的实例为颜料，例如作为无机颜料的二氧化钛，和常规的有机颜料。其它添加剂的实例为基于配方的总重量，比例通常为0.1-0.5重量％的润湿剂。其实例为多磷酸钠和钾、聚丙烯酸和其盐。可提及的其它添加剂为增稠剂，其用量基于配方的总重量通常为0.01-2.0重量％。常规的增稠剂为纤维素醚、淀粉或作为无机增稠剂的实例的斑脱土。其它添加剂为防腐剂、消泡剂、加气剂、增塑剂、阻燃剂、促进剂、防冻剂。
为了生产即用型建筑材料，在建筑工地将用在水中可再分散的可交联聚合物粉末组合物处理的干灰浆用需要量的水搅拌。
优选用于仅含有0.05-10重量％，特别优选0.05-3重量％的非常小量的无机粘合剂如水泥的建筑化学产品，在这些比例的无机粘合剂主要用于在灰浆固化期间粘合水，而不仅仅是用于建筑材料的凝固的情况下。最优选用于不含无机粘合剂，特别是不含水泥的建筑化学产品：例如，用于优选不含水泥的粉末状活性树脂接缝灰浆。这种接缝灰浆的典型配方通常含有50-80重量％的填料，例如砂和/或碳酸钙，和20-50重量％的在水中可再分散的可交联聚合物粉末组合物，所述组合物包括固化剂和如果合适，所述添加剂。
根据本发明的在水中可再分散的可交联聚合物粉末组合物与现有技术的区别在于由于固态聚集态，即使在两种交联组分(环氧化物和固化剂)都存在的情况下也不发生早期交联，因此这些混合物长时间保持稳定和耐储存。尽管在分散体粉末中有交联组分，也完全保留了再分散性。再分散在水中之后，得到快速凝固的交联剂体系，从而得到具有高机械强度的膜。在建筑领域中，用其得到例如硬化粘合剂灰浆和抹灰的产品，这些产品的显著之处在于即使没有添加无机粘合剂也具有高的拉伸强度。用本发明的在水中可再分散的可交联聚合物粉末组合物，还得到具有高的表面硬度的产品，例如在硬化接缝灰浆中。
以下实施例用于进一步说明本发明。
实施例1：
一开始将67重量份的去离子水、25重量份的部分水解的疏水聚乙烯醇的20重量％浓度水溶液和25重量份的部分水解聚乙烯醇的20重量％浓度水溶液加入到搅拌的高压釜中。用10重量％浓度甲酸调节pH至pH＝4。在搅拌下，在30分钟的时间内在30℃下计量加入包含25重量份的丙烯酸正丁酯和25重量份的苯乙烯的单体混合物。在300分钟内计量加入7重量份的叔丁基氢过氧化物的1％浓度水溶液和7重量份的甲醛次硫酸氢钠的1.5重量％浓度水溶液。当检测到反应开始时，将批料在45分钟内加热到70℃。反应开始40分钟后，在150分钟内计量加入25重量份丙烯酸正丁酯、25重量份苯乙烯和16重量份环氧树脂(Epilox F 17-00，双酚F树脂，来自Leuna Harze)的溶液。在单体计量加入结束后，再在120分钟内计量加入引发剂。
将100重量份的部分水解聚乙烯醇的10％浓度水溶液、0.2重量份的消泡剂和135重量份的水加入到200重量份的分散体(固含量约50％)中，并充分混合。将分散体通过双流体喷嘴喷雾。预先压缩到4bar的空气用作喷雾组分和形成的液滴通过用加热到125℃的空气的直流方法进行干燥。
将10重量％的可商购防结块剂(碳酸钙和高岭土的混合物)加入到得到的干燥粉末中。
对比实施例2：
类似于实施例1进行分散体的制备，但是不添加环氧树脂。所有其它过程与实施例1一致。
实施例3：
类似于实施例1进行分散体的制备，但是在干燥之前添加环氧树脂，在聚合期间不添加环氧树脂。
将35重量份的
粘度为4mPa.s和水解度为88mol％的部分水解聚乙烯醇的20％浓度水溶液、30重量份的
粘度为13mPa.s和水解度为88mol％的部分水解聚乙烯醇的11％浓度水溶液、0.2重量份的消泡剂、16重量份的环氧树脂(Epilox F 17-00)和135重量份的水加入到200重量份的分散体中，并充分混合。将分散体通过双流体喷嘴喷雾。预先压缩到4bar的空气用作喷雾组分和形成的液滴通过用加热到125℃的空气的直流方法进行干燥。
将12重量％的可商购防结块剂(碳酸钙和高岭土的混合物)加入到得到的干燥粉末中。
实施例4：
类似于实施例1进行分散体的制备，不同之处是在干燥分散体之前另外将16重量份的环氧树脂(Epilox F 17-00，双酚F树脂，来自Leuna Harze)加入到分散体中。
