CN113860823A - 一种无机气凝胶土的制备工艺 - Google Patents
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Abstract
本发明涉及一种无机气凝胶土的制备工艺,属于无机气凝胶土制备工艺技术领域。包括以下步骤:1)将水、改性剂、稳定剂、气凝胶粉体,加入到高速搅拌分散机中,然后在常温常压下以500‑5000r/min搅拌3‑20分钟,混合均匀获得了气凝胶浆料;2)将无机胶凝材料、无机晶须、聚丙烯纤维依次加入到步骤1获得的气凝胶浆料中,然后在常温常压下以500‑5000r/min的速度搅拌3‑20分钟,混合均匀获得无机气凝胶土膏状材料;3)将步骤2)获得的无机气凝胶土膏状材料在常温下静置、凝固、干燥,获得了无机气凝胶土材料。通过本发明制备工艺制得的无机气凝胶土,具有低导热、高疏水、吸音降噪的效果。
Description
技术领域
本发明涉及一种无机气凝胶土的制备工艺,属于无机气凝胶土制备工艺技术领域。
背景技术
二氧化硅气凝胶是一种纳米多孔性材料,具有导热系数低、疏水能力强、密度小、孔隙率高、比表面积大等多项优点。但气凝胶突出的强度低、韧性差的缺点,使得目前关于气凝胶的应用多以气凝胶毡和气凝胶涂料为主,而气凝胶与传统的无机材料结合制备的产品市场上则少见相关报道。这是因为气凝胶比表面积大、密度低、疏水性强,与无机胶凝材料结合时难以相容,会产生分层漂浮现象,而如果解决这些问题,利用气凝胶低导热、高疏水、密度的优点与无机胶凝材料结合,就可以制备出一种保温、隔音、疏水并具有一定强度无机复合保温材料。
发明内容
本发明的目的在于探索出一种新的气凝胶产品应用形式,提供一种低导热、高疏水、吸音降噪的无机气凝胶土的制备工艺。
为实现上述目的,本发明提供如下技术方案:
一种无机气凝胶土的制备工艺,其特殊之处在于包括以下制备工艺:
1、将水10-100份,改性剂0.1-5份,稳定剂0.1-5份,气凝胶粉体1-20份,加入到高速搅拌分散机中,然后在常温常压下以500-5000r/min搅拌3-20分钟,混合均匀获得了气凝胶浆料;
气凝胶表面充满了疏水基团甲基,因此其很难与水相互相容,分散剂和稳定剂的作用就是改变水的特性,增加水溶液的粘度,在快速搅拌的过程中改性后的水溶液包裹住气凝胶微粒,实现气凝胶和水的相互容和,形成不沉降、不分层的混合均匀的气凝胶浆料,此过程不破坏气凝胶的结构、特性,也就是不影响气凝胶超疏水、低导热的优点;
2、将无机胶凝材料10-100份、无机晶须1-10份、聚丙烯纤维1-5份依次加入到步骤1获得的气凝胶浆料中,然后在常温常压下以500-5000r/min的速度搅拌3-20分钟,混合均匀获得无机气凝胶土膏状材料;
气凝胶浆料是不具有强度的,因此需要引入无机胶凝材料以提供强度。单纯的无机胶凝材料加入气凝胶浆料后,固化干燥后可能会存在强度低、开裂、微裂纹等现象,因此需要无机晶须、聚丙烯纤维等不同尺度的材料来进行复合增强:无机晶须是在微米尺度上与无机胶凝材料进行复合增强;聚丙烯纤维是在毫米尺度上与无机胶凝材料进行复合增强。气凝胶浆料加入无机胶凝材料、无机晶须、聚丙烯纤维后,三者相互协同配合共同增强整体体系的强度,也就初步获得了无机气凝胶土材料;
3、将步骤2获得的无机气凝胶土膏状材料在常温下静置、凝固、干燥,获得了无机气凝胶土材料。
气凝胶具有密度小、比表面大、单位质量体积大等特点,步骤1形成的气凝胶浆料是水溶液包裹住气凝胶微粒制备而成的,也因此气凝胶浆料的体积是水溶液的体积和气凝胶体积的总和,是相对较大的,这确保步骤2引入无机胶凝材料和增强材料后形成的无机气凝胶土的密度是相对较小;
