CN116283253B - 一种抗菌泡沫陶瓷及其制备方法 - Google Patents
一种抗菌泡沫陶瓷及其制备方法 Download PDFInfo
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- CN116283253B CN116283253B CN202310205120.4A CN202310205120A CN116283253B CN 116283253 B CN116283253 B CN 116283253B CN 202310205120 A CN202310205120 A CN 202310205120A CN 116283253 B CN116283253 B CN 116283253B
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Abstract
本发明涉及一种抗菌泡沫陶瓷，由溶胶‑凝胶法制备出陶瓷浆料，然后通过模板法制备得到，其中陶瓷浆料包括硅溶胶、甲基三甲氧基硅烷、γ‑(2,3‑环氧丙氧基)丙基三甲氧基硅烷、NaOH溶液、石墨烯分散液、填料、颜料、弱酸和去离子水。本发明通过溶胶‑凝胶法制备陶瓷浆料，再结合模板法，经过溶胀预处理、浸渍吸浆、低温烘烤定型、热解等步骤，在较低温度下即可得到高性能泡沫陶瓷材料。与传统的陶瓷粉共混法制备陶瓷浆料，经模板法烧结制备泡沫陶瓷的方法相比，大大降低了泡沫陶瓷的制备温度和能耗。
Description
技术领域
本发明属于多孔陶瓷体领域，具体涉及一种抗菌泡沫陶瓷及其制备方法。
背景技术
泡沫陶瓷是一种具有三维空间网状结构的高气孔率的多孔陶瓷体，其造型上像钢化了的泡沫塑料或瓷化了的海绵体。由于它具有气孔率高、比表面积大、耐高温、耐化学腐蚀及良好的机械强度和过滤吸附性能，可广泛应用于隔热隔音保温材料、化学催化剂载体、工业污水处理等环境保护领域，以及耐火材料、生物材料等。
泡沫陶瓷材质由最初的普通粘土质发展到耐高温、耐腐蚀、耐热冲击性材质(如碳化硅、氧化铝、堇青石、钛酸铝、莫来石、锂辉石等)。不论采用哪种材质，都是将陶瓷粉共混后制得浆料，需要经过1000℃以上高温烧结的过程来制备，能耗非常高。例如：公开号为202011450493.0的中国发明专利公开了一种碳纤维增韧碳化硅泡沫陶瓷及其制备方法的技术方案，该技术方案需要在1450-1600℃高温下保温3-5小时，然后再在1000℃下保温3-5小时；公开号为201910422486.0的中国发明专利公开了一种泡沫陶瓷及其制备方法的技术方案，该方案通过将半焦和赤泥烧结的方式制得泡沫陶瓷，烧结温度为1100-1250℃并保温1-3小时。如何降低泡沫陶瓷的制备温度，降低能耗是我们需要努力的方向。
发明内容
本发明的目的是针对现有技术中存在的问题，提供一种抗菌泡沫陶瓷及其制备方法，可降低泡沫陶瓷的制备温度及能耗，增加泡沫陶瓷的韧性，防止开裂，并赋予泡沫陶瓷广谱抗菌性能，扩大泡沫陶瓷的应用范围。
本发明的目的可以通过以下方案来实现：
本发明提供了一种抗菌泡沫陶瓷，所述抗菌泡沫陶瓷由溶胶-凝胶法制备出陶瓷浆料，然后通过模板法制备得到，所述陶瓷浆料包括以下质量分数的各组分：
作为本发明的一个实施方案，所述硅溶胶中二氧化硅颗粒的粒径为80-150nm，固含量≥40％。硅溶胶是溶胶-凝胶反应的主要成膜物质，粒径小固含低则生成的陶瓷泡沫耐压强度低。
