CN108117832B - 双固化型单组份聚脲涂料及其制备方法 - Google Patents
双固化型单组份聚脲涂料及其制备方法 Download PDFInfo
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- CN108117832B CN108117832B CN201810003598.8A CN201810003598A CN108117832B CN 108117832 B CN108117832 B CN 108117832B CN 201810003598 A CN201810003598 A CN 201810003598A CN 108117832 B CN108117832 B CN 108117832B
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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
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- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
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- 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
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- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4808—Mixtures of two or more polyetherdiols
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
一种双固化型单组份聚脲涂料，按照重量份包括：二异氰酸酯，100‑500份，聚醚多元醇，200‑500份，干性油，100‑350份，溶剂，100‑350份，催化剂1，1‑3份，催化剂2，0.00‑0.1份，催化剂3，0.1‑3份，偶联剂，2‑5份，消泡剂1‑2份，颜填料，100‑200份，封闭胺类固化剂，2‑10份。还提供一种双固化型单组份聚脲涂料的制备方法，上述双固化型单组份聚脲涂料不易起泡、力学性能强。
Description
技术领域
本发明属于聚脲涂料领域，特别涉及一种双固化型单组份聚脲涂料及其制备方法。
背景技术
聚脲技术是近年来新兴的涂膜技术，可以在基材表面形成连续的、高强度、高延伸的保护层，防止基材裂纹及腐蚀，提高结构耐久性。双组份喷涂型聚脲，因其具有优异的理化性能、突出的防腐性能、快速固化等优点，而被广泛应用于防腐、防水、耐磨等工程中。但双组份喷涂聚脲必须使用配套设备，精确控制1:1的体积比，设备价格及维护成本高，施工专业要求高。
单组份聚脲涂料具有与基材附着力好、突出的耐候及耐磨特性；施工时可采用传统的刷、刮、滚涂等方式，也可采用单组份高压喷涂方式，无须使用价格昂贵的配套设备，可有效避免配比不准确带来的问题。可以广泛应用于港口、桥梁、码头、堤坝、水利建设地下工程等领域。
单组份聚脲以异氰酸酯树脂为主体结构，采用封端聚醚胺和封端与聚醚胺反应的官能团(如NCO)。封端基团在有湿气的条件下参与反应，进一步交联固化，形成聚脲。所以环境的温湿度对其表干和固化影响很大，湿度太大，则表干过快，水分不能进入到底层，造成固化不完全，同时反应产生的二氧化碳气体不能及时排除而造成鼓泡现象；湿度过低，则整体反应过慢，影响施工效率和表面清洁度。
