CN116589808B - 鳞片石墨氟碳膜、自粘防水卷材及制备方法 - Google Patents
鳞片石墨氟碳膜、自粘防水卷材及制备方法 Download PDFInfo
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 15
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Abstract
本发明公开了一种鳞片石墨氟碳膜、自粘防水卷材及制备方法。所述鳞片石墨氟碳膜的制备方法,包括下述步骤:将氟碳树脂与有机溶剂混合,加入纳米氧化锌和纳米二氧化钛,球磨分散,得到氧化锌‑二氧化钛‑氟碳树脂溶液;将鳞片石墨加入甲基聚硅氧烷树脂中,超声分散,得到鳞片石墨‑甲基聚硅氧烷树脂;将氧化锌‑二氧化钛‑氟碳树脂溶液、鳞片石墨‑甲基聚硅氧烷树脂和二月桂酸二丁基锡搅拌混合均匀,得到鳞片石墨氟碳溶液;将鳞片石墨氟碳溶液流延,烘干,得到所述鳞片石墨氟碳膜。本发明制备的鳞片石墨氟碳膜及其自粘防水卷材具有良好的防水性能和抗老化性能。
Description
技术领域
本发明涉及一种鳞片石墨氟碳膜、自粘防水卷材及制备方法。
背景技术
自粘防水卷材通常采用聚合物材料为基材,通过特殊工艺制成的防水材料。其特点是具有自粘性,可以直接粘贴于基层上,从而形成一层坚固的防水层。自粘防水卷材常规主要分为SBS(聚苯乙烯-丁苯橡胶-聚苯乙烯)和APP(聚丙烯-聚丁二烯-聚丙烯)两种类型。
自粘防水卷材具有以下特点:(1)施工方便快捷,不需要使用火炬等高温设备,可以在常温下进行施工。(2)自粘性强,可以直接粘贴在基层上,形成一体化的防水层,避免了施工过程中的渗漏和漏贴现象。(3)具有良好的柔韧性和变形性能,可以适应基层的变形和变化,从而保证了防水层的密闭性和可靠性。
自粘防水卷材是一种广泛应用于建筑行业的建筑材料,其主要作用是在建筑物的屋顶、墙面、地下室等部位起到防水作用。由于其具有优良的性能和施工方便等优点,已经成为现代建筑中防水工程的首选材料之一。
发明内容
针对现有技术中存在的不足,本发明所要解决的技术问题是:一种鳞片石墨氟碳膜、自粘防水卷材及制备方法。
本发明提供了一种鳞片石墨氟碳膜的制备方法,包括下述步骤:
将氟碳树脂与有机溶剂混合,加入纳米氧化锌和纳米二氧化钛,球磨分散,得到氧化锌-二氧化钛-氟碳树脂溶液;
将鳞片石墨加入甲基聚硅氧烷树脂中,超声分散,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和二月桂酸二丁基锡搅拌混合均匀,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延,烘干,得到所述鳞片石墨氟碳膜。
优选地,一种鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
将80-100份氟碳树脂与180-220份有机溶剂混合,加入1-5份纳米氧化锌和1-5份纳米二氧化钛,球磨分散,得到氧化锌-二氧化钛-氟碳树脂溶液;
将0.1-0.5份鳞片石墨加入8-12份甲基聚硅氧烷树脂中,超声分散,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.1-0.3份二月桂酸二丁基锡搅拌,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,烘干,得到所述鳞片石墨氟碳膜。
优选地,一种鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
将80-100份氟碳树脂与180-220份有机溶剂混合,加入1-5份纳米氧化锌和1-5份纳米二氧化钛,球磨分散1-3小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
将0.1-0.5份鳞片石墨加入8-12份甲基聚硅氧烷树脂中,超声分散20-60分钟,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.1-0.3份二月桂酸二丁基锡搅拌40-80分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,烘干,得到所述厚度为0.01-0.05mm鳞片石墨氟碳膜。
针对本工艺中各原料的具体作用介绍如下:
氟碳树脂,是一类具有较好耐紫外老化及耐候性的高分子材料,被用于表面覆膜以提高防水卷材产品的耐候性。氟碳树脂具有良好的防水性能,能够形成紧密的防水膜,有效地防止水分渗透进入屋内,提高建筑物的防水性能。同时氟碳树脂具有较好的强度和刚度,能够提高改性氟碳膜的力学性能,如耐磨性、耐冲击性、抗老化性等,从而延长改性氟碳膜的使用寿命。本发明中氟碳树脂优选为PVDF树脂。
