CN113043706A - 一种抗菌强化地板及其制备方法 - Google Patents
一种抗菌强化地板及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗菌强化地板及其制备方法,涉及地板技术领域。抗菌强化地板的制备方法包括:将浸渍有无机抗菌剂和有机抗菌剂的浸渍纸与基板热压成型。发明人通过将有机抗菌剂和无机抗菌剂引入浸渍胶制备得到复合抗菌浸渍胶,将复合抗菌浸渍胶作为耐磨纸和平衡纸的浸胶过程,替代了传统的表面喷涂工艺,具有生产工序少且抗菌剂不容易破坏的优势,可以制备得到既能够抗细菌又能够抗真菌,且具有持久性、高效抗菌的效果。
Description
技术领域
本发明涉及地板技术领域,具体而言,涉及一种抗菌强化地板及其制备方法。
背景技术
目前,抗菌地板大多数使用的为无机抗菌剂,主要有银系列、铜系列、锌系列和钛系列,此类无机抗菌剂具有安全性、耐热性、耐久性良好的优点。但是,无机抗菌剂的抗菌效果并不理想且价格也较高,无机抗菌剂的抑菌效果具有迟效性,不能迅速地杀灭细菌,对真菌、霉菌却几乎没有抑制效果。
此外,目前抗菌地板多数使用的是表面喷涂工艺,此工艺不仅增加了生产工序,而且对生产环境有较大影响,在实际使用过程中,表面抗菌剂极易被破坏甚至失效。
鉴于此,特提出本发明。
发明内容
本发明的目的在于提供一种抗菌强化地板及其制备方法,旨在制备得到抗细菌和抗真菌性能优良,且耐热性和持久性好的抗菌地板。
本发明是这样实现的:
本发明提供一种抗菌强化地板的制备方法,包括:
将浸渍有无机抗菌剂和有机抗菌剂的浸渍纸与基板热压成型。
本发明还提供一种抗菌强化地板,其通过上述制备方法制备而得。
本发明具有以下有益效果:本发明实施例提供的抗菌强化地板的制备方法,发明人通过将有机抗菌剂和无机抗菌剂引入浸渍纸中,再与基板进行热压成型。采用本发明实施例中的抗菌强化地板的制备方法,替代了传统的表面喷涂工艺,具有生产工序少且抗菌剂不容易破坏的优势,可以制备得到既能够抗细菌又能够抗真菌,且具有持久性、高效抗菌的效果。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
本发明实施例提供了一种抗菌强化地板的制备方法,发明人创造性地将有机抗菌剂和无机抗菌剂加入浸渍胶中,通过优选加料的工艺,解决了有机抗菌剂相容性以及无机抗菌剂分散和沉降的难题,通过这一创造性的劳动,在不增加生产工序的前提下,制备得到既能够抗细菌又能够抗真菌,且能够持久性抗菌的地板。
具体包括如下步骤:
S1、复合抗菌浸渍胶的制备
将有机抗菌剂和无机抗菌剂引入浸渍胶中,以得到复合抗菌浸渍胶。具体地,可以采用将有机抗菌剂、无机抗菌剂和浸渍原胶混合的方式进行制备,浸渍原胶的种类不限,可以为用于地板各层粘接的常用胶粘剂。在一些实施例中,浸渍原胶可以是由甲醛和三聚氰胺反应制备得到的胶粘剂,由甲醛和三聚氰胺通过加成和缩聚反应制备得到。
发明人创造地在浸渍胶的制备过程中加入有机抗菌剂,在浸渍原胶制备过程中待反应完成之后加入有机抗菌剂,形成均匀且相容性好的混溶胶,解决了直接加入相容性不好的问题,氧化锌的加入提高了抗菌浸渍胶的耐高温性,保证了在高温热压过程中有机抗菌剂的稳定性。
