CN114687248B - 一种环保装饰纸及其制备方法 - Google Patents
一种环保装饰纸及其制备方法 Download PDFInfo
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- CN114687248B CN114687248B CN202210358405.7A CN202210358405A CN114687248B CN 114687248 B CN114687248 B CN 114687248B CN 202210358405 A CN202210358405 A CN 202210358405A CN 114687248 B CN114687248 B CN 114687248B
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- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
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- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
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- 230000000052 comparative effect Effects 0.000 description 3
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
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- 125000003118 aryl group Chemical group 0.000 description 1
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Laminated Bodies (AREA)
Abstract
本发明涉及一种环保装饰纸及其制备方法，属于装饰材料技术领域，环保装饰纸从内到外依次包括装饰原纸、基材层、水性油墨装饰层和疏水保护层，基材层由聚氨酯胶液干燥后构成，疏水保护层由疏水保护剂干燥后构成，针对现有技术中对于装饰纸的要求，本发明提供了一种具有良好阻燃和耐污的环保装饰纸，不同于现有技术中利用三聚氰胺浸渍液对装饰原纸进行浸涂处理，本发明中利用制得的聚氨酯胶液和疏水保护层对其进行处理，提高其阻燃和耐污性能。选用聚氨酯树脂为原料，考虑到装饰纸的抗刮的保护作用；然后通过制备的阻燃组分和助剂作为反应的单体；引入具有阻燃和疏水耐污的结构，提高装饰纸的阻燃和耐污效果。
Description
技术领域
本发明属于装饰材料技术领域，具体地，涉及一种环保装饰纸及其制备方法。
背景技术
装饰纸是很多建材产品中必不可少的原料，如家具、橱柜用到的低压板、高压板，还有防火板、地板等。随着强化木地板、浸渍纸饰面人造板、家具和装修等产业的迅猛发展，装饰纸产业由此得到拉动进入蓬勃发展期，装饰纸用量不断增加，质量不断提高。
鉴于表面可塑性的要求以及环保，主要是无甲醛的要求，传统装饰纸利用三聚氰胺浸渍液浸涂处理，相比传统的方式在基材表面上完油墨之后，再在表面涂布水性聚氨酯树脂，水性聚氨酯树脂涂布后，可塑性好，更加环保；但聚氨酯材料是由碳-碳键为基本结构组成的有机高分子聚合物，属于可燃物质，引发火灾的几率较高。由各种引火源引发聚氨酯材料的燃烧以及伴随燃烧产生的烟雾毒性，已成为消防安全密切关注的重点之一，因此需要考虑产品的阻燃性能。
