CN106433096A - 一体化地暖软瓷及其制备方法 - Google Patents
一体化地暖软瓷及其制备方法 Download PDFInfo
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- CN106433096A CN106433096A CN201610848093.2A CN201610848093A CN106433096A CN 106433096 A CN106433096 A CN 106433096A CN 201610848093 A CN201610848093 A CN 201610848093A CN 106433096 A CN106433096 A CN 106433096A
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- porcelain tendre
- polyurethane resin
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Classifications
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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- C08K5/544—Silicon-containing compounds containing nitrogen
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Abstract
一体化地暖软瓷及其制备方法,采用软瓷层与高分子复合电热膜相结合,具有柔性好,抗撕裂性强及断裂伸长率高,且耐热性高、热效率高、升温快等优点。所述的软瓷层,它是由无机粉料和高分子材料制备而成,所述的高分子材料为水性环氧树脂乳液、水溶性环氧树脂固化剂、橡胶弹性体、含氟聚丙烯酸酯弹性乳液;所述的高分子复合电热膜,它包括聚氨酯树脂导热绝缘层、碳纳米管聚氨酯树脂发热层、聚氨酯树脂绝缘层和电极,高分子复合电热膜由聚氨酯树脂半固化导热绝缘层、碳纳米管聚氨酯树脂半固化发热层和聚氨酯树脂半固化绝缘层经热压而成,一体化地暖软瓷是通过聚氨酯树脂导热绝缘层将软瓷层与高分子复合电热膜连成一个整体。
Description
技术领域
本发明属建筑装饰材料领域,具体涉及一体化地暖软瓷及其制备方法。
技术背景
柔性饰面砖,也称软瓷,是以水性聚合物乳液与水泥作为粘合剂,以泥土、石英砂或矿粉为无机填充物,经加工成型而得到的一种面状材料。软瓷具有质轻体薄、柔软性好、外观造型丰富多彩、表现力极强等优点,且施工快捷、成本低、不易脱落,适合于建筑内、外墙及地板的装饰材料,是一种新型的节能环保生态装饰材料。
水性聚合物乳液配合水泥作为软瓷的粘合剂,赋予软瓷产品独特的防水性、柔软性、耐腐蚀性、抗开裂性,以及较好的拉伸强度和断裂伸长率。可用于软瓷的聚合物乳液主要有纯丙乳液、苯丙乳液、硅丙乳液等系列聚丙烯酸酯均聚物或共聚物乳液。如中国专利公告号CN 105731877A,公告日是2016年7月6日,名称为‘一种新型绿色环保柔性软瓷饰面砖配方及制备方法’中公开了利用丙烯酸乳液与抛光废渣及天然彩砂制备柔性软瓷饰面砖的配方及方法。如中国专利公告号CN 104453151A,公告日是2015年3月25日,名称为‘一种内外墙装饰用的彩色柔性饰面砖’中公开了利用纯丙或硅丙乳液及天然彩砂等制备的彩色柔性饰面砖。由于纯丙乳液的玻璃化转变温度较低,因而制备得到的软瓷饰面砖存在强度、耐划性等不足的缺点;尽管苯丙乳液或硅丙乳液的玻璃化转变温度稍高一些,柔性饰面砖能够满足一定温度下的强度要求,但也存在柔性不足,抗撕裂性差及断裂伸长率低等缺点。
电热膜供暖系统的供暖原理是将电能转化为热能,并以红外线形式向外辐射热量,使人体和物体均匀受热。与传统的空调、暖气等通过强制对流循环热风供暖相比,电热膜供暖系统具有舒适健康、节约空间、高效节能、热稳定性好、运行费用低、使用寿命长及安全性好等优点,电热膜供暖系统作为新型供暖技术符合未来节能环保的发展要求。
中国专利公告号CN104918341A,公告日是2015年9月16日,名称为“碳纳米管应用于地暖电热膜上的方法”中公开了以聚氨酯与碳纳米管组成的导电介质用于浸渍安装有镀锡铜箔丝的涤纶网格状基体而得到的发热材料,但存在一些不足:采用的热塑性聚氨酯树脂材料,耐热性不高,因而受热时易软化,强度低;导电介质中无有效的阻燃成分,使用安全性低;发热材料外使用的PE与PET层作为保护绝缘层,与发热体间无粘接作用,电热膜不能形成一体化,不便安装,且工作时安全性低;PE与PET层保护绝缘层为聚合物材料,不具有阻燃作用,且传热效率低。
发明内容
本发明的目的是为了克服现有技术的不足,提供了一种一体化地暖软瓷及其制备方法,采用软瓷层与高分子复合电热膜相结合,具有柔性好,抗撕裂性强及断裂伸长率高,且耐热性高、热效率高、升温快等优点。
本发明的技术方案是:一体化地暖软瓷,其特征在于:它包括软瓷层与高分子复合电热膜;