在一些实施例中,浸渍原胶的制备过程包括:将甲醛水溶液调节pH值为8-9后与三聚氰胺混合反应20-30min,再调节pH值为8-8.5之后升温至95-100℃反应60-90min。在反应过程中需要精确地控制反应的pH,以使三聚氰胺保持较好的反应活性。
在本发明优选的实施例中,在甲醛水溶液与三聚氰胺混合反应时加入稳定剂,优选地,稳定剂为二乙二醇。通过引入稳定剂以使制备得到的胶粘剂的稳定性更好,有利于进一步延长地板的使用寿命。
在本发明优选的实施例中,在与三聚氰胺混合反应20-30min之后,先升温至70-80℃加入除醛剂再调节pH值为8-8.5。升温过程采用缓慢升温的方式,通过加入除醛剂减少了胶粘剂中的甲醛含量,以符合环保的要求,除醛剂的具体成分不限,可以为如:亚乙基脲、甲壳素、生物酶除醛剂、光触媒除醛剂等。
在本发明优选的实施例中,复合抗菌浸渍胶的制备过程包括:将浸渍原胶和有机抗菌剂混合得到有机抗菌浸渍胶,再将有机抗菌浸渍胶与无机抗菌剂混合;有机抗菌浸渍胶的制备是由浸渍原胶和有机抗菌剂在50-60℃的条件下混合20-30min;有机抗菌浸渍胶与无机抗菌剂混合是待有机抗菌浸渍胶冷却至室温后再进行混合。发明人通过优化浸渍原胶与有机抗菌剂和无机抗菌剂的混合步骤、混合温度,以使有机抗菌剂保持较好的活性,若温度过低则有机抗菌剂活性不够,制备得到的地板抗菌性能不理想;若温度过高则有机抗菌剂容易失效。
进一步地,有机抗菌剂与浸渍原胶的质量比为0.5-3.3:100;无机抗菌剂与浸渍原胶的质量比为0.5-5:100。通过进一步控制有机抗菌剂和无机抗菌剂的加入量以进一步保证地板的抗菌效果,若加入量过小抗菌效果不理想,若加入量过大则会不容易分散,使抗菌剂加入浸渍胶中的工艺无法实现。
一般而言,有机抗菌剂对细菌具有快速杀灭的能力,对于真菌和霉菌也能起到良好的抑制和杀灭作用,但因其耐热性不如无机抗菌剂好,且持久性比无机抗菌剂稍差,目前对于用作地板行业的研究较少。发明人创造性地将有机抗菌剂和无机抗菌剂均用于浸渍胶中,在各层浸胶时即可将两种抗菌剂引入而无需再进行喷涂,减少了生产工序。
进一步地,有机抗菌剂选自季铵盐类、苯酚类、双胍类、异噻唑类、吡咯类、有机金属类、咪唑类和吡啶类中的至少一种;优选为吡啶类;更优选为吡啶硫铜锌。一般类型的有机抗菌剂均在本申请的保护范围内,以上几种类型是发明人筛选出的性能较优的有机抗菌剂,采用吡啶硫铜锌能够更好地和无机抗菌剂配合,制备得到综合抗菌性能更为优良的地板。
进一步地,无机抗菌剂选自纳米银、纳米铜、纳米二氧化钛和纳米氧化锌中的至少一种;优选为纳米氧化锌;更优选为改性纳米氧化锌,改性纳米氧化锌的粒径为100-500nm。一般类型的无机抗菌剂均在本申请的保护范围内,以上几种类型是发明人筛选出的性能较优的无机抗菌剂,采用纳米氧化锌能够更好地和有机抗菌剂配合,制备得到综合抗菌性能更为优良的地板。此外,纳米氧化锌成本较低且能够符合环保要求,纳米氧化银已经被美国等地区限制,纳米铜和纳米二氧化钛成本较高。
具体地,改性纳米氧化锌为市购原料,改性的方法可以为多种,如离子掺杂、表面贵金属沉积、表面光敏化、半导体复合和离子注入等方法。比如可以为Ag、Al、Fe等金属离子与氧化锌掺杂得到的改性纳米氧化锌,可以为Ag离子沉积得到的改性纳米氧化锌。
需要说明的是,采用吡啶硫铜锌和改性纳米氧化锌的配合能够进一步提升抗菌性能,且持久性较好,符合欧盟及亚洲各国的标准。