发明内容
为了解决背景技术中提到的技术问题，本发明提供一种环保装饰纸及其制备方法。
本发明的目的可以通过以下技术方案实现：
一种环保装饰纸，从内到外依次包括装饰原纸、基材层、水性油墨装饰层和疏水保护层；
所述基材层由聚氨酯胶液干燥后构成；
所述聚氨酯胶液通过如下步骤制备：
按照重量份计，将异氰酸酯、聚丙二醇、扩链剂和阻燃组分加入反应釜中，然后加入催化剂N,N-二甲基环己胺，在85℃条件下，继续搅拌2h；然后降温至50℃加入混合单体，然后加入中和剂反应15min，加入引发剂偶氮二异丁氰，保温反应2h，加入去离子水和无水乙醇，得到聚氨酯胶液。
进一步地，包括以下重量份数的制备原料：28-30份异氰酸酯、80-90份聚丙二醇、3-5份扩链剂、1-5份阻燃组分、0.2-0.6份催化剂、1-3份中和剂、10-20份混合单体、0.5-3份引发剂、75-85份去离子水和15-25份无水乙醇。
进一步地，所述阻燃组分通过如下步骤制备：
步骤S11、在氮气保护条件下，将甲代烯丙基醇和甲苯混合，升温至50℃，加入卡斯特催化剂，搅拌30-60min，然后加入四甲基二硅氧烷，加完后，升温至70℃，继续搅拌反应48h，反应结束后，减压浓缩除去溶剂，得到羟基单体；羟基单体的结构如下所示：
步骤S12、在氮气保护条件下，将羟基单体和苯膦酰二氯混合，然后加入N,N-二甲基苯胺，升温至130℃，反应10h，将得到的反应物用丙酮分散，然后加入碳酸氢钠溶液，调节pH值为7，加入冷水沉淀，经过过滤、干燥，得到阻燃组分。阻燃组分的结构如下所示：
进一步地，步骤S11中甲代烯丙基醇、四甲基二硅氧烷和卡斯特催化剂的用量比为0.018mol：0.009mol：0.2mL；步骤S12中羟基单体和苯膦酰二氯和N,N-二甲基苯胺的用量质量比为6g：2g：30mg。
含磷阻燃效率高，具有无毒、低烟等特点，阻燃组分属于含磷二元醇，在本发明中属于反应型阻燃剂，同时在聚氨酯中增加芳环的含量有助于阻燃性能的提高，以苯膦酰二氯为中心，两侧分别连接有含硅氧烷键的羟基单体，赋予聚氨酯胶液较高疏水性和耐高温性能。
进一步地，聚丙二醇的分子量约为2000；扩链剂为1,4-丁二醇；混合单体为甲基丙烯酸甲酯和丙烯酸丁酯按照重量比2：3混合而成；中和剂为三乙胺。
进一步地，疏水保护层由疏水保护剂干燥后构成，疏水保护剂通过如下步骤制备：
按照重量份计，将异氰酸酯、聚碳酸酯二醇、1,4-丁二醇和助剂加入反应釜中，然后加入N,N-二甲基环己胺，在85℃条件下，搅拌反应2h，然后降温至50℃加入三乙胺反应15min，加入体积分数90％的乙醇水溶液得到疏水保护剂。
进一步地，包括以下重量份数的制备原料：28-30份异氰酸酯、20-25份聚碳酸酯二醇、3-5份1,4-丁二醇、3-5份助剂、0.2-0.6份N,N-二甲基环己胺、1-3份三乙胺、80份体积分数90％的乙醇水溶液。
进一步地，所述助剂通过如下步骤制备：
步骤S21、在氮气保护条件下，将二乙醇胺和去离子水混合，在55℃条件下加入邻甲苯基缩水甘油醚，加完后，保持温度不变，搅拌反应3h，反应结束后，减压浓缩除去溶剂，得到中间产物a；中间产物a的结构如下所示：
步骤S22、全氟己基乙基碘和中间产物a加入正丁醇中，然后在80℃条件下，反应24h，反应结束后，减压浓缩除去溶剂，得到助剂。中间体a的结构上含有刚性链段，具有较好的耐热和防腐性能，且合成中间体a的原料邻甲苯基缩水甘油醚成本低，以中间产物a和全氟己基乙基碘为原料合成一种含氟助剂，全氟己基乙基碘中含6个碳的全氟链，具有很好的生物降解性，且在中间产物a的结构中引入全氟链，具有良好的憎水效果，制得的助剂保留的羟基，可以作为疏水保护剂原料中的反应单体，引入全氟链，提高疏水保护层的疏水性能，并赋予其一定的防霉抗菌作用。