所述的软瓷层,它是由无机粉料和高分子材料制备而成,所述的高分子材料为水性环氧树脂乳液、水溶性环氧树脂固化剂、橡胶弹性体、含氟聚丙烯酸酯弹性乳液;各原料的重量组分为:无机粉料60~100份,水性环氧树脂乳液10~25份、水溶性环氧树脂固化剂3~10份、橡胶弹性体1~5份、含氟聚丙烯酸酯弹性乳液1~5份,水10~25份;
所述的高分子复合电热膜,它包括聚氨酯树脂导热绝缘层、碳纳米管聚氨酯树脂发热层、聚氨酯树脂绝缘层和电极,高分子复合电热膜由聚氨酯树脂半固化导热绝缘层、碳纳米管聚氨酯树脂半固化发热层和聚氨酯树脂半固化绝缘层经热压而成;
所述的聚氨酯树脂导热绝缘层的物质重量组分为:芳香族聚酯多元醇100份、超细导热绝缘粉20~50份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份、溶剂200~300份及二苯基甲基二异氰酸酯65~85份;
所述的聚氨酯树脂发热层的玻纤布基材中的物质重量组分为:芳香族聚酯多元醇100份、碳纳米管50~100份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份、溶剂200~300份及二苯基甲基二异氰酸酯65~85份;
所述的聚氨酯树脂绝缘层的玻纤布基材中的物质重量组分为:芳香族聚酯多元醇100份、超细导热绝缘粉20~50份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份、溶剂200~300份及二苯基甲基二异氰酸酯65~85份;
一体化地暖软瓷是通过聚氨酯树脂导热绝缘层将软瓷层与高分子复合电热膜连成一个整体。
如上所述的一体化地暖软瓷,其特征在于:软瓷层原料还包含阻燃剂5~15份、无机颜料1~3份。
如上所述的一体化地暖软瓷,其特征在于:所述的无机粉料为,水泥15~25份、石粉15~25份、石英砂30~50份。
如上所述的一体化地暖软瓷,其特征在于:所述的水性环氧树脂乳液,固含量为50%,25℃时的其粘度为500~8,000mPa.s,环氧当量为200~1,800 g/mol。
如上所述的一体化地暖软瓷,其特征在于:所述的水溶性环氧树脂固化剂为聚酰胺;25℃时的其粘度为500~12,000mPa.s,胺值为150~350 mgKOH/g。
水性环氧树脂乳液以水为介质,不含挥发性有机溶剂,符合环保要求,聚酰胺为脂肪族二元酸与二元胺形成的低分子量水溶性聚合物,具有良好的韧性,反应活性较高,环氧树脂与固化剂聚酰胺能在室温及潮湿条件下快速固化,形成聚合物交联网络结构,因而所形成的软瓷的硬度高,具有优异的耐磨性、耐热性、耐化学药品性、防霉性及抗渗漏性等优点,以聚酰胺为固化剂,还赋予软瓷较好的韧性。
上述的含氟聚丙烯酸酯弹性乳液为含氟丙烯酸酯单体或含氟甲基丙烯酸酯单体与丙烯酸酯或甲基丙烯酸酯等共聚形成的共聚物水性乳液。
含氟聚丙烯酸酯具有良好的拒水性与拒油性,且有良好的弹性,含氟聚丙烯酸酯线性链与环氧树脂固化物的交联网络结构形成半互穿网络聚合物,保留了环氧树脂固化物的优点,同时进一步改善了其柔软性,因而制备得到的软瓷具有良好的柔软性,同时也具有良好的拒水拒油性。
上述的水泥为标号为325、425、525及625的白色硅酸盐水泥。
选择不同标号的水泥配合乳液作为粘接剂,可满足软瓷不同的使用环境及机械性能的需求。
上述的石粉的粒径为80~300目。
上述的石英砂的粒径为50~300目。
上述的软瓷层原料中的阻燃剂为三聚氰胺、聚磷酸铵、三聚氰胺聚磷酸铵中的一种或两种。
选择含磷及含氮的阻燃剂,配合无机粉料,提高软瓷的阻燃等级,满足无卤阻燃的环保要求。
上述的无机颜料为炭黑、钛白、钛黄、氧化铁红、氧化铁黄、铁蓝、镉红、镉黄中的一种或两种。
上述的芳香族聚酯多元醇的羟值为200~450mgKOH/g,酸值≤2.0mgKOH/g,25℃时的粘度为200~4000mPas。
上述的超细导热绝缘粉为氮化铝、氮化硼、氧化铝中的一种,粒径小于1.5μm。
上述的碳纳米管为单壁碳纳米管或多壁碳纳米管,其中单壁碳纳米管的直径为0.6~2nm,多壁碳纳米管的直径为2~100nm。
上述的高分子复合电热膜中的阻燃剂为氢氧化镁、氢氧化铝、聚磷酸铵、三聚氰胺中的一种或两种。
上述的硅烷偶联剂为KH-550、KH-560、KH-570、A-151、A-171中的一种。
上述的增塑剂为二丙二醇二苯甲酸酯或己二酸二(丁氧基乙氧基乙)酯中的一种。
上述的催化剂为辛酸亚锡、二月桂酸二丁基锡、草酸亚锡、二醋酸二丁基锡中的一种。
上述的超细二氧化硅粉体的细度小于2µm
上述的溶剂为乙酸乙酯、丙酮、丁酮、甲苯、二甲苯中的一种。
一种一体化地暖软瓷的制备方法,包括以下步骤:
1)软瓷层的制备:首先按重量份称取水泥15~25份、石粉15~25份及石英砂30~50份,加到捏合机中,混合均匀,得到混合粉料;然后按重量份称取水性环氧树脂乳液10~25份、含氟聚丙烯酸酯弹性乳液1~5份、阻燃剂5~15份、无机颜料1~3份及水10~25份,加到搅拌釜中,搅拌均匀,得到混合乳液;其次,将混合粉料加入混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体1~5份、搅拌,反应0.5~2小时,再加入水溶性环氧树脂固化剂3~10份,搅拌均匀,得到聚合物砂浆;最后,将聚合物砂浆注入模具中,在室温下固化0.5~1h,然后在40~90℃下干燥2~4h,得到软瓷层。