聚合物粉末的测试：
测定粉末的沉降行为(管式沉降)：
为了测定沉降行为，在每种情况下将50g分散体粉末再分散到50ml水中，然后稀释到0.5％固含量，测量100ml的该再分散体加入到刻度管中沉降1小时和24小时后的沉降高度。
测定抗结块性：
为了测定抗结块性，将分散体粉末装入到具有螺帽的铁管中，然后负载金属锤。负载之后，在50℃下的干燥烘箱中储存16小时。冷却到室温后，将粉末从管中取出，并通过粉碎粉末对抗结块稳定性进行定性测定。对抗结块稳定性进行如下分级：
1＝非常好的抗结块稳定性；2＝好的抗结块稳定性
3＝满意的抗结块稳定性；
4＝没有抗结块稳定性，在粉碎之后粉末不再是易流动的
表1
表1的结果表明根据本发明的可交联分散体粉末具有出色的再分散性，与常规的分散体粉末(没有环氧树脂的对比实施例2)不同。
性能测试：
为了测定膜强度，制备实施例1的粉末的50％浓度再分散体，并以所述摩尔混合比与所述固化剂混合。在根据DIN 53504的拉伸试验中测试干燥的膜。在水中储存7天之后，交联的膜保持完整，而未交联的膜已经被再分散。结果总结在表2中。结果表明膜有效交联。这表明用环氧树脂改性的可交联聚合物粉末组合物尽管有环氧树脂也很容易再分散。而且，还因此表明环氧官能对于胺交联剂而言是很容易获得的，并没有通过例如包含在聚合物基团中而失活。
类似地测试实施例3和4的分散体粉末。结果总结在表4和5中。
用表4所述的组合物(实施例3)也制备粉末的50％浓度再分散体，并以所述摩尔混合比与所述固化剂混合。将干燥的膜在水中储存3天，然后在根据DIN 53504的拉伸试验中进行测试。没有固化剂的参照膜在这个时间之后已经被再分散而不能再被测试。基于环氧化物/胺摩尔比为0.8的混合物的膜在湿态下测量时，显示出9.7MPa的拉伸强度，而基于环氧化物/胺摩尔比为1.2的混合物的膜在湿态下测量时，显示出5.1MPa的拉伸强度。
在另一系列测试中，测试填充砂的体系。将实施例1的粉末与砂(BCS413，平均粒径130μm)以1∶2的重量比混合，以所述摩尔混合比与所述固化剂混合，并再分散。将干燥的膜在根据DIN 53504的拉伸试验中进行测试。这些膜在水中储存7天后也保持完整，而未交联的膜被再分散。结果总结在表3中。
表2(实施例1)
表3(实施例1)
表4(实施例3)
表5(实施例4)
Claims (18)
1.在水中可再分散的可交联聚合物粉末组合物，其能通过以下步骤得到：选自具有1-15个碳原子的直链或支链烷基羧酸的乙烯基酯、具有1-15个碳原子的醇的甲基丙烯酸酯和丙烯酸酯、乙烯基芳族化合物、烯烃、二烯和卤乙烯的一种或多种单体在水性介质中进行自由基聚合，其中没有环氧官能共聚单体发生共聚合，然后干燥由此得到的聚合物分散体，其特征在于，在聚合之前和/或期间，以及/或者在干燥得到的聚合物分散体之前，加入环氧树脂，并且，如果合适，在干燥之后加入与环氧树脂交联的固化剂。
2.权利要求1的在水中可再分散的可交联聚合物粉末组合物，其特征在于，在干燥所述组合物之后将与所述环氧树脂交联的粉末状固化剂与所述在水中可再分散的可交联聚合物粉末组合物混合。
3.权利要求1的在水中可再分散的可交联聚合物粉末组合物，其特征在于仅在其使用之前将与所述环氧树脂交联的粉末状固化剂混入。
4.权利要求1-3之一的在水中可再分散的可交联聚合物粉末组合物，其特征在于所用的固化剂是与所述环氧树脂交联的胺。
5.权利要求4的在水中可再分散的可交联聚合物粉末组合物，其特征在于所用的胺为选自以下组中的具有两个或更多个氨基的那些胺：脂肪族聚胺、聚氧化烯基胺、聚乙烯亚胺、氨基硅烷和其缩合物、氨基官能聚乙烯醇。
6.权利要求1-5之一的在水中可再分散的可交联聚合物粉末组合物，其特征在于，基础聚合物是通过乙酸乙烯酯的聚合、乙酸乙烯酯与乙烯的共聚合、乙酸乙烯酯与乙烯和一种或多种其它乙烯基酯的共聚合、氯乙烯与乙烯的共聚合、氯乙烯与乙烯和一种或多种乙烯基酯的共聚合、或乙酸乙烯酯与乙烯和一种或多种丙烯酸酯的共聚合、或（甲基）丙烯酸酯的均聚和共聚、或苯乙烯与一种或多种丙烯酸酯的共聚合、或苯乙烯与1,3-丁二烯的共聚合而得到的，如果合适，在每种情况下还可以共聚合辅助单体。
