CN110951385A - 一种环氧改性的聚氨酯防水涂料及其制备方法 - Google Patents
一种环氧改性的聚氨酯防水涂料及其制备方法 Download PDFInfo
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- CN110951385A CN110951385A CN201911322180.4A CN201911322180A CN110951385A CN 110951385 A CN110951385 A CN 110951385A CN 201911322180 A CN201911322180 A CN 201911322180A CN 110951385 A CN110951385 A CN 110951385A
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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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
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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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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
本发明属于涂料技术领域，具体涉及一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性聚醚多元醇30‑50份、多异氰酸酯单体10‑20份、增塑剂10‑20份、固体填料30‑50份、潜固化剂1‑5份、催化剂0.3‑3份、消泡剂0.1‑2份、抗流挂剂1‑5份。本发明的有益效果在于：（1）采用E‑51环氧树脂对聚醚多元醇混合物进行接枝改性，提高了涂料体系的黏度；（2）改性的固体填料与聚醚具有较强的键合作用，进一步提高了其抗沉降和抗流挂性能；（3）本发明制备的涂料体系通过对多种组分的改性使其工艺性能、力学性能均大大改善。
Description
技术领域
本发明属于涂料技术领域，具体涉及一种环氧改性的聚氨酯防水涂料及其制备方法。
背景技术
涂料是一种含颜料或不含颜料的，用树脂及油等制成的化工产品。将涂料涂覆在物体表面上能够干结成膜，使被涂物体的表面与环境介质相隔离，从而对被涂物体起到的保护和装饰的作用。
聚氨酯防水涂料属于化学反应型防水涂料，固化后是一种橡胶状的高弹性涂膜，该材料以其优良的综合性能，在世界范围内广泛应用。聚氨酯防水涂料根据其组成和固化机理，分为单组分和多组分两大类。多组分聚氨酯防水涂料现场施工时需按一定比例配料，机械搅拌，其搅拌过程中引入的起泡以及配料不准，搅拌不均匀等问题均会影响产品质量，因此而造成防水质量事故时有发生；而单组分涂料也存在一些难以避免的问题，尤其是由于液体聚氨酯流平性好，立面施工流淌特别严重，在立面施工无法上厚度等问题，已成为行业的难题。
针对以上问题，本领域多年来进行了深入探索，已有的解决方案致力于通过额外加入触变剂来改善产品的触变性能，使之粘而不稠，即可以好施工，又能在立面施工不流淌。但聚氨酯是极性材料，触变剂如气相白炭黑、氢化蓖麻油及其衍生物、有机膨润土等在聚氨酯体系中的触变效果不理想，存在粘度变大，不好施工等缺陷。
发明内容
为解决现有技术的不足，本发明提供一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性聚醚多元醇30-50份、多异氰酸酯单体10-20份、增塑剂10-20份、固体填料30-50份、潜固化剂1-5份、催化剂0.3-3份、消泡剂0.1-2份、抗流挂剂1-5份；