发明内容
基于此，有必要提供一种不易起泡、力学性能强的双固化型单组份聚脲涂料及其制备方法。
一种双固化型单组份聚脲涂料，按照重量份包括：
在其中一个实施例中，所述二异氰酸酯为芳香族异氰酸酯或脂肪族类的异氰酸酯。
在其中一个实施例中，所述聚醚多元醇为聚醚PPG2000、聚醚PPG1000、PTMG1000、PTMG2000、聚醚330N、聚醚3050中的至少一种。
在其中一个实施例中，所述干性油为亚麻油、脱水蓖麻油、油酸、亚油酸、亚麻酸和桐油酸中的至少一种。
在其中一个实施例中，所述偶联剂为硅烷偶联剂，所述消泡剂为BYK066N。
在其中一个实施例中，所述溶剂为醋酸丁酯、丙二醇甲醚醋酸酯、醋酸正丙酯、醋酸乙酯、异佛尔酮、环己酮中的至少一种。
在其中一个实施例中，所述颜填料为轻钙、碳酸钙、改性碳酸钙、硫酸钡、硫酸钙和氢氧化钙、氧化镁、氧化钙中的至少一种。
在其中一个实施例中，所述催化剂1为固体超强酸，催化剂2为有机锡类催化剂，催化剂3为钴盐和锰盐中的至少一种。
在其中一个实施例中，所述封闭胺类固化剂为酮亚胺和噁唑烷的至少一种。
一种如上所述的双固化型单组份聚脲涂料的制备方法，包括：
按照重量组分，将100-350份干性油和200-500份聚醚多元醇加入至100-350份的溶剂中，再加入1-3份催化剂1，在氮气保护下搅拌，加热到回流，并在回流温度下反应4～10小时，过滤出催化剂1，并真空条件下脱水，降温至65℃后加入0.00-0.1份催化剂2，搅拌均匀后再加入100-500份二异氰酸酯，然后升温至85℃反应1.5～2小时，降温到60℃，然后加入2-5份偶联剂、1-2份消泡剂、0.1-3份催化剂3、2-10份封闭胺类固化剂及100-200份颜填料，得到双固化型单组份聚脲涂料。
在上述双固化型单组份聚脲涂料及其制备方法中，通过活泼亚甲基与氧气反应进而产生交联反应，催化剂传递氧气的作用强，能使涂料表干加快，具有较好的光泽度；再利用封端聚醚胺的湿气固化反应使底层固化完全，达到体系的“实干”，湿气固化表现出较好的冲击强度和柔韧性。利用这种双重固化反应机理能够实现涂层的全面固化。得到的双固化型单组份聚脲涂料储存稳定性好，干燥迅速，不易起泡，力学性能强。
具体实施方式
下面结合实施方式，对一种双固化型单组份聚脲涂料及其制备方法作进一步的详细说明。
一实施方式的双固化型单组份聚脲涂料，按照重量份包括：
上述双固化型单组份聚脲涂料储存稳定性好，干燥迅速，不易起泡，力学性能强。
在一实施方式中，二异氰酸酯为芳香族异氰酸酯，如二苯基甲烷二异氰酸酯(Diphenyl-methane-diisocyanate，MDI)，甲苯二异氰酸酯(Toluene-2,4-diisocyanate，TDI)，苯二亚甲基二异氰酸酯(Xylene Diisocyanate，XDI)等中的一种或多种，也可以是脂肪族类的异氰酸酯，如异佛尔酮二异氰酸酯(isophorone diisocyanate，IPDI)，六亚甲基二异氰酸酯(Hexamethylene Diisocyanate，HDI)，4,4'-二环己基甲烷二异氰酸酯(Methylene-bis(4-cyclohexylisocyanate)，HMDI)中的一种或多种。
在一实施方式中，所述聚醚多元醇为聚醚PPG2000、聚醚PPG1000、聚四氢呋喃多元醇PTMG1000、PTMG2000、聚醚330N、聚醚3050中的至少一种。