具体地,吡啶硫铜锌是一种高效安全的抗菌化学品,被广泛应用于去屑洗发水中,对人体安全无毒;将吡啶硫铜锌用于地板表面和背面能有效抑制和杀灭地板表面以及背面潮湿环境下滋生的细菌和霉菌。吡啶硫铜锌对多种细菌和真菌霉菌有良好的抑制和杀灭效果,其通过将K+和Mg2+带出细菌细胞,将Na+带入细菌细胞,消除细菌获取营养的离子梯度,使细胞最终被“饿死”,所以吡啶硫铜锌的杀菌机理与许多抗菌剂并不相同,它在杀死细菌的同时本身并未被消耗。
具体地,纳米氧化锌具有较强的氧化还原性,其价带上的电子e—和H+会与吸附在材料表面的羟基和水等反应产生氢氧根、氧负离子和过氧化氢等物质,其中H+和氢氧根具有极强的氧化活性,可以使大部分有机物的化学键断裂,所以能够将组成微生物的化学成分分解,从而达到杀菌作用。此外,氧化锌中的锌离子能与细胞蛋白质上的基团反应,破坏细菌细胞和生理活性,进入微生物细胞后破坏电子传递系统的酶与-SH基反应,从而达到杀菌目的。
在具体实施例中可以采用如下的制备工艺:将30~55份的浓度为35%~45%的甲醛与10~20份的蒸馏水混合均匀,加入适量20~35%的氢氧化钠溶液,调节PH为8~9。然后加入92%~98%的二乙二醇3~5份、三聚氰胺30~45份,搅拌20~30分钟,然后缓慢升温至70~80℃,加入1~3份除醛剂,通过氢氧化钠调节PH至8~8.5,然后继续升温至95~100℃,保温60~90分钟,降温至50~60℃,加入0.5~2份吡啶硫铜锌,搅拌保温20~30分钟,冷却至室温,即得有机抗菌浸渍胶。将0.5~3份粒径100~500nm的经过改性的纳米氧化锌加入到有机抗菌浸渍胶中,混合均匀。
S2、浸胶
将耐磨纸、装饰纸和平衡纸进行浸胶得到浸渍耐磨纸、浸渍装饰纸和浸渍平衡纸,其中,耐磨纸和平衡纸均是采用复合抗菌浸渍胶进行浸胶,装饰纸的浸胶过程所用胶水不做限定,可以为一般市购的浸渍胶。将浸渍纸通过浸渍复合抗菌浸渍胶,再进行压贴,解决了表面喷涂工艺在地板使用过程中表面抗菌剂被磨损甚至失效的问题,提升了抗菌持久性。
在一些实施例中,浸渍耐磨纸、浸渍装饰纸和浸渍平衡纸的制备过程包括:将耐磨纸、装饰纸和平衡纸分别浸入胶水中,取出后进行预固化形成预固化度为40-60%的浸胶纸;预固化是向胶水中加入固化剂并在85-95℃下处理2-5min,固化剂的加入量与胶水质量的质量比为0.1-0.5:100。具体地,固化剂为MF固化剂-710、MF固化剂-740、MF固化剂-21133中的一种或多种,优选为MF固化剂-740,加入量为0.3%。预固化的过程可以采用常规的方式在烘道中进行处理即可。耐磨纸、装饰纸和平衡纸的浸胶量为100-240g/m3,耐磨纸和平衡纸是采用本发明实施例中的复合抗菌浸渍胶进行浸胶,装饰纸采用一般的市购胶水如聚氨酯胶进行浸胶。
进一步地,浸渍耐磨纸的重量为(含胶)100-160g/cm3,厚度为0.1-0.4mm;浸渍装饰纸的重量为(含胶)120-200g/cm3,厚度为0.1-0.4mm;基板的厚度为8-16mm,密度为0.5~1.0g/cm3;浸渍平衡纸的重量为(含胶)150-300g/cm3,厚度为0.2-0.5mm;各层的浸胶量会影响最终地板的抗菌性能,若浸胶量过少会由于有机抗菌剂的分解使地板的抗菌性能不能得到提升;若浸胶量过多会增加生产成本。
S3、热压成型
将依次设置的浸渍耐磨纸、浸渍装饰纸、基板和浸渍平衡纸热压成型,热压成型的具体工艺可以采用现有的工艺。