2) 导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份、超细导热绝缘粉20~50份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份及溶剂200~300份,置于研磨分散机中分散研磨后,静置1小时,再按芳香族聚酯多元醇100份计,加入二苯基甲基二异氰酸酯65~85份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在25~100µm,置于50~60℃烘箱中,预固化0.5~1h,得到覆有半固化聚氨酯胶层的软瓷。
3) 半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份、碳纳米管50~100份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份及溶剂200~300份,置于研磨分散机中分散研磨后,静置1小时,再按芳香族聚酯多元醇100份计,加入二苯基甲基二异氰酸酯65~85份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于50~60℃的烘箱中,预固化0.5~1h,得到半固化发热层。
4) 半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份、超细二氧化硅20~50份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份及溶剂200~300份,置于研磨分散机中分散研磨后,静置1小时,再按芳香族聚酯多元醇100份计,加入二苯基甲基二异氰酸酯65~85份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于50~60℃的烘箱中,预固化0.5~1h,得到半固化绝缘层。
5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷胶层表面,在温度60~80℃、压力10~30kgf/cm2、固化时间1~3h条件下,经热压得到一体化地暖软瓷。
由于采用上述技术方案,制备得到的一体化地暖软瓷具有以下优点:
1)由于采用水性环氧树脂及聚酰胺固化剂能够固化形成交联网络聚合物,制备得到的软瓷硬度高,具有优异的耐热性、耐化学药品性、防霉性及抗渗漏性等优点,软瓷层的耐磨硬度满足地板耐磨性要求。
2)以高活性及柔韧性好的聚酰胺作为固化剂,软瓷层制备工艺简单,能在室温及潮湿条件下快速固化,固化时间为1h左右,且制备得到的软瓷具有一定的柔软性,较硬质地板更舒适。
3)采用含氟聚丙烯酸酯弹性乳液,与环氧树脂固化物形成半互穿网络聚合物,保留了环氧树脂交联固化物的优点,同时赋予软瓷层优异的柔软性及拒水拒油的特性。
4)软瓷层中含有大量无机粉料,结合含磷或含氮阻燃剂,满足无卤阻燃的环保要求;同时,在聚氨酯导电胶及绝缘胶中均添加了无卤阻燃剂,制备得到的高分子复合电热膜也满足无卤阻燃环保要求,所形成的一体化地暖软瓷达到难燃级,应用安全性能高。
5)采用芳香族聚酯多元醇与耐热性好的二苯基甲烷二异氰酸酯单体通过交联反应制备热固性聚氨酯,而且以耐热性及阻燃性玻纤布进一步增强,因而制备得到的高分子复合电热膜比现有的热塑性聚氨酯电热膜的耐热性及强度要高,在160度范围内都不会软化,强度不降低。
6)在电热材料中采用了偶联剂,提高了碳纳米管在聚氨酯中的分散性,并增强了碳纳米管与聚氨酯间的相互作用,因而发热膜发热较均匀。
7)在软瓷层与发热层之间的导热绝缘层中引入导热绝缘粉,提高电热膜向软瓷层热量的传导速率,同时软瓷层具有良好的透气性,有利于热量散发出来,因而一体化地暖软瓷升温迅速,热效率高。
8)在一体化地暖软瓷的制备过程中,先将聚氨酯树脂导热绝缘胶涂覆在软瓷层,提高了电热膜与软瓷层的粘结作用,预固化后,与半固化聚氨酯树脂发热层及半固化聚氨酯树脂绝缘层,经组合后热压、固化,使软瓷层与高分子复合电热膜的各层之间有较好的粘合作用,从而形成一体化地暖软瓷,方便安装。
具体实施方式
以下结合具体实施方式,对本发明的技术方案作进一步的描述。
实施例1
一种一体化地暖软瓷,其制备方法包括如下步骤:
(1)软瓷层的制备:
1) 按重量份称取标号为325的硅酸盐白水泥25份、80目的石粉15份及300目的石英砂50份,加到捏合机中,混合均匀,得到混合粉料;
2) 按重量份称取水性环氧树脂乳液10份(25℃时粘度为500mPa.s,环氧当量为200g/mol)、含氟聚丙烯酸酯弹性乳液2份、阻燃剂三聚磷酸10份、无机颜料钛白1份及水10份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体3份、搅拌,反应0.5小时,再加入固化剂聚酰胺10份(25℃时粘度为12,000mPa.s,胺值为350mgKOH/g),搅拌均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化0.5 h,然后在40℃下干燥4h,得到软瓷层。