进一步地，步骤S21中二乙醇胺、邻甲苯基缩水甘油醚和去离子水的用量质量比为5：3：2；
步骤S22中全氟己基乙基碘和中间产物a的用量质量比为9.4：2.5；正丁醇作为溶剂。
进一步地，所述装饰原纸为PVC涂层纸、纯纸、无纺纸、无纺布、纱布中的一种。
一种环保装饰纸的制备方法，包括如下步骤：
第一步、分别制备聚氨酯胶液、疏水保护剂；
第二步、将装饰原纸浸入聚氨酯胶液中2h，放入烘箱在100℃下干燥处理10min，得到基材层；用水性油墨进行装饰图案印刷，后在80-100℃条件下烘干，得到水性油墨装饰层；最后在水性油墨装饰层表面涂布疏水保护剂，后经130-150℃烘箱烘干，得疏水保护层，收卷，得一种环保装饰纸。
本发明的有益效果：
针对现有技术中对于装饰纸的要求，本发明提供了一种具有良好阻燃和耐污的环保装饰纸，不同于现有技术中利用三聚氰胺浸渍液对装饰原纸进行浸涂处理，本发明中利用制得的聚氨酯胶液和疏水保护层对其进行处理，提高其阻燃和耐污性能。
选用聚氨酯树脂为原料，考虑到装饰纸的抗刮的保护作用；然后通过制备的阻燃组分和助剂作为反应的单体；引入具有阻燃和疏水耐污的结构，提高装饰纸的阻燃和耐污效果。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
制备阻燃组分：
步骤S11、在氮气保护条件下，将甲代烯丙基醇和甲苯混合，升温至50℃，加入卡斯特催化剂，搅拌30-60min，然后加入四甲基二硅氧烷，加完后，升温至70℃，继续搅拌反应48h，反应结束后，减压浓缩除去溶剂，得到羟基单体；甲代烯丙基醇、四甲基二硅氧烷和卡斯特催化剂的用量比为0.018mol：0.009mol：0.2mL；
步骤S12、在氮气保护条件下，将羟基单体和苯膦酰二氯混合，然后加入N,N-二甲基苯胺，升温至130℃，反应10h，将得到的反应物用丙酮分散，然后加入碳酸氢钠溶液，调节pH值为7，加入冷水沉淀，经过过滤、干燥，得到阻燃组分。羟基单体和苯膦酰二氯和N,N-二甲基苯胺的用量质量比为6g：2g：30mg。
实施例2
制备聚氨酯胶液：
按照重量份计，将甲苯二异氰酸酯、聚丙二醇、扩链剂和实施例1制得的阻燃组分加入反应釜中，然后加入催化剂N,N-二甲基环己胺，在85℃条件下，继续搅拌2h；然后降温至50℃加入混合单体，然后加入中和剂反应15min，加入引发剂偶氮二异丁氰，保温反应2h，加入去离子水和无水乙醇，得到聚氨酯胶液。
原料：28份甲苯二异氰酸酯、80份聚丙二醇、3份扩链剂、1份阻燃组分、0.2份催化剂、1份中和剂、10份混合单体、0.5份引发剂、75份去离子水和15份无水乙醇。扩链剂为1,4-丁二醇；混合单体为甲基丙烯酸甲酯和丙烯酸丁酯按照重量比2：3混合而成；中和剂为三乙胺。
实施例3
制备聚氨酯胶液：
按照重量份计，将甲苯二异氰酸酯、聚丙二醇、扩链剂和实施例1制得的阻燃组分加入反应釜中，然后加入催化剂N,N-二甲基环己胺，在85℃条件下，继续搅拌2h；然后降温至50℃加入混合单体，然后加入中和剂反应15min，加入引发剂偶氮二异丁氰，保温反应2h，加入去离子水和无水乙醇，得到聚氨酯胶液。
原料：30份甲苯二异氰酸酯、90份聚丙二醇、5份扩链剂、5份阻燃组分、0.6份催化剂、3份中和剂、20份混合单体、3份引发剂、85份去离子水和25份无水乙醇。扩链剂为1,4-丁二醇；混合单体为甲基丙烯酸甲酯和丙烯酸丁酯按照重量比2：3混合而成；中和剂为三乙胺。