在一实施方式中，干性油为双键数≥2个的双键干性油，即每个干性油分子必须有两个或两个以上的活泼亚甲基。优选地，干性油为亚麻油、脱水的蓖麻油、油酸(十八碳烯-9-酸)、亚油酸(十八碳二烯-9，12-酸)、亚麻酸(十八碳三烯-9,12,15-酸)、桐油酸(十八碳三烯-9,11,13-酸)。
在一实施方式中，偶联剂为硅烷偶联剂，优选为硅烷偶联剂KH550、硅烷偶联剂KH560。
在一实施方式中，溶剂为醋酸丁酯、丙二醇甲醚醋酸酯、醋酸正丙酯、醋酸乙酯、异佛尔酮和环己酮中的至少一种。
在一实施方式中，消泡剂为BYK066N。
在一实施方式中，颜填料为轻钙、碳酸钙、改性碳酸钙、硫酸钡、硫酸钙、氢氧化钙、氧化镁和氧化钙中的至少一种。优选地，颜填料在使用前进行烘干脱水处理。
在一实施方式中，催化剂1为固体超强酸，优选地，可以为SO4 2-/MxOy固体超强酸；催化剂2为有机锡类催化剂，优选地选自二月桂酸二丁基锡和二月桂酸二正辛基锡中的一种，催化剂3为钴盐和锰盐中的至少一种。如果没有催化剂的作用，反应速率很慢。采用钴盐和锰盐中的至少一种作为催化剂，可以加速过氧化物的分解。同时钴盐也有助于体系吸氧和氢过氧化物的形成。催化剂传递氧的作用强，能使涂料表干加快。体系在发生氧化反应的同时，湿固化反应也同时进行。氧化反应开始过程中交联形成的结构有利于湿气固化。湿固化原理是环境中的水分子与体系内封端的聚醚胺反应，生产聚醚胺，聚醚胺再与异氰酸酯反应生成聚脲。
在一实施方式中，封闭胺类固化剂包含但不限于酮亚胺及噁唑烷类物质。如3-丁基-2-(1-乙基戊基)噁唑烷、3-羟乙基-1,3噁唑烷、2-异丙基-3-羟乙基-1,3噁唑烷、2-苯基-3-羟乙基-1,3-噁唑烷中的至少一种。
一实施方式的双固化型单组份聚脲涂料的制备方法，包括：
按照重量组分，将100-350份干性油和200-500份聚醚多元醇加入至100-350份的溶剂中，再加入1-3份催化剂1，在氮气保护下搅拌，加热到回流，并在回流温度下反应4～10小时，过滤出催化剂1，并真空条件下脱水，降温至65℃后加入0.00-0.1份催化剂2，搅拌均匀后再加入100-500份二异氰酸酯，然后升温至85℃反应1.5～2小时，降温到60℃，然后加入2-5份偶联剂、1-2份消泡剂、0.1-3份催化剂3、2-10份封闭胺类固化剂及100-200份颜填料，得到双固化型单组份聚脲涂料。
在一实施方式中，二异氰酸酯为芳香族异氰酸酯，如二苯基甲烷二异氰酸酯(Diphenyl-methane-diisocyanate，MDI)，甲苯二异氰酸酯(Toluene-2,4-diisocyanate，TDI)，苯二亚甲基二异氰酸酯(Xylene Diisocyanate，XDI)等中的一种或多种，也可以是脂肪族类的异氰酸酯，如异佛尔酮二异氰酸酯(isophorone diisocyanate，IPDI)，六亚甲基二异氰酸酯(Hexamethylene Diisocyanate，HDI)，4,4'-二环己基甲烷二异氰酸酯(Methylene-bis(4-cyclohexylisocyanate)，HMDI)中的一种或多种。
在一实施方式中，所述聚醚多元醇为聚PPG2000、聚醚PPG1000、聚四亚甲基醚二醇PTMG1000、PTMG2000、聚醚330N、聚醚3050中的至少一种。
在一实施方式中，干性油为双键数≥2个的双键干性油，即每个干性油分子必须有两个或两个以上的活泼亚甲基。优选地，干性油为亚麻油、脱水的蓖麻油、油酸(十八碳烯-9-酸)、亚油酸(十八碳二烯-9，12-酸)、亚麻酸(十八碳三烯-9,12,15-酸)、桐油酸(十八碳三烯-9,11,13-酸)。