甲基三甲氧基硅烷是溶胶-凝胶反应的辅助成膜物质，是水解速度最快的硅烷，可缩短反应时间，提高生产效率。γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷是溶胶-凝胶反应的辅助成膜物质，含柔性分子链，可增加泡沫陶瓷的柔韧性；加入量太少，制备出的泡沫陶瓷脆性大易开裂；加入量太多，导致成品颜色发黄、抗压强度降低。
作为本发明的一个实施方案，NaOH溶液的质量百分浓度为1-1.5％；调节研磨后色浆的pH值在9.5以上。选用NaOH是因为它常见便宜，且碱性合适，易调节pH值；若选用碱性更强的碱(如KOH)，则需要配制成浓度更低的溶液，配方中引入更多的水，将导致固含降低，制得的陶瓷泡沫耐压强度低；若选用碱性更弱的碱(如Na2CO3)，对pH的调节作用太弱，pH值的变化小。
作为本发明的一个实施方案，所述石墨烯分散液中石墨烯的固含量为20-30％。石墨烯分散液可增加泡沫陶瓷的韧性和强度；还能够赋予体系良好的广谱抗菌性能。石墨烯分散液选用WJ-WG01(合肥微晶材料科技有限公司)。
作为本发明的一个实施方案，所述填料包括煅烧高岭土、重钙、云母粉、气相二氧化硅、硅微粉、纳米氧化铝中的一种或几种。所述颜料包括钛白粉、铜铬黑、氧化铁黄、氧化铁红、钴蓝中的一种或几种；本发明中的颜料，仅提供颜色，可根据制备的陶瓷泡沫的颜色选择相应的颜料。
作为本发明的一个实施方案，所述弱酸包括甲酸、乙酸中的一种或多种。甲酸溶液的质量百分浓度为20-30％，优选为25％。乙酸溶液的质量百分浓度高于90％，或为不稀释的乙酸，由于酸性弱，故乙酸添加量需要略增加。弱酸为溶胶-凝胶反应催化剂，涂料制备完成后pH值控制在4.2-4.8之间；如用纯甲酸添加量太少，少量的添加误差可以引起涂料pH值的较大波动，将甲酸稀释成25％左右的溶液，可以减少添加误差引起的pH值波动。
本发明还提供了一种抗菌泡沫陶瓷的制备方法，所述制备方法包括如下步骤
S1、陶瓷浆料的制备：
S1-1、制备色浆：按照质量分数称取各组分原料，将硅溶胶、NaOH溶液、填料、颜料、去离子水混合，研磨、过滤后，滤液中加入石墨烯分散液，混合均匀后得到色浆；
S1-2、将甲基三甲氧基硅烷、γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷混合后加入弱酸混合均匀，然后倒入所得色浆中混合均匀，得陶瓷浆料；
S2、泡沫塑料溶胀预处理：
将泡沫塑料放入丙酮溶液中，浸泡后冲洗、烘干后待用；
S3、浸渍吸浆：
将预处理后的泡沫塑料浸渍于所得陶瓷浆料中，然后取出自然风干、烘干，得吸浆泡沫塑料；
S4、热解除去泡沫塑料：
将所得吸浆泡沫塑料高温热解，待泡沫塑料完全热解后，最后经自然降温后得到泡沫陶瓷。
作为本发明的一个实施方案，步骤S1-1中，所述研磨的细度小于20μm，研磨在研磨机上进行，使固体颗粒的粒径小于20μm；过滤是使用250-350目滤布过滤，优选300目。
作为本发明的一个实施方案，步骤S1-2中，色浆的混合是在10-35℃的温度下，以100-180转/分的转速反应4-5小时。该陶瓷浆料通过溶胶-凝胶反应得到，首先硅烷在有机酸的催化下水解生成硅醇，然后硅醇与硅溶胶发生缩聚反应，形成具有Si-O-Si交联结构的大分子。
本发明中制备好色浆部分再与硅烷混合，色浆部分需要调整pH值为碱性，且大于9.5，因为色浆部分储存时pH值会略下降，当pH下降到9.0以下时，由于硅溶胶无法稳定存在而发生沉降，色浆即失效。同时，色浆单独研磨，可以作为半成品储存，利于提高研磨效率。