(2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为200mgKOH/g,酸值为1.0mgKOH/g,粘度为4000mPas)、氮化铝50份、氢氧化镁40份、氢氧化铝40份、KH-560 5份、二丙二醇二苯甲酸酯20份、辛酸亚锡2份及乙酸乙酯300份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯65份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在25µm,置于50℃烘箱中,预固化1h,得到覆有半固化聚氨酯胶层的软瓷。
(3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为200mgKOH/g,酸值为1.0mgKOH/g,粘度为4000mPas)、2nm单壁碳纳米管100份、氢氧化镁40份、氢氧化铝40份、KH-550 5份、二丙二醇二苯甲酸酯20份、辛酸亚锡2份及乙酸乙酯300份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯65份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于50℃的烘箱中,预固化0.5h,得到半固化发热层。
(4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为200mgKOH/g,酸值为1.0mgKOH/g,粘度为4000mPas)、超细二氧化硅50份、氢氧化镁40份、氢氧化铝40份、KH-560 5份、二丙二醇二苯甲酸酯20份、辛酸亚锡2份及乙酸乙酯300份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯65份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于50℃的烘箱中,预固化1h,得到半固化绝缘层。
(5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷的胶层表面,在温度60℃、压力30kgf/cm2、固化时间3h条件下,经热压得到一体化地暖软瓷。
实施例2
一种一体化地暖软瓷,其制备方法包括如下步骤:
(1)软瓷层的制备:
1)称取标号为425的硅酸盐白水泥20份、100目的石粉20份及150目的石英砂40份,加到捏合机中,混合均匀,得到混合粉料;
2) 称取水性环氧树脂乳液15份(25℃时粘度为6,000mPa.s,环氧当量为1,400g/mol)、含氟聚丙烯酸酯弹性乳液5份、阻燃剂三聚氰胺3份、聚磷酸铵5份、无机颜料炭黑2份及水15份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体5份、搅拌,反应2小时,再加入固化剂聚酰胺3份(25℃时粘度为1,000mPa.s,胺值为180mgKOH/g),搅拌均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化0.5 h,然后在50℃下干燥4h,得到软瓷层。
(2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为300mgKOH/g,酸值为2.0mgKOH/g,粘度为2000mPas)、氮化硼40份、三聚氰胺60份、KH-550 3份、己二酸二(丁氧基乙氧基乙)酯10份、二月桂酸二丁基锡1份及丙酮250份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯72份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在50µm,置于55℃烘箱中,预固化1h,得到覆有半固化聚氨酯胶层的软瓷。
(3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为300mgKOH/g,酸值为2.0mgKOH/g,粘度为2000mPas)、直径为2nm的多壁碳纳米管80份、三聚氰胺60份、KH-560 3份、己二酸二(丁氧基乙氧基乙)酯10份、二月桂酸二丁基锡1份及丙酮250份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯72份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于55℃的烘箱中,预固化0.5h,得到半固化发热层。
(4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为300mgKOH/g,酸值为2.0mgKOH/g,粘度为2000mPas)、超细二氧化硅40份、三聚氰胺60份、KH-550 3份、己二酸二(丁氧基乙氧基乙)酯10份、二月桂酸二丁基锡1份及丙酮250份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯72份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于50℃的烘箱中,预固化1h,得到半固化绝缘层。