实施例4
制备助剂：
步骤S21、在氮气保护条件下，将二乙醇胺和去离子水混合，在55℃条件下加入邻甲苯基缩水甘油醚，加完后，保持温度不变，搅拌反应3h，反应结束后，减压浓缩除去溶剂，得到中间产物a；二乙醇胺、邻甲苯基缩水甘油醚和去离子水的用量质量比为5：3：2；
步骤S22、全氟己基乙基碘和中间产物a加入正丁醇中，然后在80℃条件下，反应24h，反应结束后，减压浓缩除去溶剂，得到助剂。全氟己基乙基碘和中间产物a的用量质量比为9.4：2.5；正丁醇作为溶剂。
实施例5
制备疏水保护剂：
按照重量份计，将甲苯二异氰酸酯、聚碳酸酯二醇、1,4-丁二醇和实施例4制得的助剂加入反应釜中，然后加入N,N-二甲基环己胺，在85℃条件下，搅拌反应2h，然后降温至50℃加入三乙胺反应15min，加入体积分数90％的乙醇水溶液得到疏水保护剂。
原料：28份甲苯二异氰酸酯、20份聚碳酸酯二醇、3份1,4-丁二醇、3份助剂、0.2份N,N-二甲基环己胺、1份三乙胺、80份体积分数90％的乙醇水溶液。
实施例6
制备疏水保护剂：
按照重量份计，将甲苯二异氰酸酯、聚碳酸酯二醇、1,4-丁二醇和实施例4制得的助剂加入反应釜中，然后加入N,N-二甲基环己胺，在85℃条件下，搅拌反应2h，然后降温至50℃加入三乙胺反应15min，加入体积分数90％的乙醇水溶液得到疏水保护剂。
原料：30份甲苯二异氰酸酯、25份聚碳酸酯二醇、5份1,4-丁二醇、5份助剂、0.6份N,N-二甲基环己胺、3份三乙胺、80份体积分数90％的乙醇水溶液。
实施例7
第一步、一种环保装饰纸，从内到外依次包括装饰原纸、基材层、水性油墨装饰层和疏水保护层；
第二步、将装饰原纸浸入实施例3制得的聚氨酯胶液中2h，放入烘箱在100℃下干燥处理10min，得到基材层；用水性油墨进行装饰图案印刷，后在80-100℃条件下烘干，得到水性油墨装饰层；最后在水性油墨装饰层表面涂布实施例5制得的疏水保护剂，后经130-150℃烘箱烘干，得疏水保护层，收卷，得一种环保装饰纸。其中，装饰原纸为PVC涂层纸。
实施例8
第一步、一种环保装饰纸，从内到外依次包括装饰原纸、基材层、水性油墨装饰层和疏水保护层；
第二步、将装饰原纸浸入实施例4制得的聚氨酯胶液中2h，放入烘箱在100℃下干燥处理10min，得到基材层；用水性油墨进行装饰图案印刷，后在80-100℃条件下烘干，得到水性油墨装饰层；最后在水性油墨装饰层表面涂布实施例6制得的疏水保护剂，后经130-150℃烘箱烘干，得疏水保护层，收卷，得一种环保装饰纸。其中，装饰原纸为PVC涂层纸。
实施例9
第一步、一种环保装饰纸，从内到外依次包括装饰原纸、基材层、水性油墨装饰层和疏水保护层；
第二步、将装饰原纸浸入实施例3制得的聚氨酯胶液中2h，放入烘箱在100℃下干燥处理10min，得到基材层；用水性油墨进行装饰图案印刷，后在80-100℃条件下烘干，得到水性油墨装饰层；最后在水性油墨装饰层表面涂布实施例6制得的疏水保护剂，后经130-150℃烘箱烘干，得疏水保护层，收卷，得一种环保装饰纸。其中，装饰原纸为PVC涂层纸。
对比例1
与实施例4相比，不添加阻燃组分制得聚氨酯胶液a，将实施例8中的聚氨酯胶液换成聚氨酯胶液a，其余原料及制备过程保持不变。
对比例2
与实施例6相比，不添加助剂制得疏水保护剂a，将实施例8中的疏水保护剂换成疏水保护剂a，其余原料及制备过程保持不变。
本实验例对实施例7-9和对比例1-2制得样品的阻燃性能进行检测，阻燃性能根据标准GB/T2406.2-2009，标准GB/T14656-2009测定；根据标准GB/T15102-2006《浸渍胶膜纸饰面人造板》测试耐污性；结果如表1所示；