所述环氧改性的聚醚多元醇为E-51接枝改性的混合聚醚，所述混合聚醚为聚醚DL-2000D和聚醚EP-330N的混合物，混合比为1：0.5-1；所述E-51接枝混合聚醚的方法，包括如下步骤：(1)按质量比将聚醚DL-2000D和聚醚EP-330N称量后加入反应釜中进行充分混合；(2)向混合物中滴加混合聚醚质量3％的三氟化硼乙醚络合物，然后将一定量的E-51树脂加入反应釜中，升高温度到50-60℃，保温反应30-40min；(3)反应结束后加入氨气中和三氟化硼乙醚络合物，然后真空蒸馏除去体系中的水分，得改性聚醚多元醇；
所述多异氰酸酯单体包括异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯中的至少一种；
所述增塑剂包括三乙酸丙三醇酯，乙酰柠檬酸三丁酯，壬酯、氯化石蜡、中的至少一种；
所述固体填料包括滑石粉、纳米二氧化硅、纳米氧化铝、纳米碳化硅、红金石型钛白粉中的一种或多种；使用时需对填料进行表明改性，具体步骤如下：(1)将固体填料在2％的稀硝酸中浸泡24h，以除去表面的杂质并使表面形成足够多的空隙以便于承接改性剂；然后200℃下干燥2h，彻底除去表面水分；(2)将处理后的填料与硅烷偶联剂按质量比称量后加入捏合机中充分捏合1-2h，然后转入烘箱中，加热处理2-3h，使硅烷偶联剂处分浸渍到表面空隙中，获得改性填料；改性后的填料可以与改性聚醚较好的键合，提高了粘度和抗沉降性能；
所述潜固化剂包括2-异丙基恶唑烷、2,2-二氢恶唑烷、2-异丙基-N-羟乙基-恶唑烷或2,2-二氢-N-羟乙基恶唑烷中的至少一种。
所述催化剂为有机锡催化剂，包括二丁基锡二月桂酸酯、辛酸亚锡、二醋酸二丁基锡中的至少一种；
所述消泡剂为有机硅消泡剂，优先聚醚改性有机硅消泡剂；
所述抗流挂剂为改性气相二氧化硅，所述改性气相二氧化硅是利用二氧化硅易于形成氢键的特性，与二元醇反应使其表面形成二元醇接枝的结构，进而提高其与涂料体系的相互作用，起到抗流挂的目的。所述二元醇优选聚醚二元醇；具体改性方法是将气相二氧化硅加入二元醇中，70-80℃下反应2-3h，降温得到二元醇接枝的气相二氧化硅结构。
本发明还提供所述一种环氧树脂改性聚氨酯防水涂料的制备方法，具体包括如下步骤：
(1)在高速搅拌的密闭反应釜中，依次加入环氧改性聚醚多元醇、增塑剂、改性填料，快速搅拌并升高温度到100-105℃，开启真空泵在-0.08MPa以下抽2-3h，彻底脱除体系的水分，然后通氮气恢复至常压；
(2)将反应釜降温到60℃以下，搅拌情况下加入多异氰酸酯单体，控制温度在65-70℃进行聚合反应，反应30-40min后将温度降至45℃以下；
(3)向步骤(2)所得反应体系中依次加入消泡剂、潜固化剂、催化剂、抗流挂剂搅拌分散30-40min，然后抽真空除气泡制得抗流挂聚氨酯防水涂料。
本发明的有益效果在于：(1)采用E-51环氧树脂对聚醚多元醇混合物进行接枝改性，提高了涂料体系的黏度；(2)改性的固体填料与聚醚具有较强的键合作用，进一步提高了其抗沉降和抗流挂性能；(3)本发明制备的涂料体系通过对多种组分的改性使其工艺性能、力学性能均大大改善。
具体实施方式
以下对本发明的原理和特征进行描述，所举实施例只用于解释本发明，并非用于限定本发明的范围。
本发明实施例所用环氧改性的聚醚多元醇为E-51接枝改性的混合聚醚，所述混合聚醚为聚醚DL-2000D和聚醚EP-330N的混合物，混合比为1：0.8；所述E-51接枝混合聚醚的方法，包括如下步骤：(1)将聚醚DL-2000D 500g和聚醚EP-330N 400g加入反应釜中，40-50℃下充分搅拌混合；(2)向混合物中滴加30g的三氟化硼乙醚络合物，然后将混合聚醚质量E-51树脂加入反应釜中，升高温度到50-60℃，保温反应30-40min；(3)反应结束后加入氨气中和三氟化硼乙醚络合物，然后真空蒸馏除去体系中的水分，得改性聚醚多元醇。