(5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷的胶层表面,在温度65℃、压力25kgf/cm2、固化时间2.5h条件下,经热压得到一体化地暖软瓷。
实施例3
一种一体化地暖软瓷,其制备方法包括如下步骤:
(1)软瓷层的制备:
1)称取标号为525的硅酸盐白水泥15份、300目的石粉25份及80目的石英砂30份,加到捏合机中,混合均匀,得到混合粉料;
2) 称取水性环氧树脂乳液20份(25℃时粘度为2,000mPa.s,环氧当量为800g/mol)、含氟聚丙烯酸酯弹性乳液2份、阻燃剂三聚氰胺聚磷酸铵5份、聚磷酸铵7份、无机颜料炭黑1份、镉红1份及水10份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体3份、搅拌,反应1小时,再加入固化剂聚酰胺6份(25℃时粘度为8,000mPa.s,胺值为300mgKOH/g),搅拌均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化1 h,然后在60℃下干燥3h,得到软瓷层。
(2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为450mgKOH/g,酸值为0.5mgKOH/g,粘度为200mPas)、氧化铝30份、聚磷酸铵50份、KH-570 1份、二丙二醇二苯甲酸酯5份、草酸亚锡0.5份及丁酮200份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯85份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在75µm,置于60℃烘箱中,预固化1h,得到覆有半固化聚氨酯胶层的软瓷。
(3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为450mgKOH/g,酸值为0.5mgKOH/g,粘度为200mPas)、直径为0.6nm的单壁碳纳米管70份、聚磷酸铵50份、KH-570 1份、二丙二醇二苯甲酸酯5份、草酸亚锡0.5份及丁酮200份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯85份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于55℃的烘箱中,预固化0.5h,得到半固化发热层。
(4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为450mgKOH/g,酸值为0.5mgKOH/g,粘度为200mPas)、超细二氧化硅30份、聚磷酸铵50份、KH-570 1份、二丙二醇二苯甲酸酯5份、草酸亚锡0.5份及丁酮200份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯85份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于55℃的烘箱中,预固化1h,得到半固化绝缘层。
(5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷的胶层表面,在温度70℃、压力25kgf/cm2、固化时间2h条件下,经热压得到一体化地暖软瓷。
实施例4
一种一体化地暖软瓷,其制备方法包括如下步骤:
(1)软瓷层的制备:
1)称取标号为325的硅酸盐白水泥22份、250目的石粉18份及120目的石英砂35份,加到捏合机中,混合均匀,得到混合粉料;
2) 称取水性环氧树脂乳液13份(25℃时粘度为1,000mPa.s,环氧当量为250g/mol)、含氟聚丙烯酸酯弹性乳液4份、阻燃剂三聚氰胺聚磷酸铵5份、无机颜料铁蓝1份及水20份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体2份、搅拌,反应1小时,再加入固化剂聚酰胺4份(25℃时粘度为5,000mPa.s,胺值为250mgKOH/g),搅拌均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化 40min,然后在40℃下干燥1h,60℃下干燥2h,得到软瓷层。
(2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为400mgKOH/g,酸值为0.8mgKOH/g,粘度为450mPas)、氮化硼45份、氢氧化铝35份、聚磷酸铵20份、A-151 4份、己二酸二(丁氧基乙氧基乙)酯15份、二醋酸二丁基锡1.5份及甲苯280份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯80份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在100µm,置于60℃烘箱中,预固化1h,得到覆有半固化聚氨酯胶层的软瓷。
