CN109400064B - 一种硫酸钙晶须气凝胶泡沫混凝土及其制备方法 - Google Patents

一种硫酸钙晶须气凝胶泡沫混凝土及其制备方法 Download PDF

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CN109400064B
CN109400064B CN201811388859.9A CN201811388859A CN109400064B CN 109400064 B CN109400064 B CN 109400064B CN 201811388859 A CN201811388859 A CN 201811388859A CN 109400064 B CN109400064 B CN 109400064B
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吴会军
付平
杨丽修
徐涛
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Abstract

本发明公开了一种硫酸钙晶须气凝胶泡沫混凝土及其制备方法。本发明所述硫酸钙晶须气凝胶泡沫混凝土，其制备原料包括胶凝材料、气凝胶粉体、硫酸钙晶须、增稠剂、发泡剂和水；其中，所述胶凝材料、气凝胶粉体、硫酸钙晶须的质量比为1:0.01～0.3:0.001～0.01；所述硫酸钙晶须直径为1～10μm，长径比10～500，廉价的硫酸钙晶须掺入在气凝胶泡沫混凝土基体中，高长径比的晶须具有很强的柔性、粘结效率高，能减少气凝胶泡沫混凝土基体裂纹的扩张，显著改善了气凝胶泡沫混凝土的力学性能和成块性，还简化了制备工艺。可广泛应用于建筑墙体保温、道路填充、屏障隔声等领域。

Description

一种硫酸钙晶须气凝胶泡沫混凝土及其制备方法
技术领域
本发明属于土木建筑与保温材料领域，具体涉及一种硫酸钙晶须气凝胶泡沫混凝土及其制备方法。
背景技术
泡沫混凝土是一种节能、环保型墙体保温材料，具有密度小、保温隔热性好、隔音耐火性强和抗震性优良等特点，被广泛用于建筑节能等领域。但轻质的泡沫混凝土也存在一定的局限性，例如强度低、吸水开裂等缺点。
随着泡沫混凝土的快速发展，目前，市面上已出现掺杂各种外加料的泡沫混凝土，而气凝胶泡沫混凝土是其中最为轻质的泡沫混凝土；气凝胶是一种轻质多孔、非晶体固体材料，具有超级保温隔热性能，将气凝胶掺入泡沫混凝土中具有降低泡沫混凝土的自重和填充气孔孔隙的潜在优势，有望在低孔隙率下制备出低密度，低导热的泡沫混凝土。专利CN205804646 U提出了一种气凝胶泡沫混凝土保温防火板，该板具有低密度、低导热系数、低吸水率，但气凝胶与胶凝材料之间常常因为界面强度低，导致泡沫混凝土力学性能显著降低，且容易导致气凝胶粉体从混凝土基体中脱落，严重影响泡沫混凝土的工程应用。文献《轻质低导热气凝胶泡沫混凝土的制备与性能实验研究》实验制备出一种密度270.2kg/m3、导热系数0.069W/(m.K)的超轻质泡沫混凝土，但制做的泡沫混凝土存在孔径大小不均匀、强度低等缺点，难以获得较高力学性能的超轻泡沫混凝土。
近年来，在人工控制条件下以单晶形式生长制得纤维—晶须，其直径非常小(微米数量级)而且原子排列高度有序，使其具有高强度、高模量和高伸长率，在复合材料增强方面取得了显著的效果，明显优于其他短切纤维或纤维毡。其中，硫酸钙晶须是以生石膏为原料经特定工艺及配方合成的硫酸钙纤维状单晶体，具有单晶形式、均匀横截面和完善的内部结构，使其具有高强度、高模量、高韧性耐磨耗、耐高温、耐酸碱、抗腐蚀、无毒等特点，作为增强材料具有广泛应用前景。
发明内容