本发明所用固体填料为改性滑石粉、纳米二氧化硅、纳米氧化铝、纳米碳化硅、红金石型钛白粉中的一种或多种；具体改性步骤如下：(1)将1000kg固体填料在2％的稀硝酸500mL中浸泡24h，以除去表面的杂质并使表面形成足够多的空隙以便与承接改性剂；然后200℃下干燥2h，彻底除去表面水分；(2)将处理后的填料与20g硅烷偶联剂加入捏合机中充分捏合1-2h，然后转入烘箱中，加热处理2-3h，使硅烷偶联剂充分浸渍到表面空隙中，获得改性填料。
本发明实施例所用抗流挂剂为改性气相二氧化硅，所述改性气相二氧化硅是利用二氧化硅易于形成氢键的特性，与二元醇反应使其表面形成二元醇接枝的结构，进而提高其与涂料体系的相互作用，起到抗流化的目的。所述二元醇优选聚醚二元醇；具体改性方法是将气相二氧化硅加入聚醚DL-2000D中，70-80℃下反应2-3h，降温得到二元醇接枝的气相二氧化硅结构。
实施例1：
本实施例提供一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性的聚醚多元醇40份、异佛尔酮二异氰酸酯10份、二环己基甲烷二异氰酸酯8份、三乙酸丙三醇酯13份、改性纳米二氧化硅40份、2-异丙基恶唑烷3份、二丁基锡二月桂酸酯1份、聚醚改性有机硅消泡剂0.3份、改性气相二氧化硅3份；
所述环氧改性的聚氨酯防水涂料的制备方法主要包括如下步骤：
(1)在高速搅拌的密闭反应釜中，依次加入环氧改性聚醚多元醇400g、、三乙酸丙三醇酯130g、、改性纳米二氧化硅400g，快速搅拌并升高温度到100-105℃，开启真空泵在-0.08MPa以下抽2-3h，彻底脱除体系的水分，然后通氮气恢复至常压；
(2)将反应釜降温到60℃以下，搅拌情况下加入异佛尔酮二异氰酸酯100g、二环己基甲烷二异氰酸酯80g，控制温度在65-70℃进行聚合反应，反应30-40min后将温度降至45℃以下；
(3)向步骤(2)所得反应体系中依次加入聚醚改性有机硅消泡剂3g、2-异丙基恶唑烷30g、催化剂二丁基锡二月桂酸酯10g、改性气相二氧化硅30g搅拌分散30-40min，然后抽真空除气泡后，补充氮气恢复常压，制得抗流挂聚氨酯防水涂料。
实施例2：
本实施例提供一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性的聚醚多元醇35份、异佛尔酮二异氰酸酯8份、六亚甲基二异氰酸酯10份、三乙酸丙三醇酯15份、改性纳米二氧化硅35份、2,2-二氢恶唑烷2份、醋酸二丁基锡1份、聚醚改性有机硅消泡剂0.3份、改性气相二氧化硅4份；
所述防水涂料的制备方法同实施例1。
实施例3：
本实施例提供一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性的聚醚多元醇45份、苯二亚甲基二异氰酸酯7份、六亚甲基二异氰酸酯8份、氯化石蜡15份、改性纳米氧化铝45份、2,2-二氢恶唑烷2份、二丁基锡二月桂酸酯1份、聚醚改性有机硅消泡剂0.3份、改性气相二氧化硅1份；
所述防水涂料的制备方法同实施例1。
实施例4：
本实施例提供一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性的聚醚多元醇40份、二环己基甲烷二异氰酸酯7份、异佛尔酮二异氰酸酯8份、氯化石蜡15份、改性滑石粉40份、2-异丙基恶唑烷2份、二丁基锡二月桂酸酯1份、聚醚改性有机硅消泡剂0.3份、改性气相二氧化硅1份；
所述防水涂料的制备方法同实施例1。
对比例
为展示本发明的技术效果，以现有专利技术(CN201510039842.2)的防水涂料进行比较，所述涂料的组成如下：聚醚二元醇2000D 50份，聚醚三元醇330N，氯化石蜡30份，苯甲酸0.2份，乙二醇胺0.4份，钛白粉10份，重钙60份，有机锡催化剂0.5份，消泡剂0.5份，溶剂15份；