(3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为400mgKOH/g,酸值为0.8mgKOH/g,粘度为450mPas)、直径为50nm的多壁碳纳米管60份、氢氧化铝35份、聚磷酸铵20份、A-151 4份、己二酸二(丁氧基乙氧基乙)酯15份、二醋酸二丁基锡1.5份及甲苯280份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯80份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于60℃的烘箱中,预固化0.5h,得到半固化发热层。
(4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为400mgKOH/g,酸值为0.8mgKOH/g,粘度为450mPas)、超细二氧化硅45份、氢氧化铝35份、聚磷酸铵20份、A-151 4份、己二酸二(丁氧基乙氧基乙)酯15份、二醋酸二丁基锡1.5份及甲苯280份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯80份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于55℃的烘箱中,预固化1h,得到半固化绝缘层。
(5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷的胶层表面,在温度75℃、压力20kgf/cm2、固化时间1.5h条件下,经热压得到一体化地暖软瓷。
实施例5
一种一体化地暖软瓷,其制备方法包括如下步骤:
(1)软瓷层的制备:
1)称取标号为625的硅酸盐白水泥17份、150目的石粉15份及100目的石英砂45份,加到捏合机中,混合均匀,得到混合粉料;
2) 称取水性环氧树脂乳液25份(25℃时粘度为8,000mPa.s,环氧当量为1,800g/mol)、含氟聚丙烯酸酯弹性乳液1份、阻燃剂三聚氰胺5份、聚磷酸铵10份、无机颜料炭黑1份、氧化铁红2份及水12份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体4份、搅拌,反应1小时,再加入固化剂聚酰胺5份(25℃时粘度为500mPa.s,胺值为150mgKOH/g),搅拌均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化50min,然后在70℃下干燥3h,得到暖软瓷层。
(2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为360mgKOH/g,酸值为1.5mgKOH/g,粘度为1200mPas)、氧化铝25份、氢氧化镁25份、三聚氰胺40份、A-171 2份、二丙二醇二苯甲酸酯12份、草酸亚锡0.8份及二甲苯260份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯75份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在75µm,置于60℃烘箱中,预固化0.5h,得到覆有半固化聚氨酯胶层的软瓷。
(3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为360mgKOH/g,酸值为1.5mgKOH/g,粘度为1200mPas)、直径为100nm的多壁碳纳米管90份、氢氧化镁25份、三聚氰胺40份、A-171 2份、二丙二醇二苯甲酸酯12份、草酸亚锡0.8份及二甲苯260份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯75份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于50℃的烘箱中,预固化1h,得到半固化发热层。
(4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为360mgKOH/g,酸值为1.5mgKOH/g,粘度为1200mPas)、超细二氧化硅25份、氢氧化镁25份、三聚氰胺40份、A-171 2份、二丙二醇二苯甲酸酯12份、草酸亚锡0.8份及二甲苯260份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯75份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于55℃的烘箱中,预固化1h,得到半固化绝缘层。
(5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷的胶层表面,在温度80℃、压力10kgf/cm2、固化时间1h条件下,经热压得到一体化地暖软瓷。