有机溶剂,可以起到溶解氟碳树脂和促进填料分散等作用。具体的,氟碳树脂是一种高分子化合物,需要通过有机溶剂来溶解。有机溶剂可以在分子水平上与氟碳树脂相互作用,使其变为均匀的液体溶液;并且可以帮助填料与氟碳树脂溶液更好地混合和分散,有助于提高材料的均匀性和稳定性。本发明中,有机溶剂为乙酸乙酯、乙酸丁酯、TEP、DMAc、DMF和环己酮中的至少一种。优选为乙酸丁酯。
纳米氧化锌,其在本发明中的作用:(1)增强氟碳树脂的力学性能:纳米氧化锌具有较高的比表面积和活性,加入到氟碳树脂中能够有效地增强其力学性能,如强度、硬度和耐磨性等。(2)提高改性氟碳树脂的耐候性和耐腐蚀性:氧化锌具有良好的抗氧化性和抗腐蚀性,能够有效地提高改性氟碳树脂的耐候性和耐腐蚀性,使其能够在恶劣的环境下长期使用。(3)促进纳米二氧化硅的分散:纳米氧化锌可能有助于提高纳米二氧化硅的分散性,因为纳米氧化锌具有较好的分散性和良好的分散效果。通过在氟碳树脂中添加纳米氧化锌,纳米氧化锌可以在溶液中均匀分散,从而增加了纳米二氧化硅的分散性。
纳米二氧化钛,其在本发明中的作用:(1)提高复合材料的强度和硬度:纳米二氧化硅具有高比表面积和强度,能够增加复合材料的强度和硬度,从而提高其力学性能。(2)提高复合材料的耐磨性和耐腐蚀性:纳米二氧化硅具有良好的耐磨性和耐腐蚀性,能够有效地提高复合材料的耐磨性和耐腐蚀性,延长使用寿命。(3)改善复合材料的耐热性和防水性:纳米二氧化硅能够吸收热量,从而改善复合材料的耐热性;同时,其还能够增加复合材料的密实性,提高防水性能。(4)促进氟碳树脂的分散:纳米二氧化硅能够促进氟碳树脂的分散,增强复合材料的稳定性和一致性。
鳞片石墨,具有良好的物理、化学性质和高比表面积,因此它可以在复合材料中发挥多种作用,例如增强力学性能、提高导电性、改善防水性能和抗老化性能等。在上述工艺中,添加鳞片石墨可以通过增加复合材料的屏障效应来提高防水性能,同时,鳞片石墨还具有良好的耐光、耐热、耐氧化等性能,可以提高复合材料的抗老化性能。因此,添加鳞片石墨可以在一定程度上提高改性氟碳膜防水卷材的防水性能和抗老化性能。
甲基聚硅氧烷树脂,是一种有机硅树脂,作为改性氟碳膜的重要成分之一,主要起到增强改性氟碳膜的力学性能和耐候性能的作用。有机硅树脂可以提高改性氟碳膜的硬度和耐磨性,同时还可以增强其抗氧化性、耐腐蚀性和耐化学性。此外,有机硅树脂还可以降低改性氟碳膜的表面张力和粘附力,从而提高其疏水性能和抗粘性能。特别的,甲基聚硅氧烷树脂具有极高的表面积和多孔结构,可以吸附和修饰石墨烯表面的化学官能团,对鳞片石墨进行有效改性。
在添加有机硅树脂甲基聚硅氧烷树脂时,还需要加入相应的有机硅树脂催化剂二月桂酸二丁基锡,以促进有机硅树脂的固化和交联反应,从而提高改性氟碳膜的力学性能。
本发明还提供了一种鳞片石墨氟碳膜,采用上述方法制备而成。
本发明还提供了一种鳞片石墨氟碳膜自粘防水卷材,包括表层、自粘层和背底层,所述表层为上述鳞片石墨氟碳膜。
在鳞片石墨氟碳膜自粘防水卷材中各层结构的基本介绍如下:
表层:鳞片石墨氟碳膜,具有防水、防紫外线、耐候性和化学稳定性的表面材料,常用于屋面、墙面等需要高性能防水保护的建筑部位。
自粘层:由自粘聚合物制成,能够粘结在建筑表面,具有很好的密封和防水效果。本发明对自粘层没有特殊限制,采用本领域技术人员熟知方法或采购市售商品即可。
背底层:这一层通常由塑料薄膜制成,既能够起到防水的作用,又能够保护自粘层,避免自粘层受到外界的损害。本发明对背底层没有特殊限制,采用本领域技术人员熟知方法或采购市售商品即可。
本发明还提供了一种鳞片石墨氟碳膜在制备自粘防水卷材中的应用。
本发明制备的鳞片石墨氟碳膜及其自粘防水卷材具有良好的防水性能和抗老化性能。
具体实施方式
一种鳞片石墨氟碳膜的制备方法,包括下述步骤:
将氟碳树脂与有机溶剂混合,加入纳米氧化锌和纳米二氧化钛,球磨分散,得到氧化锌-二氧化钛-氟碳树脂溶液;
将鳞片石墨加入甲基聚硅氧烷树脂中,超声分散,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和二月桂酸二丁基锡搅拌混合均匀,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延,烘干,得到所述鳞片石墨氟碳膜。
进一步的,鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
将80-100份氟碳树脂与180-220份有机溶剂混合,加入1-5份纳米氧化锌和1-5份纳米二氧化钛,球磨分散1-3小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