为进一步验证本发明的技术效果，将合成的改性聚氨酯防水涂料进行涂膜，厚度约为1.5mm，按照GB/T19250-2013《聚氨酯防水涂料》进行性能测试，主要测试了拉伸强度和断裂伸长率；另外采用现场施工考察了涂料的抗流挂性能，具体方法是将涂料涂刷2次后测量涂层的厚度；具体测试结果如表1所示
表1.环氧改性聚氨酯涂料性能参数
从表1可见，本发明实施例所制备的涂料无论在力学性能还是抗流挂性能方面均优于现有专利技术。以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种环氧树脂改性的聚氨酯防水涂料，所述涂料包括如下重量份数的组成，环氧改性聚醚多元醇 30-50份、多异氰酸酯单体 10-20份、增塑剂 10-20份、固体填料 30-50份、潜固化剂 1-5份、催化剂 0.3-3份、消泡剂 0.1-2份、抗流挂剂 1-5份；
所述环氧改性的聚醚多元醇为E-51接枝改性的混合聚醚，所述混合聚醚为聚醚DL-2000D和聚醚EP-330N的混合物，混合比为1：0.5-1；
所述多异氰酸酯单体包括异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯中的至少一种；
所述增塑剂包括三乙酸丙三醇酯，乙酰柠檬酸三丁酯，壬酯、氯化石蜡、中的至少一种；
所述固体填料包括滑石粉、纳米二氧化硅、纳米氧化铝、纳米碳化硅、红金石型钛白粉中的一种或多种，使用时需对填料进行表面改性；
所述潜固化剂包括2-异丙基恶唑烷、2 ,2-二氢恶唑烷、2-异丙基-N-羟乙基-恶唑烷或2 ,2-二氢-N-羟乙基恶唑烷中的至少一种;
所述催化剂为有机锡催化剂，包括二丁基锡二月桂酸酯、辛酸亚锡、二醋酸二丁基锡中的至少一种；
所述消泡剂为聚醚改性有机硅消泡剂；
所述抗流挂剂为改性气相二氧化硅，所述改性气相二氧化硅是利用二氧化硅易于形成氢键的特性，与二元醇反应使其表面形成二元醇接枝的结构，进而提高其与涂料体系的相互作用，起到抗流挂的目的。
2.根据权利要求1所示的一种环氧树脂改性的聚氨酯防水涂料，其特征在于，所述E-51接枝改性混合聚醚的方法，其特征在于包括如下步骤：（1）按质量比将聚醚DL-2000D和聚醚EP-330N称量后加入反应釜中进行充分混合；（2）向混合物中滴加混合聚醚质量3%的三氟化硼乙醚络合物，然后将一定量的E-51树脂加入反应釜中，升高温度到50-60℃，保温反应30-40min；（3）反应结束后加入氨气中和三氟化硼乙醚络合物，然后真空蒸馏除去体系中的水分，得改性聚醚多元醇。
3.根据权利要求1所述的一种环氧树脂改性的聚氨酯防水涂料，其特征在于，所述固体填料的改性方法，具体步骤如下：（1）将固体填料在2%的稀硝酸中浸泡24h，以除去表面的杂质并使表面形成足够多的空隙以便于承接改性剂；然后200℃下干燥2h，彻底除去表面水分；（2）将处理后的填料与硅烷偶联剂按质量比称量后加入捏合机中充分捏合1-2h，然后转入烘箱中，加热处理2-3h，使硅烷偶联剂处分浸渍到表面空隙中，获得改性填料；改性后的填料可以与改性聚醚较好的键合，提高了粘度和抗沉降性能。
4.根据权利要求1所示的一种环氧树脂改性的聚氨酯防水涂料，其特征在于，所述改性气相二氧化硅的方法是将气相二氧化硅加入二元醇中，70-80℃下反应2-3h，降温得到二元醇接枝的气相二氧化硅结构。
5.权利要求1-4中任一项所述的环氧树脂改性的聚氨酯防水涂料的制备方法，具体包括如下步骤：
（1）在高速搅拌的密闭反应釜中，依次加入环氧改性聚醚多元醇、增塑剂、改性填料，快速搅拌并升高温度到100-105℃，开启真空泵在-0.08MPa以下抽2-3h，彻底脱除体系的水分，然后通氮气恢复至常压；
（2）将反应釜降温到60℃以下，搅拌情况下加入多异氰酸酯单体，控制温度在65-70℃进行聚合反应，反应30-40min后将温度降至45℃以下；
（3）向步骤（2）所得反应体系中依次加入消泡剂、潜固化剂、催化剂、抗流挂剂搅拌分散30-40min，然后抽真空除气泡制得抗流挂聚氨酯防水涂料。
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