7.权利要求6的在水中可再分散的可交联聚合物粉末组合物，其中在乙酸乙烯酯与乙烯和一种或多种其它乙烯基酯的共聚合中，所述其它乙烯基酯选自叔烷烃一元羧酸乙烯酯和月桂酸乙烯酯；在氯乙烯与乙烯和一种或多种乙烯基酯的共聚合中，所述乙烯基酯选自乙酸乙烯酯和月桂酸乙烯酯。
8.制备权利要求1-7之一的在水中可再分散的可交联聚合物粉末组合物的方法，所述方法是通过自由基乳液聚合或悬浮聚合。
9.权利要求8的制备在水中可再分散的可交联聚合物粉末组合物的方法，其特征在于环氧树脂在聚合之前或期间加入，其中环氧树脂可以在聚合之前完全加入，或者在聚合期间完全计量加入，或者在聚合之前部分加入，其余部分在聚合期间计量加入。
10.权利要求1-7之一的在水中可再分散的可交联聚合物粉末组合物在建筑化学产品中的用途。
11.权利要求1-7之一的在水中可再分散的可交联聚合物粉末组合物的用途，所述用途是在涂料或粘合材料中用作粘合剂，或在机织织物和无纺织物和纸张中用作涂料或粘合剂。
12.权利要求10的用途，其是用于生产建筑粘合剂、抹灰、填料、地板填料、流平化合物、浆料型密封涂料、接缝灰浆和涂料。
13.权利要求10或12的用途，其是用在干灰浆组合物中。
14.权利要求10的用途，其特征在于存在0.05-10重量%的无机粘合剂。
15.权利要求10的用途，其特征在于不存在无机粘合剂。
16.权利要求14或15的用途，其是用在活性树脂接缝灰浆中。
17.权利要求10或11的用途，其特征在于，在制备干组合物时，将所述在水中可再分散的可交联聚合物粉末组合物与粉末状固化剂分别单独混合，任选与配方中的其它组分预混合。
18.权利要求10或11的用途，其特征在于，在制备糊状组合物时，将所述在水中可再分散的可交联聚合物粉末组合物在使用前与液体固化剂混合，或者将在水中可再分散的可交联聚合物粉末组合物与固化剂仅在混合水中混合。
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| DE102010003919A1 (de) | 2010-04-13 | 2011-10-13 | Wacker Chemie Ag | Oberflächenbehandlung von zementären Untergründen |
| DE102011076407A1 (de) | 2011-05-24 | 2012-11-29 | Wacker Chemie Ag | Verfahren zur Herstellung von Schutzkolloid-stabilisierten Polymerisaten |
| US9758667B2 (en) | 2012-10-03 | 2017-09-12 | Rohm And Haas Company | Alkali-soluble resin (ASR) shell epoxy RDP exhibiting improved shelf stability |
| DE102012220149B4 (de) * | 2012-11-06 | 2014-12-11 | ibex Beteiligungs- und Managementgesellschaft mbH | Zusammensetzung mit Kapseln, deren Verwendung sowie ein Verfahren zum Verfugen von Wand- und Bodenbelägen |
| DE102013219325A1 (de) | 2013-09-25 | 2015-03-26 | Wacker Chemie Ag | Verwendung von modifizierten wasserlöslichen Polymeren als Vernetzungshilfsmittel |