表1
从上表1可知，本发明制得的环保装饰纸具有良好的阻燃性，耐污、耐腐蚀性好。
在说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。
Claims (5)
1.一种环保装饰纸，从内到外依次包括装饰原纸、基材层、水性油墨装饰层和疏水保护层；其特征在于，所述基材层由聚氨酯胶液干燥后构成；
所述聚氨酯胶液通过如下步骤制备：
将异氰酸酯、聚丙二醇、扩链剂和阻燃组分加入反应釜中，然后加入催化剂，在85℃条件下，继续搅拌2h；然后降温至50℃加入混合单体，然后加入中和剂反应15min，加入引发剂，保温反应2h，加入去离子水和无水乙醇，得到聚氨酯胶液；混合单体为甲基丙烯酸甲酯和丙烯酸丁酯按照重量比2：3混合而成；
所述阻燃组分通过如下步骤制备：
步骤S11、在氮气保护条件下，将甲代烯丙基醇和甲苯混合，升温至50℃，加入卡斯特催化剂，搅拌30-60min，然后加入四甲基二硅氧烷，加完后，升温至70℃，继续搅拌反应48h，得到羟基单体；甲代烯丙基醇、四甲基二硅氧烷和卡斯特催化剂的用量比为0.018mol：0.009mol：0.2mL；
步骤S12、在氮气保护条件下，将羟基单体和苯膦酰二氯混合，然后加入N,N-二甲基苯胺，升温至130℃，反应10h，得到阻燃组分；羟基单体和苯膦酰二氯和N,N-二甲基苯胺的用量质量比为6g：2g：30mg；
疏水保护层由疏水保护剂干燥后构成，疏水保护剂通过如下步骤制备：
步骤S21、在氮气保护条件下，将二乙醇胺和去离子水混合，在55℃条件下加入邻甲苯基缩水甘油醚，加完后，保持温度不变，搅拌反应3h，得到中间产物a；二乙醇胺、邻甲苯基缩水甘油醚和去离子水的用量质量比为5：3：2；
步骤S22、全氟己基乙基碘和中间产物a加入正丁醇中，然后在80℃条件下，反应24h，得到助剂；全氟己基乙基碘和中间产物a的用量质量比为9.4：2.5；
按照重量份计，将异氰酸酯、聚碳酸酯二醇、1,4-丁二醇和助剂加入反应釜中，然后加入N,N-二甲基环己胺，在85℃条件下，搅拌反应2h，然后降温至50℃加入三乙胺反应15min，加入体积分数90%的乙醇水溶液得到疏水保护剂。
2.根据权利要求1所述的一种环保装饰纸，其特征在于，所述聚氨酯胶液包括以下重量份数的制备原料：28-30份异氰酸酯、80-90份聚丙二醇、3-5份扩链剂、1-5份阻燃组分、0.2-0.6份催化剂、1-3份中和剂、10-20份混合单体、0.5-3份引发剂、75-85份去离子水和15-25份无水乙醇。
3.根据权利要求1所述的一种环保装饰纸，其特征在于，所述扩链剂为1,4-丁二醇；中和剂为三乙胺。
4.根据权利要求1所述的一种环保装饰纸，其特征在于，所述疏水保护剂包括以下重量份数的制备原料：28-30份异氰酸酯、20-25份聚碳酸酯二醇、3-5份1,4-丁二醇、3-5份助剂、0.2-0.6份N,N-二甲基环己胺、1-3份三乙胺、80份体积分数90%的乙醇水溶液。
5.根据权利要求1-4任意一项所述的一种环保装饰纸的制备方法，其特征在于，包括如下步骤：
第一步、分别制备聚氨酯胶液、疏水保护剂；
第二步、将装饰原纸浸入聚氨酯胶液中2h，放入烘箱在100℃下干燥处理10min，得到基材层；用水性油墨进行装饰图案印刷，后在80-100℃条件下烘干，得到水性油墨装饰层；最后在水性油墨装饰层表面涂布疏水保护剂，后经130-150℃烘箱烘干，得疏水保护层，收卷，得一种环保装饰纸。
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