为解决现有技术的缺点和不足之处，本发明的首要目的在于提供一种硫酸钙晶须气凝胶泡沫混凝土保温材料，该保温材料在具有超轻、良好保温隔热性能的同时，也使得气凝胶泡沫混凝土具有良好的力学性能和稳定性。
将硫酸钙晶须用于气凝胶泡沫混凝土增强，一方面利用硫酸钙晶须的针状完善结构和高强度、高模量、高伸长率，可取得较短切纤维或纤维毡更好的泡沫混凝土增强效果；另一方面，由于硫酸钙晶须的微细直径与气凝胶粉体纳米尺寸更为接近，可获得更好的界面优化性能，从而有效提高泡沫混凝土的稳定性和可靠性。
本发明的另一目的在于提供了一种硫酸钙晶须气凝胶泡沫混凝土的制备方法。克服现有技术中制备工艺复杂、气凝胶与混凝土结合程度不高等问题。
本发明目的通过以下技术方案实现：
一种硫酸钙晶须气凝胶泡沫混凝土材料，其制备原材料包括胶凝材料、气凝胶粉体、硫酸钙晶须、增稠剂、发泡剂和水；其中，所述胶凝材料、气凝胶粉体、硫酸钙晶须的质量比为1:0.01～0.3:0.001～0.01；所述硫酸钙晶须呈均匀分散状，直径为1～10μm，长径比为10～500。
所述硫酸钙晶须气凝胶泡沫混凝土材料是先将增稠剂和水配制成增稠水，将发泡剂和水制成泡沫；然后将胶凝材料、气凝胶粉体、硫酸钙晶须和增稠水制成硫酸钙晶须气凝胶混凝土浆体，再将硫酸钙晶须气凝胶混凝土浆体与泡沫混合得到混合浆体，最后将混合浆体进行静置及养护后得到。
进一步地，所述硫酸钙晶须呈均匀分散状。
本发明通过在泡沫混凝土中掺入轻质多孔网络结构、导热系数低于空气(常温下0.023W·m-1·K-1)的气凝胶粉体，并通过掺入分散状硫酸钙晶须增强气凝胶泡沫混凝土的力学性能和柔韧性；本发明不需要对气凝胶粉体进行疏水改性，大大简化了气凝胶泡沫混凝土的制备工艺；另外，分散状硫酸钙晶须掺入在气凝胶泡沫混凝土基体中，高长径比的晶须具有很强的柔性、粘结效率高，能减少气凝胶泡沫混凝土基体裂纹的扩张，显著改善了气凝胶泡沫混凝土的力学性能和成块性。
本发明所述气凝胶是一种轻质、多孔的非晶体固体材料，呈网络结构，具有超级保温隔热性能，即常温下其热导率可低至0.013W·m-1·K-1、比表面积高达 500～1000m2·g-1、密度低至0.003g·cm-3和孔隙尺寸约为10～100nm。
进一步地，所述气凝胶粉体包括二氧化硅气凝胶粉体、粘土气凝胶粉体、碳气凝胶粉体、聚乙烯醇气凝胶粉体和金属醇盐气凝胶粉体中的一种或者至少两种以上。
进一步地，所述增稠剂包括钠基膨润土、有机膨润土、硅藻土、棒石土、硅凝胶、甲基纤维素、羟丙基甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、淀粉和明胶中的一种或者至少两种以上；所述发泡剂包括茶皂素发泡剂、皂角苷发泡剂、松香类发泡剂、蹄角发泡剂和毛发角质蛋白发泡剂中的一种或者至少两种以上。
使用增稠剂的目的是使气凝胶粉体与胶凝材料能够充分均匀的混合，防止气凝胶粉体与胶凝材料出现分层现象，漂浮在浆体上面。
进一步地，所述水分为两部分，第一部分水用于配制增稠水，该部分水与增稠剂按质量比1000:1～100:1混合并搅拌均匀后得到增稠水，所述胶凝材料、气凝胶粉体、硫酸钙晶须和增稠水的质量比为1:0.01～0.3:0.001～0.01:0.35～1；第二部分水用于与发泡剂制备泡沫。
进一步地，所述发泡剂与第二部分水的质量比为1/100～1/10，将发泡剂与水混合液采用机械加压法制成泡沫，制作泡沫的密度控制在25～60kg/m3，实验发现在该范围内泡沫的稳定性能最好；所加入的泡沫与胶凝材料的质量比为 0.1～0.5:1。
本发明所述机械加压法是通过空气压缩机给发泡机加压发泡，即机械搅拌预制泡沫法，属于物理发泡。
进一步地，所述胶凝材料包括硅酸盐水泥、铝酸盐水泥、硫铝酸盐水泥、氯氧镁水泥、矿渣水泥、粉煤灰水泥、火山灰质水泥、石灰、石膏、水玻璃、沥青、树脂和聚合物中的一种或者至少两种以上。