| DE102014220859A1 (de) | 2014-10-15 | 2016-04-21 | Wacker Chemie Ag | Verwendung von in Wasser redispergierbaren Polymerpulver-Zusammensetzungen mit kationischer Funktionalität als Flockungshilfsmittel |
| WO2017021917A1 (en) * | 2015-08-06 | 2017-02-09 | Basf Se | Finely divided, anionic, aqueous polymer dispersions, processes for the preparation and use as sizes in papermaking |
| ES2938644T3 (es) * | 2017-05-31 | 2023-04-13 | Sika Tech Ag | Mortero monocomponente de cemento resina epoxi |
| CN113508157A (zh) * | 2019-02-26 | 2021-10-15 | 瓦克化学股份公司 | 可再分散于水中的可交联聚合物粉末组合物 |
| WO2020178457A1 (en) * | 2019-03-07 | 2020-09-10 | Sika Technology Ag | Cementitious hybrid flooring composition |
| BR112021010033A2 (pt) * | 2019-03-21 | 2021-10-13 | Sika Technology Ag | Composição à base de água com transparência aprimorada |
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| US6235811B1 (en) | 1999-06-08 | 2001-05-22 | Air Products And Chemicals, Inc. | Epoxy resin-vinyl acetate polymer blends |
| DE10004319C2 (de) | 2000-02-01 | 2002-04-18 | Wacker Chemie Gmbh | Vernetzbare Polymerzusammensetzung, Verfahren zur Herstellung und Verwendung derselben |
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| US3652723A (en) * | 1970-11-16 | 1972-03-28 | Ford Motor Co | Thermoset molding powders employing polycarboxyl functional prepolymer and diepoxide crosslinking agent |
| CN101168577A (zh) * | 2006-10-25 | 2008-04-30 | 瓦克聚合系统两合公司 | 包括二聚表面活性剂的分散粉末组合物 |
| CN100999612A (zh) * | 2006-11-30 | 2007-07-18 | 许富安 | 改进耐水粘结性能的可再分散聚合物粉末的制备方法及其用途 |
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| WO2010086217A2 (de) | 2010-08-05 |
| CN102300940A (zh) | 2011-12-28 |
| BRPI1008108A2 (pt) | 2016-03-08 |
| IN2011CN05532A (zh) | 2015-08-21 |
| EP2391659A2 (de) | 2011-12-07 |
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