将0.1-0.5份鳞片石墨加入8-12份甲基聚硅氧烷树脂中,超声分散20-60分钟,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.1-0.3份二月桂酸二丁基锡搅拌40-80分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,烘干,得到所述厚度为0.01-0.05mm鳞片石墨氟碳膜。
具体在下述实施例和对比例中的具体原料:
实施例中采用的马来酸酐接枝聚偏氟乙烯的制备方法参照CN108863160B中实施例2记载的方法制备而成,具体为:将聚偏氟乙烯(PVDF树脂)和马来酸酐按照质量比1:0.8混合,油浴温度100℃左右依次加入二月桂二丁基锡和过氧化氢,搅拌反应5h得到马来酸酐接枝聚偏氟乙烯。
实施例1
鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
室温下,将90份PVDF树脂与200份乙酸丁酯混合,加入0.3份鳞片石墨、3份纳米氧化锌和3份纳米二氧化钛,球磨分散2小时40分钟;
室温下,再加入10份甲基聚硅氧烷树脂和0.15份二月桂酸二丁基锡搅拌500转/min搅拌60分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,240℃烘干,得到厚度为0.03mm鳞片石墨氟碳膜。
实施例2
鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
室温下,将90份PVDF树脂与200份乙酸丁酯混合,加入3份纳米氧化锌和3份纳米二氧化钛,球磨分散2小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
室温下,将氧化锌-二氧化钛-氟碳树脂溶液、0.3份鳞片石墨、10份甲基聚硅氧烷树脂和0.15份二月桂酸二丁基锡搅拌500转/min搅拌100分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,240℃烘干,得到厚度为0.03mm鳞片石墨氟碳膜。
实施例3
鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
室温下,将90份PVDF树脂与200份乙酸丁酯混合,加入3份纳米氧化锌和3份纳米二氧化钛,球磨分散2小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
室温下,将0.3份鳞片石墨加入10份甲基聚硅氧烷树脂中,1800W、26KHz超声分散40分钟,得到鳞片石墨-甲基聚硅氧烷树脂;
室温下,将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.15份二月桂酸二丁基锡搅拌500转/min搅拌60分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,240℃烘干,得到厚度为0.03mm鳞片石墨氟碳膜。
实施例4
鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
室温下,将3重量份马来酸酐接枝聚偏氟乙烯、90份PVDF树脂与200份乙酸丁酯混合,加入3份纳米氧化锌和3份纳米二氧化钛,球磨分散2小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
室温下,将0.3份鳞片石墨加入10份甲基聚硅氧烷树脂中,1800W-26KHz超声分散40分钟,得到鳞片石墨-甲基聚硅氧烷树脂;
室温下,将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.15份二月桂酸二丁基锡搅拌500转/min搅拌60分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,240℃烘干,得到厚度为0.03mm鳞片石墨氟碳膜。
应用例1-4
将实施例1-4所制备鳞片石墨氟碳膜表面涂覆0.001mm厚的聚氨酯胶黏剂,利用压延机与1.5mm厚的丁基橡胶层以及0.005mm厚的PET隔离膜加压热复合,收卷,得到本发明的鳞片石墨氟碳膜自粘防水卷材。
本发明的鳞片石墨氟碳膜自粘防水卷材为层状结构,具体依次为三层结构,表层:鳞片石墨氟碳膜;自粘层:丁基橡胶层;背底层:PET隔离膜。
测试例1
对实施例1-4制备的鳞片石墨氟碳膜进行防水性能、抗老化性测试。
抗老化测试:将各实施例制备得到的鳞片石墨氟碳膜置于85℃、85%RH静置3000h,观察鳞片石墨氟碳膜是否黄变。