一种硫酸钙晶须气凝胶泡沫混凝土的制备方法，包括以下步骤：
(1)将增稠剂和水配制成增稠水；将胶凝材料与气凝胶粉体混合，加入增稠水，搅拌均匀得到气凝胶混凝土浆；然后再加入硫酸钙晶须，搅拌均匀，得到硫酸钙晶须气凝胶混凝土浆体；
(2)将发泡剂与水混合后进行发泡，然后将泡沫加入硫酸钙晶须气凝胶混凝土浆体中，混合搅拌，得到硫酸钙晶须气凝胶泡沫混凝土浆体；其中，所加入的泡沫与胶凝材料的质量比为0.1～0.5:1；
(3)将硫酸钙晶须气凝胶泡沫混凝土浆体静置和养护后，得到一种硫酸钙晶须气凝胶泡沫混凝土。
进一步地，步骤(3)所述静置和养护，包括将硫酸钙晶须气凝胶泡沫混凝土浆体倒入模具内，使用薄膜封盖，静置24～48小时后拆模，再进行养护。
进一步地，步骤(3)所述养护包括常温常压养护、恒温恒湿箱养护、干燥箱养护、温湿交变箱养护、喷雾养护、浸水养护或蒸压养护中的一种。
进一步地，步骤(3)所述养护的温度为40～80℃，养护的湿度为50～95％RH。
本发明还提供了一种硫酸钙晶须增强气凝胶泡沫混凝土材料在建筑墙体保温、冷藏运输、道路填充和屏障隔声等领域的应用。
与现有技术相比，本发明具有如下优点和有益效果：
(1)利用硫酸钙晶须的高度有序结构和高强度、高模量、高韧性等优良性能显著改善了气凝胶泡沫混凝土的力学性能和成块性。
(2)采用硫酸钙晶须，其直径为1～10μm、长径比为10～500，其均匀分散在气凝胶泡沫混凝土基体中，高长径比的晶须具有很强的柔性、粘结效率高，能减少气凝胶泡沫混凝土基体裂纹的扩张，起到硫酸钙晶须增韧的效果。
(3)本发明采用增稠水替换气凝胶粉体疏水改性步骤，极大的简化气凝胶泡沫混凝土的制备工艺，使得制备工艺更加简单，易操作。
(4)利用硫酸钙晶须的高熔点使气凝胶泡沫混凝土具有良好的耐高温性能，且高温下不产生有害气体，安全性高。使得本发明制备的硫酸钙晶须气凝胶泡沫混凝土具有超级保温隔热性能，防火性能好及使用寿命长等优点，可广泛应用于建筑墙体保温，道路填充，屏障隔声等领域，有巨大的市场应用前景。
附图说明
图1是制备硫酸钙晶须气凝胶泡沫混凝土的工艺流程图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。如无特别说明，本发明所有原料均能从市场上直接购买得到。
实施例1
本实施例制备硫酸钙晶须粘土气凝胶泡沫混凝土，是以粘土气凝胶粉体为填充材料，其粒径为85目(约162μm)、孔隙率为95％、孔隙直径为45nm；以分散状的硫酸钙晶须为增强体，直径为1μm、长径比为10。具体制备步骤如下：
(1)将水与有机膨润土按照质量比1000:1.5进行混合，并搅拌均匀，得到增稠水；
(2)将硅酸盐PO42.5水泥与粘土气凝胶粉体进行干混，然后加入步骤(1) 得到的增稠水，搅拌均匀，得到粘土气凝胶混凝土浆体；其中硅酸盐PO42.5水泥、粘土气凝胶粉体和增稠水三者之间的质量比为1:0.10:0.7；
(3)将呈分散状的硫酸钙晶须缓慢加入至步骤(2)得到的粘土气凝胶混凝土浆体中，搅拌均匀，得到硫酸钙晶须/粘土气凝胶混凝土浆体；其中，硅酸盐PO42.5水泥、粘土气凝胶粉体和硫酸钙晶须三者之间的质量比为1:0.1:0.003；
(4)将松香类发泡剂与水按照质量比为1/40混合，再采用机械加压进行发泡，得到泡沫的密度为45kg/m3，然后将其加入至步骤(3)得到的硫酸钙晶须 /粘土气凝胶混凝土浆体中，混合搅拌，得到硫酸钙晶须/粘土气凝胶泡沫混凝土浆体。其中，所加入的泡沫与胶凝材料硅酸盐PO42.5水泥的质量比为0.15:1。
(5)将步骤(4)得到的硫酸钙晶须/粘土气凝胶泡沫混凝土浆体倒入模具内，使用薄膜封盖，静置24h后拆模，最后在温度为60℃、湿度为60％RH的恒温恒湿箱内进行养护，28d后取出，得到硫酸钙晶须粘土气凝胶泡沫混凝土样品1。