实施例6
一种一体化地暖软瓷,其制备方法包括如下步骤:
(1)软瓷层的制备:
1)称取标号为425的硅酸盐白水泥16份、80目的石粉20份及250目的石英砂40份,加到捏合机中,混合均匀,得到混合粉料;
2) 称取水性环氧树脂乳液22份(25℃时粘度为5,000mPa.s,环氧当量为1,250g/mol)、含氟聚丙烯酸酯弹性乳液3份、阻燃剂聚磷酸铵14份、无机颜料钛黄1份及水13份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体3份、搅拌,反应2小时,再加入固化剂聚酰胺8份(25℃时粘度为3,000mPa.s,胺值为210mgKOH/g),搅拌均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化 1h,然后在50℃下干燥1h,90℃下干燥1h,得到软瓷层。
(2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为250mgKOH/g,酸值为1.5mgKOH/g,粘度为3000mPas)、氮化铝20份、氢氧化铝70份、KH-5704.5份、己二酸二(丁氧基乙氧基乙)酯18份、辛酸亚锡1.6份及乙酸乙酯220份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯69份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在50µm,置于60℃烘箱中,预固化1h,得到覆有半固化聚氨酯胶层的软瓷。
(3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为250mgKOH/g,酸值为1.5mgKOH/g,粘度为3000mPas)、直径为1nm的单壁碳纳米管85份、氢氧化铝70份、KH-570 4.5份、己二酸二(丁氧基乙氧基乙)酯18份、辛酸亚锡1.6份及乙酸乙酯220份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯69份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于55℃的烘箱中,预固化1h,得到半固化发热层。
(4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份(羟值为250mgKOH/g,酸值为1.5mgKOH/g,粘度为3000mPas)、超细二氧化硅20份、氢氧化铝70份、KH-570 4.5份、己二酸二(丁氧基乙氧基乙)酯18份、辛酸亚锡1.6份及乙酸乙酯220份,置于研磨分散机中分散研磨后,静置1小时,加入二苯基甲基二异氰酸酯69份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于55℃的烘箱中,预固化1h,得到半固化绝缘层。
(5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷的胶层表面,在温度75℃、压力15kgf/cm2、固化时间1.5h条件下,经热压得到一体化地暖软瓷。
对比例1
一种聚合物水泥基软瓷层,其制备方法包括如下步骤:
1) 按重量份称取标号为325的硅酸盐白水泥25份、80目的石粉15份及300目的石英砂50份,加到捏合机中,混合均匀,得到混合粉料;
2) 按重量份称取纯丙乳液20份、含氟聚丙烯酸酯弹性乳液2份、阻燃剂三聚磷酸10份、无机颜料钛白1份及水10份,加到搅拌釜中,搅拌均匀,得到混合乳液;
3) 将步骤2)中得到的混合粉料加入到步骤1)中得到的混合乳液中,充分搅拌,混合均匀,得到聚合物砂浆;
4) 将聚合物砂浆注入模具中,在室温下固化0.5 h,然后在40℃下干燥4h,得到聚合物水泥基柔性饰面砖。
对实施例1-6和对比例1得到的软瓷样品进行测试,测试结果见表1,其中, GB/T8624-2006测试阻燃性,采用拉伸强度测试仪测试拉伸强度,利用欧盟PrEn660-1:1995测定磨耗硬度。
由表1可知,以弹性含氟聚丙烯酸酯线性链、水性环氧树脂固化物作为交联网络形成的软瓷层的拉伸强度远高于纯丙形成的软瓷层的拉伸强度;同时,由表1可以看出,对比例1中以纯丙乳液取代实施例1中水性环氧树脂及其固化剂组分时,当环境温度由25℃升至40℃时,对比例1中所制备的软瓷层的强度急剧下降,由1.54MPa降至0.62MPa,而实施例1所得到的软瓷层样品则由7.74MPa降至5.92MPa,仍保持较高的强度。从表1可以看出,水性环氧树脂固化物形成的软瓷层作为地板的耐磨等级明显高于纯丙形成的软瓷层的耐磨等级,后者仅为T级。由于采用大量无机粉料,配合阻燃剂,制备得到的一体化地暖软瓷的阻燃性均较好。
表1
Claims (6)
1.一体化地暖软瓷,其特征在于:它包括软瓷层与高分子复合电热膜;
所述的软瓷层,它是由无机粉料和高分子材料制备而成,所述的高分子材料为水性环氧树脂乳液、水溶性环氧树脂固化剂、橡胶弹性体、含氟聚丙烯酸酯弹性乳液;各原料的重量组分为:无机粉料60~100份,水性环氧树脂乳液10~25份、水溶性环氧树脂固化剂3~10份、橡胶弹性体1~5份、含氟聚丙烯酸酯弹性乳液1~5份,水10~25份;