在一实施方式中，偶联剂为硅烷偶联剂，优选为硅烷偶联剂KH550、硅烷偶联剂KH560。
在一实施方式中，溶剂为醋酸丁酯、丙二醇甲醚醋酸酯、醋酸正丙酯、醋酸乙酯、异佛尔酮和环己酮中的至少一种。
在一实施方式中，颜填料为轻钙、碳酸钙、改性碳酸钙、硫酸钡、硫酸钙、氢氧化钙、氧化镁和氧化钙中的至少一种。优选地，颜填料在使用前进行烘干脱水处理。
在一实施方式中，催化剂1为固体超强酸,SO4 2-/MxOy固体超强酸；催化剂2为有机锡类催化剂,二月桂酸二丁基锡和二月桂酸二正辛基锡中的一种，催化剂3为钴盐和锰盐中的至少一种。
首先，干性油与聚醚多元醇在催化剂1的作用下发生酯化反应，生成羟基封端的含有双键的酯类。生成的这个酯类再与二异氰酸酯反应,生成含有双键的预聚体P。然后加入封闭胺类固化剂及其他助剂。
单组份涂料的固化反应机理分为两部分：一方面，含有预聚体P中的双键在空气中氧化交联形成一层膜。P中的不饱和双键在氧气的作用下打开，可以形成微小的网状结构。反应过程可用下式表示：
此过程采用钴盐和锰盐中的至少一种作为催化剂，可以加速过氧化物的分解。同时钴盐也有助于体系吸氧和氢过氧化物的形成。催化剂传递氧的作用强，能使涂料表干加快。
另一方面，体系在发生氧化反应的同时，湿固化反应也同时进行。氧化反应开始过程中交联形成的结构有利于湿气固化。湿固化原理是环境中的水分子与体系内封端聚醚胺反应，生产聚醚胺，聚醚胺再与异氰酸酯反应生成聚脲。反应原理如下式所示：
在一实施方式中，封闭胺类固化剂为3-丁基-2-(1-乙基戊基)噁唑烷、3-羟乙基-1,3噁唑烷、2-异丙基-3-羟乙基-1,3噁唑烷、2-苯基-3-羟乙基-1,3-噁唑烷中的至少一种。
上述双固化型单组份聚脲涂料的制备方法中，通过活泼亚甲基与氧气反应进而产生交联反应，催化剂传递氧气的作用强，能使涂料表干加快，具有较好的光泽度；再利用封端聚醚胺的湿气固化反应使底层固化完全，达到体系的“实干”，湿气固化表现出较好的冲击强度和柔韧性。利用这种双重固化反应机理能够实现涂层的全面固化。得到的双固化型单组份聚脲涂料储存稳定性好，干燥迅速，不易起泡，力学性能强。
根据本申请技术方案获得的双固化型单组份聚脲涂料的性能参数如表1所示，其中本产品表示根据本申请技术方案制得的产品，市面产品为采用常规方法获得的产品。
表1
实施例l
一种双固化型单组份聚脲涂料，包括以下重量份的组份：
采用的亚油酸是大豆油，经高压水解压滤蒸馏制得的，以亚油酸为主，包括软质酸油酸亚麻酸在内的C16-C18脂肪酸的混合物，亚油酸的酸值大于190mgKOH/g，碘值大于140.5g/mg。分别将亚油酸和聚醚PPG1000按一定比例(摩尔比1:1)加入带有搅拌器温度计分水器冷凝管的四口瓶中，四口瓶中装有醋酸丁酯，再加入催化剂SO4 2-/MxOy固体超强酸，用磁力搅拌器在氮气保护下搅拌，加热到回流，并在混回流温度下反应4到10小时。过滤固体催化剂，并真空条件下脱水，2小时，降温达到60℃一下后加入二苯基甲烷二异氰酸酯，85℃条件下反应1.5～2小时，降温到60℃。然后加入上述偶联剂、消泡剂、钴盐催化剂、封闭胺类固化剂、颜填料。可以制得双固化型单组份聚脲涂料。得到的双固化型单组份聚脲涂料主要技术指标如下表2所述。
表2
实施例2
一种双固化型单组份聚脲涂料，包括以下重量份的组份：