防水性能测试:将各实施例制备得到的鳞片石墨氟碳膜测定水(5μL)在膜表面的平均接触角。
表1鳞片石墨氟碳膜性能的测试结果
接触角(°) | 抗老化性 | |
实施例1 | 132 | 无黄变 |
实施例2 | 128 | 轻微黄变 |
实施例3 | 141 | 无黄变 |
实施例4 | 145 | 无黄变 |
甲基聚硅氧烷树脂在本发明中的作用有两个方面:一方面是作为改性氟碳膜的重要成分之一,主要起到增强改性氟碳膜的力学性能和耐候性能的作用;另一方面是具有极高的表面积和多孔结构,可以吸附和修饰石墨烯表面的化学官能团,对鳞片石墨进行有效改性。
实施例1-3的不同之处在于分散鳞片石墨的步骤不同。在实施例1中,鳞片石墨与其他原料一起球磨分散;实施例2中,纳米氧化锌和纳米二氧化钛先与氟碳树脂混合分散,然后加入鳞片石墨和其他原料一起制备溶液;而在实施例3中,鳞片石墨与甲基聚硅氧烷树脂一起超声分散。实施例3中采用甲基聚硅氧烷树脂对鳞片石墨进行改性,提升其性能。从实验数据中可以看出,实施例3的效果明显优于实施例1和实施例2,这可能与采用甲基聚硅氧烷树脂对鳞片石墨进行改性有关。
测试例2
对应用例3的鳞片石墨氟碳膜自粘防水卷材,进行测试:
表2:检验结果
上述实施方式仅为本发明的优选实施方式,不能以此来限定本发明保护的范围,本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。
Claims (9)
1.一种鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
将80-100份氟碳树脂与180-220份有机溶剂混合,加入1-5份纳米氧化锌和1-5份纳米二氧化钛,球磨分散,得到氧化锌-二氧化钛-氟碳树脂溶液;
将0.1-0.5份鳞片石墨加入8-12份甲基聚硅氧烷树脂中,超声分散,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.1-0.3份二月桂酸二丁基锡搅拌,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,烘干,得到所述鳞片石墨氟碳膜;
所述甲基聚硅氧烷树脂为湖北新四海化工股份有限公司提供的牌号SH-9502甲基聚硅氧烷树脂。
2.如权利要求1所述的鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
将80-100份氟碳树脂与180-220份有机溶剂混合,加入1-5份纳米氧化锌和1-5份纳米二氧化钛,球磨分散1-3小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
将0.1-0.5份鳞片石墨加入8-12份甲基聚硅氧烷树脂中,超声分散20-60分钟,得到鳞片石墨-甲基聚硅氧烷树脂;
将氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.1-0.3份二月桂酸二丁基锡搅拌40-80分钟,得到鳞片石墨氟碳溶液;
将鳞片石墨氟碳溶液流延呈均匀液体膜,烘干,得到所述厚度为0.01-0.05mm鳞片石墨氟碳膜。
3.如权利要求1或2所述的鳞片石墨氟碳膜的制备方法,其特征在于:所述氟碳树脂为PVDF树脂。
4.如权利要求1或2所述的鳞片石墨氟碳膜的制备方法,其特征在于:有机溶剂为乙酸乙酯、乙酸丁酯、TEP、DMAc、DMF和环己酮中的至少一种。
5.如权利要求4所述的鳞片石墨氟碳膜的制备方法,其特征在于:所述有机溶剂为乙酸丁酯。
6.如权利要求1所述的鳞片石墨氟碳膜的制备方法,各原料重量份计,包括下述步骤:
室温下,将3重量份马来酸酐接枝聚偏氟乙烯、90份PVDF树脂与200份乙酸丁酯混合,加入3份纳米氧化锌和3份纳米二氧化钛,球磨分散2小时,得到氧化锌-二氧化钛-氟碳树脂溶液;
室温下,将0.3份鳞片石墨加入10份甲基聚硅氧烷树脂中,1800W-26KHz超声分散40分钟,得到鳞片石墨-甲基聚硅氧烷树脂;
室温下,将所述氧化锌-二氧化钛-氟碳树脂溶液、鳞片石墨-甲基聚硅氧烷树脂和0.15份二月桂酸二丁基锡搅拌500转/min搅拌60分钟,得到鳞片石墨氟碳溶液;
将所述鳞片石墨氟碳溶液流延呈均匀液体膜,240℃烘干,得到厚度为0.03mm所述鳞片石墨氟碳膜。
7.一种鳞片石墨氟碳膜,采用权利要求1-6任一项所述方法制备而成。
8.一种鳞片石墨氟碳膜自粘防水卷材,包括表层、自粘层和背底层,所述表层为权利要求7所述鳞片石墨氟碳膜。
9.如权利要求7所述鳞片石墨氟碳膜在制备自粘防水卷材中的应用。
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