实施例2
本实施例制备硫酸钙晶须碳气凝胶泡沫混凝土，是以碳气凝胶粉体为填充材料，其粒径为80目(约180μm)、孔隙率为93％、孔隙直径为40nm；以分散状的硫酸钙晶须为增强体，直径为5μm、长径比为100。具体制备步骤如下：
(1)将水与棒石土按质量比例1000:3进行混合，并搅拌均匀，得到增稠水；
(2)将氯氧镁PO42.5水泥与碳气凝胶粉体进行干混，然后加入步骤(1) 配制的增稠水，搅拌均匀，得到碳气凝胶混凝土浆体；所述氯氧镁PO 42.5水泥、碳气凝胶粉体和增稠水三者之间的质量比为1:0.2:0.8；
(3)将呈分散状的硫酸钙晶须缓慢加入至步骤(2)得到的碳气凝胶混凝土浆体中，搅拌均匀，得到硫酸钙晶须/碳气凝胶混凝土浆体；其中，氯氧镁PO 42.5水泥、碳气凝胶粉体和硫酸钙晶须三者之间的质量比为1:0.2:0.006；
(4)将蹄角发泡剂与水按照质量比为1/60混合，再采用机械加压进行发泡，得到泡沫的密度为50kg/m3。然后将其加入至步骤(3)得到的硫酸钙晶须/碳气凝胶混凝土浆体中，混合搅拌，得到硫酸钙晶须/碳气凝胶泡沫混凝土浆体。其中，所加入的泡沫与胶凝材料氯氧镁PO42.5水泥的质量比为0.2:1。
(5)将步骤(4)得到的硫酸钙晶须/碳气凝胶泡沫混凝土浆体倒入模具内，使用薄膜封盖，静置30h后拆模，最后在温度为50℃、湿度为70％RH的恒温恒湿箱内进行养护，28d后取出，得到硫酸钙晶须碳气凝胶泡沫混凝土样品2。
实施例3
本实施例制备硫酸钙晶须SiO2气凝胶泡沫混凝土，是以SiO2气凝胶粉体为填充材料、其粒径为70目(约212μm)、孔隙率为90％、孔隙直径为35nm；以分散状的硫酸钙晶须为增强体，直径为10μm、长径比为500。具体制备步骤如下：
(1)将水与硅藻土按质量比例1000:5进行混合，并搅拌均匀，得到增稠水；
(2)将硫铝酸盐PO 42.5水泥与SiO2气凝胶粉体进行干混，然后加入步骤 (1)配制的增稠水，搅拌均匀，得到SiO2气凝胶混凝土浆体；所述硫铝酸盐PO 42.5水泥、SiO2气凝胶粉体和增稠水三者之间的质量比为1:0.3:0.9；
(3)将呈分散状的硫酸钙晶须缓慢加入至步骤(2)得到的SiO2气凝胶混凝土浆体中，搅拌均匀，得到硫酸钙晶须/SiO2气凝胶混凝土浆体；其中，硫铝酸盐PO 42.5水泥、SiO2气凝胶粉体和硫酸钙晶须三者之间的质量比为1:0.3:0.01；
(4)将皂角苷发泡剂与水按照质量比为1/80混合，再采用机械加压进行发泡，得到泡沫的密度为55kg/m3。然后将其加入至步骤(3)得到的硫酸钙晶须 /SiO2气凝胶混凝土浆体中，混合搅拌，得到硫酸钙晶须/SiO2气凝胶泡沫混凝土浆体。其中，所加入的泡沫与胶凝材料硫铝酸盐PO 42.5水泥的质量比为0.25:1。
(5)将步骤(4)得到的硫酸钙晶须/SiO2气凝胶泡沫混凝土浆体倒入模具内，使用薄膜封盖，静置36h后拆模，最后在温度为40℃、湿度为80％RH的恒温恒湿箱内进行养护，28d后取出，得到硫酸钙晶须SiO2气凝胶泡沫混凝土样品3。
按照标准《泡沫混凝土》JG/T266-2011测试泡沫混凝土的密度，试验前取三块相同试件放入电热鼓风干燥箱，在105℃下烘干直到质量恒定；取三次结果的平均值，再已知试块体积，利用密度公式计算得出纤维气凝胶泡沫混凝土的密度；试样参照GB10294-2008执行，试验前先将试件放入电热鼓风干燥箱内，在105℃连续烘干4小时，然后取出试件，放至干燥器中冷却至室温，实验采用由瑞典Hot Disk公司生产的型号为1500S的热导率分析仪测试其导热系数。按照标准《泡沫混凝土》JG/T266-2011测试其抗压强度，试验前将砌块放于温度为(60±5)℃干燥箱内烘干至前后两次相隔4小时质量差不大于0.1g的恒质量。测试仪器由上海试验设备贸易有限公司生产的型号INSTRON-5984的强度万能试验机进行测试。