其中，采用的亚麻酸，将亚麻酸和聚醚PPG1000与聚醚3050按一定比例(摩尔比1:0.5：0.5)加入带有搅拌器温度计分水器冷凝管的四口瓶中，四口瓶装有溶剂醋酸正丙酯，再加入催化剂SO4 2-/MxOy固体超强酸，用磁力搅拌器在氮气保护下搅拌，加热到回流，并在混回流温度下反应4到10小时。过滤超强酸催化剂，并真空条件下脱水，2小时，降温达到60℃以下后加入以下后加入二月桂酸二丁基锡搅拌均匀再4,4'-二环己基甲烷二异氰酸酯，85℃条件下反应1.5～2小时，降温到60℃。然后加入偶联剂、消泡剂、锰盐催化剂、封闭胺类固化剂、颜填料，得到双固化型单组份聚脲涂料。
本实施例所得的双固化型单组份聚脲涂料的性能如下表3所示：
表3
实施例3
一种双固化型单组份聚脲涂料，包括以下重量份的组份：
其中，采用的桐油酸，将桐油酸和聚醚PPG1000与330N按一定比例(摩尔比1:0.5：0.5)加入带有搅拌器温度计分水器冷凝管的四口瓶中，四口瓶装有溶剂醋酸正丙酯，再加入催化剂SO4 2-/MxOy固体超强酸，用磁力搅拌器在氮气保护下搅拌，加热到回流，并在混回流温度下反应4到10小时。过滤超强酸催化剂，并真空条件下脱水，2小时，降温达到60℃以下后加入二月桂酸二丁基锡搅拌均匀后加入异佛尔酮二异氰酸酯，85℃条件下反应1.5～2小时，降温到60℃。然后加入偶联剂、消泡剂、锰盐催化剂、封闭胺类固化剂、颜填料，得到双固化型单组份聚脲涂料。
溶剂为醋酸正丙酯，封闭胺类固化剂为醛亚胺，氧化镁和氧化钙1:1复配。
本实施例所得的双固化型单组份聚脲涂料的性能如下表4所示：
表4
根据上述实施例可知，采用本申请的技术方案获得的产品的拉升强度大，最大伸长率大，撕裂强度高，表干时间和实干时间大大缩短。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (8)
1.一种双固化型单组份聚脲涂料，其特征在于，按照重量份包括：
所述干性油为亚麻油、脱水蓖麻油、油酸、亚油酸、亚麻酸和桐油酸中的至少一种；
所述催化剂1为固体超强酸，催化剂2为有机锡类催化剂，催化剂3为钴盐和锰盐中的至少一种。
2.根据权利要求1所述的双固化型单组份聚脲涂料，其特征在于，所述二异氰酸酯为芳香族异氰酸酯或脂肪族类的异氰酸酯。
3.根据权利要求1所述的双固化型单组份聚脲涂料，其特征在于，所述聚醚多元醇为聚醚PPG2000、聚醚PPG1000、PTMG1000、PTMG2000、聚醚330N和聚醚3050中的至少一种。
4.根据权利要求1所述的双固化型单组份聚脲涂料，其特征在于，所述偶联剂为硅烷偶联剂，所述消泡剂为BYK066N。
5.根据权利要求1所述的双固化型单组份聚脲涂料，其特征在于，所述溶剂为醋酸丁酯、丙二醇甲醚醋酸酯、醋酸正丙酯、醋酸乙酯、异佛尔酮和环己酮中的至少一种。
6.根据权利要求1所述的双固化型单组份聚脲涂料，其特征在于，所述颜填料为轻钙、碳酸钙、改性碳酸钙、硫酸钡、硫酸钙、氢氧化钙、氧化镁和氧化钙中的至少一种。
7.根据权利要求1所述的双固化型单组份聚脲涂料，其特征在于，所述封闭胺类固化剂为酮亚胺和噁唑烷的至少一种。
8.一种如权利要求1所述的双固化型单组份聚脲涂料的制备方法，其特征在于，包括：
按照重量组分，将100-350份干性油和200-500份聚醚多元醇加入至100-350份的溶剂中，再加入1-3份催化剂1，在氮气保护下搅拌，加热到回流，并在回流温度下反应4～10小时，过滤出催化剂1，并真空条件下脱水，降温至65℃后加入0.00-0.1份催化剂2，搅拌均匀后再加入100-500份二异氰酸酯，然后升温至85℃反应1.5～2小时，降温到60℃，然后加入2-5份偶联剂、1-2份消泡剂、0.1-3份催化剂3、2-10份封闭胺类固化剂及100-200份颜填料，得到双固化型单组份聚脲涂料。
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