在优选的实施例中,热压成型的操作温度为190-220℃,操作压力为20-25MPa;热压成型的热压时间为15-40s。通过进一步优化热压的温度、压力和时间,有利于进一步提升抗菌效果,防止热压温度过高使有机抗菌剂分解,也防止热压温度过低影响成型效果。
本发明实施例还提供了一种抗菌强化地板,其通过上述制备方法制备而得,具有生产工序少且抗菌剂不容易破坏的优势,既能够抗细菌又能够抗真菌,且具有持久性、高效抗菌的效果。
需要补充的是,本发明实施例中提供的抗菌强化地板对金黄色葡萄球菌、大肠杆菌、白念球菌以及常见真菌能起到良好的抑制和杀灭作用,根据《ISO 22196-2016塑料制品表面抗菌性能评价方法》,对金黄色葡萄球菌和大肠杆菌有效杀灭率>99.9%。根据《ISO16869-2008塑料.塑料成份中抑制真菌化合物的效果评估》,对黑曲霉、球毛壳菌、宛氏拟青霉、蝇状青霉、长枝木霉达到1级抗菌性。
以下结合实施例对本发明的特征和性能作进一步的详细描述。
实施例1
本实施例提供一种抗菌强化地板的制备方法,包括如下步骤:
(1)复合抗菌浸渍胶的制备:以重量份数计,将35份浓度为40%的甲醛与16份蒸馏水混合均匀,加入适量25%的氢氧化钠溶液,调节PH为8~8.5。然后加入98%的二乙二醇3.6份、三聚氰胺36份,搅拌25分钟,然后缓慢升温至70℃,加入1.5份亚乙基脲,通过氢氧化钠调节PH至8~8.5,然后继续升温至95℃,保温80分钟,降温至55℃,加入1.2份吡啶硫铜锌,搅拌保温25分钟,冷却至室温,即得有机抗菌浸渍胶。将1.5份粒径约100nm的经过改性的纳米氧化锌加入到有机抗菌浸渍胶中,混合均匀。
(2)抗菌浸渍纸的制备:将耐磨纸和平衡纸浸入含有复合抗菌浸渍胶中,向浸渍胶中加入MF固化剂-740,固化剂加入量与胶水质量比为0.3:100,经过85℃烘道(3分钟),形成55%预固化度的浸胶纸,浸胶量为耐磨纸110g、平衡纸160g,经过裁切,密封保存,即得浸渍耐磨纸、浸渍平衡纸。将装饰纸浸入三聚氰胺甲醛胶水中(即不含有复合抗菌剂的胶水中),向浸渍胶中加入MF固化剂-710,固化剂加入量与胶水质量比为0.4:100,经过85℃烘道(3分钟),形成55%预固化度的浸渍装饰纸。
(3)抗菌强化地板的制备:按照从上至下:浸渍耐磨纸、浸渍装饰纸、基材、浸渍平衡纸依次组合后进行热压。其中,浸渍耐磨纸厚度0.15mm,重量130g/m3;浸渍装饰纸厚度0.25mm,重量150g/m3;基材厚度8mm,密度0.66g/cm3;浸渍平衡纸厚度0.3mm,重量240g/m3。热压温度205℃,压力21Mpa,时间20秒,热压完成后冷却即得抗菌强化地板。
实施例2
本实施例提供一种抗菌强化地板的制备方法,包括如下步骤:
(1)复合抗菌浸渍胶的制备:以重量份数计,将37份浓度为38%的甲醛与18份蒸馏水混合均匀,加入适量25%的氢氧化钠溶液,调节PH为8~8.5。然后加入96%的二乙二醇3.5份、三聚氰胺35份,搅拌20分钟,然后缓慢升温至80℃,加入1.3份亚乙基脲,通过氢氧化钠调节PH至8~8.5,然后继续升温至100℃,保温70分钟,降温至50℃,加入1.5份吡啶硫铜锌,搅拌保温25分钟,冷却至室温,即得有机抗菌浸渍胶。将1.2份粒径约500nm的经过改性的纳米氧化锌加入到有机抗菌浸渍胶中,混合均匀。