作为本发明的一个实施方案，步骤S2中，泡沫塑料包括聚氨酯泡沫塑料、聚苯乙烯塑料泡沫中的一种。
作为本发明的一个实施方案，步骤S2中，浸泡是在在常温下浸泡5-30分钟，待泡沫塑料表面轻微溶胀后用清水冲洗。步骤S2为了使泡沫表面粗糙度增加，结构发生改变，易于后期上浆，经预处理过的泡沫塑料挂浆量达到30g/g以上。
作为本发明的一个实施方案，步骤S3中，泡沫塑料浸渍时，用压辊反复挤压3次以上，优选为3-5次，使泡沫塑料的孔隙吸饱陶瓷浆料。自然风干是时间为24-48小时；烘干的温度为150-200℃，时间为8-12小时。
作为本发明的一个实施方案，步骤S4中，高温热解是升温至500-550℃，并保温1-2小时。升温速度为15-25℃/min。保温时待泡沫塑料完全热解后，最后经自然降温后得到泡沫陶瓷。步骤S4是在高温热解气化炉中进行。
与现有技术相比，本发明具有如下有益效果：
(1)本发明提出了一种溶胶-凝胶法结合模板法制备高性能泡沫陶瓷的方法，溶胶-凝胶法是化学反应的方法，可形成的结构为Si-O-Si类似陶瓷的无机结构，只需在150-200℃低温下即可固化成型，不需要经过高温烧结的过程，通过溶胶-凝胶法制备陶瓷浆料，再结合模板法，经过溶胀预处理、浸渍吸浆、低温烘烤定型、热解等步骤，在500℃以下的较低温度下即可得到高性能泡沫陶瓷材料。与传统的陶瓷粉共混法制备陶瓷浆料，经模板法烧结制备泡沫陶瓷的方法(该方法是将陶瓷粉在七八百度甚至上千度融化后形成浆料)相比，大大降低了泡沫陶瓷的制备温度和能耗；传统的溶胶-凝胶法仅可制备孔径为纳米级的微孔泡沫陶瓷薄膜，本发明结合了模板法，可制备出大孔体型泡沫陶瓷材料。
(2)本发明得到的泡沫陶瓷，以Si-O-Si无机交联结构为骨架，具有抗压强度高的特点，由于陶瓷浆料中加入了γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷和石墨烯分散液，增加了泡沫陶瓷的柔韧性，防止泡沫陶瓷的开裂；
(3)由于加入了石墨烯分散液，使得泡沫陶瓷具有广谱抗菌性，对金黄色葡萄球菌、大肠杆菌、白色念珠菌、绿脓杆菌、真菌等，均具有优异的杀菌和抑菌作用。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实例在本发明技术方案的前提下进行实施，提供了详细的实施方式和具体的操作过程，将有助于本领域的技术人员进一步理解本发明。需要指出的是，本发明的保护范围不限于下述实施例，在本发明的构思前提下做出的若干调整和改进，都属于本发明的保护范围。
实施例1
本实施例提供了一种抗菌泡沫陶瓷，所述抗菌泡沫陶瓷由溶胶-凝胶法制备出陶瓷浆料，然后通过模板法制备得到，具体制备方法如下：
1、陶瓷浆料的制备：
(1)制备色浆：按表1的质量分数称取原料，将硅溶胶、NaOH溶液、填料、颜料、去离子水混合，在研磨机上研磨至细度小于20μm，用300目滤布过滤后，加入石墨烯分散液，混合均匀后得到色浆。
(2)将甲基三甲氧基硅烷、γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷混合均匀后，加入甲酸溶液混合均匀，然后倒入步骤(1)制备出的色浆组分中混合均匀，在25℃下，以120转/分的转速反应4.5小时。该陶瓷浆料通过溶胶-凝胶反应得到，首先硅烷在有机酸的催化下水解生成硅醇，然后硅醇与硅溶胶发生缩聚反应，形成具有Si-O-Si交联结构的大分子。