优选的,步骤1中所述气凝胶粉体是二氧化硅气凝胶粉体,粒径为15-1000微米,密度为50-200kg/m3,超疏水,导热系数为0.013-0.03w/m·k;
气凝胶是超疏水、低密度、低导热的,它的加入才能确保获得无机气凝胶土具有低导热、高疏水等优点;
优选的,步骤1中所述的改性剂为聚乙烯醇、邻苯二甲酸二丁酯、硅烷偶联剂KH602的一种或任意多种的混合物,稳定剂为膨润土、凹凸棒土、硅藻土、蒙脱土中的任意一种或多种混合;
改性剂和稳定剂的相互协调配合,使超疏水气凝胶粉末与水相容混合形成气凝胶浆料这一体系,并同时使得气凝胶浆料以及后续步骤2的无机气凝胶土膏状材料不沉降、不分层、不浠水,最终可以在室温下就可以凝固固化,而不需要采用其它的特殊手段;
优选的,步骤2中所述的无机胶凝材料为普通硅酸盐水泥、硫铝酸盐水泥、复合硅酸酸盐水泥,氯氧镁水泥、石膏、石灰中的任意一种或多种混合;
水泥、石灰、石膏传统的无机胶凝材料,与水搅拌后能在空气中硬化,与气凝胶浆料结合则保证了形成的无机气凝胶土在常温下就可以凝固固化;
优选的,步骤2中所述的晶须为陶瓷晶须,硫酸钙晶须,碳酸钙晶须中的任意一种或多种混合,聚丙烯纤维为长度3-20mm的纤维;
晶须是微纳米级别的短纤维,主要在微纳米这个尺度上增强复合材料,聚丙烯纤维是毫米级别的短纤维,主要在毫米这个尺度上增强复合材料。晶须和聚丙烯纤维相互协调配合,在纳米、微米、毫米三个尺度上增强无机气凝胶土,避免各个尺度上产生的微裂纹和开裂的现象,大大增强的无机气凝胶土的强度。
本发明的无机气凝胶土的制备工艺,有益效果如下:
1、无机气凝胶土具有优良的导热系数和疏水能力,是因为其中引入了超疏水、低导热的的气凝胶。气凝胶与水是不相容,而分散剂和稳定剂通过改变水溶液的特性将气凝胶与水混合形成不沉降、不分层、不浠水的气凝胶浆料,解决了气凝胶与水不容的问题,从而保证了获得气凝胶土的优良性能;
2、无机胶凝材料引入气凝胶浆料进行改性复合,是为了制备出具有一定的强度和韧性复合材料,无机晶须和聚丙烯纤维是在纳米、微米、毫米三种微观尺度上增强复合材料,从而使制备出的无机气凝胶土具有理想的强度;
3、步骤1解决了水与气凝胶不相容和的问题,步骤2解决了气凝胶浆料强度的问题,两者相互结合才能制备出优良的无机气凝胶土材料。
具体实施方式
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,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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
本实施例的一种无机气凝胶土的制备工艺,包括以下步骤:
(1)将水100份,改性剂邻苯二甲酸二丁酯1份,膨润土1份、凹凸棒土1份,50微米的气凝胶粉体8份,加入到高速搅拌分散机容器中步,然后在常温常压下以4000r/min搅拌10分钟,混合均匀获得气凝胶浆料;
(2)将普通硅酸盐水100份,碳酸钙晶须8份,3mm的聚丙烯纤维1.5份依次加入到高速分散机的容器内,然后在常温常压下以1500r/min的速度搅拌5分钟,混合均匀获得无机气凝胶土膏状材料;
(3)将步骤(2)获得无机气凝土膏状材料在室温下静置凝固、干燥,获得了保温隔音的无机气凝胶土材料。
该无机气凝胶土,密度280kg/m3,抗压强度0.25MPa,导热系数为0.048w/(m·k),吸水率3%,有机物的含量<1%,A级不燃。
实施例2
本实施例的一种无机气凝胶土的制备工艺,包括以下步骤:
(1)将水80份,改性剂聚乙烯醇1份,膨润土0.6份、凹凸棒土0.6份,75微米的气凝胶粉体10份,加入到高速搅拌分散机容器中,然后在常温常压下以5000r/min搅拌5分钟,混合均匀获得气凝胶浆料;