(2)抗菌浸渍纸的制备:将耐磨纸和平衡纸含有复合抗菌剂的浸渍胶中,向浸渍胶中加入MF固化剂-740,固化剂加入量与胶水质量比为0.5:100,经过90℃烘道(4分钟),形成一定55%预固化度的浸胶纸,浸胶量为耐磨纸100g、平衡纸150g经过裁切,密封保存,即得抗菌浸渍纸。将装饰纸浸入三聚氰胺甲醛胶水中(即不含有复合抗菌剂的胶水中),向浸渍胶中加入MF固化剂-740,固化剂加入量与胶水质量比为0.5:100,经过85℃烘道(3分钟),形成55%预固化度的浸渍装饰纸。
(3)抗菌强化地板的制备:按照从上至下:浸渍耐磨纸、浸渍装饰纸、基材、浸渍平衡纸依次组合后进行热压。其中,浸渍耐磨纸厚度0.15mm、重量120g/m3;浸渍装饰纸厚度0.25mm、重量160g/m3;基材厚度8mm,密度0.66g/cm3;浸渍平衡纸厚度0.3mm,重量250g/m3。热压温度200℃,压力21Mpa,时间25秒,热压完成后冷却即得抗菌强化地板。
实施例3
本实施例提供一种抗菌地板的制备方法,具体步骤与实施例1大致相同,不同之处仅在于:控制浸渍耐磨纸厚度0.1mm、重量100g/m3;浸渍装饰纸厚度0.1mm、重量120g/m3;基材厚度8mm,密度0.5g/cm3;浸渍平衡纸厚度0.2mm,重量150g/m3。
实施例4
本实施例提供一种抗菌地板的制备方法,具体步骤与实施例1大致相同,不同之处仅在于:控制浸渍耐磨纸厚度0.4mm、重量160g/m3;浸渍装饰纸厚度0.4mm、重量200g/m3;基材厚度16mm,密度1.0g/cm3;浸渍平衡纸厚度0.5mm,重量300g/m3。
实施例5
本实施例提供一种抗菌地板的制备方法,具体步骤与实施例1大致相同,不同之处仅在于:热压温度190℃,压力25Mpa,时间40秒。
实施例6
本实施例提供一种抗菌地板的制备方法,具体步骤与实施例1大致相同,不同之处仅在于:热压温度220℃,压力20Mpa,时间15秒。
试验例1
采用常规的方法测试实施例1-6制备得到的抗菌地板的抗菌性能,结果显示:对金黄色葡萄球菌和大肠杆菌有效杀灭率>99.9%;对于五种真菌:黑曲霉、球毛壳菌、宛氏拟青霉、蝇状青霉和长枝木霉达到1级抗菌性。
对比例1
本对比例提供一种抗菌地板的制备方法,具体步骤与实施例1大致相同,不同之处仅在于:在步骤(1)中不加入有机抗菌剂,待反应完成之后冷却至室温直接加入无机抗菌剂。
结果显示:抗菌效果无法达到要求,对金黄色葡萄球菌和大肠杆菌有效杀灭率>99%;对黑曲霉、球毛壳菌、宛氏拟青霉、蝇状青霉、长枝木霉仅为3级抗菌性。
对比例2
本对比例提供一种抗菌地板的制备方法,具体步骤与实施例1大致相同,不同之处仅在于:在步骤(1)中不加入无机抗菌剂。
结果显示:抗菌效果无法达到要求,对金黄色葡萄球菌和大肠杆菌有效杀灭率>98%;对黑曲霉、球毛壳菌、宛氏拟青霉、蝇状青霉、长枝木霉达到1级抗菌性。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。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 (10)
1.一种抗菌强化地板的制备方法,其特征在于,包括:
将浸渍有无机抗菌剂和有机抗菌剂的浸渍纸与基板热压成型。
2.根据权利要求1所述的制备方法,其特征在于,包括:将有机抗菌剂和无机抗菌剂引入浸渍胶中,以得到复合抗菌浸渍胶;采用所述复合抗菌浸渍胶进行浸胶得到所述浸渍纸,再将所述浸渍纸与所述基板热压成型;