经检测，上述制备的硫酸钙晶须粘土气凝胶泡沫混凝土样品1、硫酸钙晶须碳气凝胶泡沫混凝土样品2、硫酸钙晶须SiO2气凝胶泡沫混凝土样品3的密度均在200kg/m3以下，导热系数均在0.4～0.25W·m-1·K-1，均可耐800℃高温，抗压强度可达1MPa以上，压缩模量可达5MPa，具有超级隔热性能、耐火不燃、密度低等优点，能显著提高改善气凝胶泡沫混凝土的成块性与力学性能。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (6)

1.一种硫酸钙晶须气凝胶泡沫混凝土，其特征在于，其制备原料包括胶凝材料、气凝胶粉体、硫酸钙晶须、增稠剂、发泡剂和水；其中，所述胶凝材料、气凝胶粉体、硫酸钙晶须的质量比为1:0.01～0.3:0.001～0.01；所述硫酸钙晶须直径为1～10μm，长径比为10～500；所述气凝胶粉体包括二氧化硅气凝胶粉体、粘土气凝胶粉体、碳气凝胶粉体、聚乙烯醇气凝胶粉体和金属醇盐气凝胶粉体中的一种或者至少两种以上；
所述的水分为两部分，第一部分水用于配制增稠水，该部分水与增稠剂按质量比1000:1～100:1混合并搅拌均匀后得到增稠水，所述胶凝材料、气凝胶粉体、硫酸钙晶须和增稠水的质量比为1:0.01～0.3:0.001～0.01:0.35～1；第二部分水用于与发泡剂制备泡沫；所述发泡剂与第二部分水的质量比为1/100～1/10，发泡剂与水采用机械加压法制成泡沫，制作泡沫的密度控制在25～60kg/m3；所加入的泡沫与胶凝材料的质量比为0.1～0.5:1；
所述硫酸钙晶须增强气凝胶泡沫混凝土是先将增稠剂和水配制成增稠水，将发泡剂和水制成泡沫；然后将胶凝材料、气凝胶粉体、硫酸钙晶须和增稠水制成硫酸钙晶须气凝胶混凝土浆体，再将硫酸钙晶须气凝胶混凝土浆体与泡沫混合得到混合浆体，最后将混合浆体进行静置及养护后得到。
2.根据权利要求1所述的一种硫酸钙晶须气凝胶泡沫混凝土，其特征在于，所述硫酸钙晶须呈均匀分散状。
3.根据权利要求1或2所述的一种硫酸钙晶须气凝胶泡沫混凝土，其特征在于，所述增稠剂包括钠基膨润土、有机膨润土、硅藻土、棒石土、硅凝胶、甲基纤维素、羟丙基甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、淀粉和明胶中的一种或者至少两种以上；所述发泡剂包括茶皂素发泡剂、皂角苷发泡剂、松香类发泡剂、蹄角发泡剂和毛发角质蛋白发泡剂中的一种或者至少两种以上。
4.根据权利要求1或2所述的一种硫酸钙晶须气凝胶泡沫混凝土，其特征在于，所述胶凝材料包括硅酸盐水泥、铝酸盐水泥、硫铝酸盐水泥、氯氧镁水泥、矿渣水泥、粉煤灰水泥、火山灰质水泥、石灰、石膏、水玻璃、沥青、树脂和聚合物中的一种或者至少两种以上。
5.权利要求1至4任一项所述的一种硫酸钙晶须气凝胶泡沫混凝土的制备方法，其特征在于，包括以下步骤：
(1)将增稠剂和水配制成增稠水；将胶凝材料与气凝胶粉体混合，加入增稠水，搅拌均匀得到气凝胶混凝土浆；然后再加入硫酸钙晶须，搅拌均匀，得到硫酸钙晶须气凝胶混凝土浆体；
(2)将发泡剂与水混合后进行发泡，然后将泡沫加入硫酸钙晶须气凝胶混凝土浆体中，混合搅拌，得到硫酸钙晶须气凝胶泡沫混凝土浆体；其中，所加入的泡沫与胶凝材料的质量比为0.1～0.5:1；
(3)将硫酸钙晶须气凝胶泡沫混凝土浆体静置和养护后，得到所述硫酸钙晶须气凝胶泡沫混凝土。
6.权利要求1至4任一项所述的一种硫酸钙晶须气凝胶泡沫混凝土材料在建筑墙体保温、冷藏运输、道路填充和屏障隔声领域中的应用。
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