所述的高分子复合电热膜,它包括聚氨酯树脂导热绝缘层、碳纳米管聚氨酯树脂发热层、聚氨酯树脂绝缘层和电极,高分子复合电热膜由聚氨酯树脂半固化导热绝缘层、碳纳米管聚氨酯树脂半固化发热层和聚氨酯树脂半固化绝缘层经热压而成;
所述的聚氨酯树脂导热绝缘层的物质重量组分为:芳香族聚酯多元醇100份、超细导热绝缘粉20~50份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份、溶剂200~300份及二苯基甲基二异氰酸酯65~85份;
所述的聚氨酯树脂发热层的玻纤布基材中的物质重量组分为:芳香族聚酯多元醇100份、碳纳米管50~100份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份、溶剂200~300份及二苯基甲基二异氰酸酯65~85份;
所述的聚氨酯树脂绝缘层的玻纤布基材中的物质重量组分为:芳香族聚酯多元醇100份、超细导热绝缘粉20~50份、阻燃剂40~80份、硅烷偶联剂1~5份、增塑剂5~20份、催化剂0.5~2份、溶剂200~300份及二苯基甲基二异氰酸酯65~85份;
一体化地暖软瓷是通过聚氨酯树脂导热绝缘层将软瓷层与高分子复合电热膜连成一个整体。
2.如权利要求1的一体化地暖软瓷,其特征在于:软瓷层原料还包含阻燃剂5 ~ 15份、无机颜料1 ~ 3份。
3.如权利要求1所述的一体化地暖软瓷,其特征在于:所述的无机粉料为,水泥15 ~ 25份、石粉15 ~ 25份、石英砂30 ~ 50份。
4.如权利要求1所述的一体化地暖软瓷,其特征在于:所述的水性环氧树脂乳液,固含量为50%,25℃时的其粘度为500 ~ 8,000mPa.s,环氧当量为200 ~ 1,800 g/mol。
5.如权利要求1所述的一体化地暖软瓷,其特征在于:所述的水溶性环氧树脂固化剂为聚酰胺,25℃时的其粘度为500 ~ 12,000mPa.s,胺值为150 ~ 350 mgKOH/g。
6.一种一体化地暖软瓷的制备方法,包括以下步骤:
1) 软瓷层的制备:首先按重量份称取水泥15~25份、石粉15~25份及石英砂30~50份,加到捏合机中,混合均匀,得到混合粉料;然后按重量份称取水性环氧树脂乳液10~25份、含氟聚丙烯酸酯弹性乳液1~5份、阻燃剂5~15份、无机颜料1~3份及水10~25份,加到搅拌釜中,搅拌均匀,得到混合乳液;其次,将混合粉料加入混合乳液中,充分搅拌,混合均匀后,加入橡胶弹性体1-5份、搅拌,反应0.5-2小时,再加入水溶性环氧树脂固化剂3~10份,搅拌均匀,得到聚合物砂浆;最后,将聚合物砂浆注入模具中,在室温下固化0.5~1h,然后在40~90℃下干燥2~4h,得到软瓷层;
2)导热绝缘半固化胶层的制备:按重量份称取芳香族聚酯多元醇100份、超细导热绝缘粉20 ~ 50份、阻燃剂40 ~ 80份、硅烷偶联剂1 ~ 5份、增塑剂5 ~ 20份、催化剂0.5 ~ 2份及溶剂200 ~ 300份,置于研磨分散机中分散研磨后,静置1小时,再按芳香族聚酯多元醇100份计,加入二苯基甲基二异氰酸酯65 ~ 85份,搅拌均匀,得到聚氨酯树脂导热绝缘胶,将导热绝缘胶涂覆在步骤1)制备得到的软瓷层,通过刮刀控制胶层的厚度在25 ~ 100µm,置于50 ~ 60℃烘箱中,预固化0.5 ~ 1h,得到覆有半固化聚氨酯胶层的软瓷;
3)半固化发热层的制备:按重量份称取芳香族聚酯多元醇100份、碳纳米管50 ~ 100份、阻燃剂40 ~ 80份、硅烷偶联剂1 ~ 5份、增塑剂5 ~ 20份、催化剂0.5 ~ 2份及溶剂200~ 300份,置于研磨分散机中分散研磨后,静置1小时,再按芳香族聚酯多元醇100份计,加入二苯基甲基二异氰酸酯65 ~ 85份,搅拌均匀,得到聚氨酯树脂导电胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍两侧分别织入了铜箔丝的玻纤布基材,并置于50 ~ 60℃的烘箱中,预固化0.5 ~ 1h,得到半固化发热层;
4)半固化绝缘层的制备:按重量份称取芳香族聚酯多元醇100份、超细二氧化硅20 ~50份、阻燃剂40 ~ 80份、硅烷偶联剂1 ~ 5份、增塑剂5 ~ 20份、催化剂0.5 ~ 2份及溶剂200 ~ 300份,置于研磨分散机中分散研磨后,静置1小时,再按芳香族聚酯多元醇100份计,加入二苯基甲基二异氰酸酯65 ~ 85份,搅拌均匀,得到聚氨酯树脂导热绝缘胶;然后用上述得到的聚氨酯树脂导电胶充分浸渍玻纤布基材,并置于50 ~ 60℃的烘箱中,预固化0.5~ 1h,得到半固化绝缘层;
5)一体系化地暖软瓷的制备:将步骤3)制备得到的半固化发热层及步骤4)制备得到的半固化绝缘层依次组合到步骤2)制备得到的覆有半固化聚氨酯胶层的软瓷胶层表面,在温度60 ~ 80℃、压力10 ~ 30kgf/cm2、固化时间1 ~ 3h条件下,经热压得到一体化地暖软瓷。
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