优选地,将耐磨纸、装饰纸和平衡纸进行浸胶得到浸渍耐磨纸、浸渍装饰纸和浸渍平衡纸,再将依次设置的浸渍耐磨纸、浸渍装饰纸、基板和浸渍平衡纸热压成型;其中,所述耐磨纸和所述平衡纸均是采用所述复合抗菌浸渍胶进行浸胶。
3.根据权利要求2所述的制备方法,其特征在于,所述复合抗菌浸渍胶的制备过程包括:将浸渍原胶和有机抗菌剂混合得到有机抗菌浸渍胶,再将所述有机抗菌浸渍胶与所述无机抗菌剂混合;
优选地,所述有机抗菌浸渍胶的制备是由所述浸渍原胶和所述有机抗菌剂在50-60℃的条件下混合20-30min,且在所述浸渍原胶制备过程中待反应完成之后加入所述有机抗菌剂;
优选地,所述有机抗菌浸渍胶与所述无机抗菌剂混合是待所述有机抗菌浸渍胶冷却至室温后再进行混合。
4.根据权利要求3所述的制备方法,其特征在于,所述浸渍原胶是由甲醛和三聚氰胺反应而得;
优选地,所述浸渍原胶的制备过程包括:将甲醛水溶液调节pH值为8-9后与三聚氰胺混合反应20-30min,再调节pH值为8-8.5之后升温至95-100℃反应60-90min;
优选地,在甲醛水溶液与三聚氰胺混合反应时加入稳定剂,更优选地,所述稳定剂为二乙二醇;
优选地,在与三聚氰胺混合反应20-30min之后,先升温至70-80℃加入除醛剂再调节pH值为8-8.5。
5.根据权利要求4所述的制备方法,其特征在于,所述有机抗菌剂与所述浸渍原胶的质量比为0.5-3.3:100;
优选地,所述无机抗菌剂与所述浸渍原胶的质量比为0.5-5:100。
6.根据权利要求2所述的制备方法,其特征在于,所述有机抗菌剂选自季铵盐类、苯酚类、双胍类、异噻唑类、吡咯类、有机金属类、咪唑类和吡啶类中的至少一种;优选为吡啶类;更优选为吡啶硫铜锌;
优选地,所述无机抗菌剂选自纳米银、纳米铜、纳米二氧化钛和纳米氧化锌中的至少一种;优选为纳米氧化锌;更优选为改性纳米氧化锌;
进一步优选地,所述改性纳米氧化锌的粒径为100-500nm。
7.根据权利要求2-6中任一项所述的制备方法,其特征在于,所述浸渍耐磨纸、所述浸渍装饰纸和所述浸渍平衡纸的制备过程包括:将所述耐磨纸、所述装饰纸和所述平衡纸分别浸入胶水中,取出后进行预固化形成预固化度为40-60%的浸胶纸;
优选地,所述预固化是向胶水中加入固化剂,固化剂的加入量与胶水质量的质量比为0.1-0.5:100;
优选地,所述预固化是在85-95℃下处理2-5min;
优选地,所述耐磨纸、所述装饰纸和所述平衡纸的浸胶量为100-240g/m3。
8.根据权利要求7所述的制备方法,其特征在于,所述浸渍耐磨纸的重量为100-160g/cm3,所述浸渍装饰纸的重量为120-200g/cm3,所述浸渍平衡纸的重量为150-300g/cm3;
优选地,所述浸渍耐磨纸的厚度为0.1-0.4mm,所述浸渍装饰纸的厚度为0.1-0.4mm,所述基板的厚度为8-16mm,所述浸渍平衡纸的厚度为0.2-0.5mm。
9.根据权利要求1所述的制备方法,其特征在于,所述热压成型的操作温度为190-220℃,操作压力为20-25MPa;
优选地,所述热压成型的热压时间为15-40s。
10.一种抗菌强化地板,其特征在于,其通过权利要求1-9中任一项所述的制备方法制备而得。
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