(2)将硫铝酸盐水泥60份,硫酸钙晶须5份,6mm的聚丙烯纤维2份依次加入到高速分散机的容器内,然后在常温常压下以1500r/min的速度搅拌5分钟,混合均匀获得无机气凝胶土膏状材料;
(3)将步骤(2)获得无机气凝土膏状材料在室温下静置凝固、干燥,获得了保温隔音的无机气凝胶土材料。
该无机气凝胶土抗压强度0.16MPa,导热系数为0.042w/(m·k),吸水率4.3%,有机物的含量<2%,A级不燃。
实施例3
本实施例的一种无机气凝胶土的制备工艺,包括以下步骤:
(1)将水100份,改性剂硅烷偶联剂kh602 1份,膨润土1份、凹凸棒土1份,15微米的气凝胶粉体10份,加入到高速搅拌分散机容器中步,然后在常温常压下以5000r/min搅拌10分钟,混合均匀获得气凝胶浆料;
(2)将普通硅酸盐水泥100份,陶瓷晶须10份,9mm的聚丙烯纤维5份依次加入到高速分散机的容器内,然后在常温常压下以1500r/min的速度搅拌5分钟,混合均匀获得无机气凝胶土膏状材料;
(3)将步骤(2)获得无机气凝土膏状材料在室温下静置凝固、干燥,获得保温隔音的无机气凝胶土材料。
该无机气凝胶土材料,抗压强度0.23MPa,导热系数为0.043w/(m·k),吸水率为2%,A级不燃。
本发明通过特殊的的配方和工艺突破解决了气凝胶粉体与无机胶凝材料难以相容的问题,先将气凝胶与水复合形成一个浆料体系然后添加无机胶凝材料,制备成了一种膏状室温静置可以凝固并具有一定强度的无机气凝胶土材料。该无机气凝胶土保温材料是一种A级防火材料,有机物含量极低,不仅避免传统保温隔音材料释放甲醛等危害人体健康的VOC气体的缺点,而且同时具有低导热、强疏水、吸音降噪的优点,可应用于建筑内下水管道产生的噪音,邻里之间的噪音以及建筑外墙的空腔,避免外面的嘈杂的声音传递到室内同时也进行了建筑的保温防护。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种无机气凝胶土的制备工艺,其特征在于包括以下制备工艺:
1)将水10-100份,改性剂0.1-5份,稳定剂0.1-5份,气凝胶粉体1-20份,加入到高速搅拌分散机中,然后在常温常压下以500-5000r/min搅拌3-20分钟,混合均匀获得了气凝胶浆料;
2)将无机胶凝材料10-100份、无机晶须1-10份、聚丙烯纤维1-5份依次加入到步骤1获得的气凝胶浆料中,然后在常温常压下以500-5000r/min的速度搅拌3-20分钟,混合均匀获得无机气凝胶土膏状材料;
3)将步骤2)获得的无机气凝胶土膏状材料在常温下静置、凝固、干燥,获得了无机气凝胶土材料。
2.按照权利要求1所述的一种无机气凝胶土的制备工艺,其特征在于步骤1)中所述气凝胶粉体是二氧化硅气凝胶粉体,粒径为15-1000微米,密度为50-200kg/m3,超疏水,导热系数为0.013-0.03w/m·k。
3.按照权利要求1所述的一种无机气凝胶土的制备工艺,其特征在于步骤1)中所述的改性剂为聚乙烯醇、邻苯二甲酸二丁酯、硅烷偶联剂KH602的一种或任意多种的混合物,稳定剂为膨润土、凹凸棒土、硅藻土、蒙脱土中的任意一种或多种混合。
4.按照权利要求1所述的一种无机气凝胶土的制备工艺,其特征在于步骤2)中所述的无机胶凝材料为普通硅酸盐水泥、硫铝酸盐水泥、复合硅酸酸盐水泥,氯氧镁水泥、石膏、石灰中的任意一种或多种混合。
5.按照权利要求4所述的一种无机气凝胶土的制备工艺,其特征在于步骤2)中所述的晶须为陶瓷晶须,硫酸钙晶须,碳酸钙晶须中的任意一种或多种混合,聚丙烯纤维为长度3-20mm的纤维。
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