2、聚氨酯泡沫塑料溶胀预处理：
将聚氨酯泡沫塑料放入丙酮溶液中，在常温下浸泡15分钟，待聚氨酯泡沫塑料表面轻微溶胀后，用清水冲洗，烘干后待用；该步骤为了使聚氨酯泡沫表面粗糙度增加，结构发生改变，易于后期上浆，经预处理过的聚氨酯泡沫塑料挂浆量达到30g/g以上。
3、浸渍吸浆：
将预处理后的聚氨酯泡沫塑料浸渍于步骤1得到的陶瓷浆料中，并用压辊反复挤压4次，使泡沫塑料的孔隙吸饱陶瓷浆料，然后自然风干36小时后，在180℃下烘干10小时。
4、热解除去聚氨酯泡沫塑料
将步骤3得到样块放入高温热解气化炉中，以20℃/min的升温速度，由室温升至500℃，并保温1小时，待泡沫塑料完全热解后，最后经自然降温后得到泡沫陶瓷。
表1
其中，表1中的硅溶胶粒径为100-120nm，固含量50％，NaOH溶液的质量百分浓度为1％，石墨烯分散液选择WJ-WG01(合肥微晶材料科技有限公司)，甲酸溶液的质量百分浓度为25％。
实施例2
本实施例提供一种抗菌泡沫陶瓷，组分如表1所示，制备方法与实施例1相同。
实施例3
本实施例提供一种抗菌泡沫陶瓷，组分如表1所示，制备方法与实施例1相同。
实施例4
本实施例提供一种抗菌泡沫陶瓷，组分如表1所示，制备方法与实施例1相同。
对比例1
本对比例提供了一种抗菌泡沫陶瓷，制备方法与实施例1基本相同，区别之处仅在于：未加入γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷，甲基三甲氧基硅烷用量为26％。
对比例2
本对比例提供了一种抗菌泡沫陶瓷，制备方法与实施例1基本相同，区别之处仅在于：将甲基三甲氧基硅烷替换为甲基三乙氧基硅烷。
由于甲基三乙氧基硅烷水解速度慢，在该反应时间下还没水解完全，无法形成均一的浆料体系，不进行后续步骤及性能测试，若使用甲基三乙氧基硅烷需要延长反应时间至14-16小时才可以形成均相体系。
对比例3
本对比例提供了一种抗菌泡沫陶瓷，制备方法与实施例1基本相同，区别之处仅在于：未加石墨烯分散液。制备的泡沫陶瓷进行抗菌测试，结果细菌正常繁殖，不具备抗菌效果。
对比例4
本对比例提供了一种抗菌泡沫陶瓷，制备方法与实施例1基本相同，区别之处仅在于：聚氨酯泡沫塑料溶胀预处理时间为40分钟。
对比例5
本对比例提供了一种抗菌泡沫陶瓷，制备方法与实施例1基本相同，区别之处仅在于：浸渍吸浆步骤用压辊挤压2次。
主要性能测试如表2所示：
表2
其中，各性能测试标准如下：
抗压强度：万能力学试验机，压头移动速率0.5mm/min，抗压强度＝施加在有效面积上的压力(N)/受压面积(mm2)；
挂浆量：(聚氨酯泡沫挂浆后质量-聚氨酯泡沫挂浆前质量)/聚氨酯泡沫挂浆前质量；
真气孔率：密度法；真气孔率过大，抗压强度会低；过小，影响其使用的效果，例如：作为隔热隔音保温材料的效果、化学催化剂载体的催化效果、工业污水处理的效果等。
耐冷热冲击：首先300℃32min，然后0℃32min为一个循环，放大镜观察，重复10个循环。
本发明还进行了抗菌性检测，标准或方法为GB/T 21866-2008，结果如表3所示。
表3
以上对本发明的具体实施例进行了描述。需要理解的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变形或修改，这并不影响本发明的实质内容。
Claims (10)
1.一种抗菌泡沫陶瓷，其特征在于，所述抗菌泡沫陶瓷由溶胶-凝胶法制备出陶瓷浆料，然后通过模板法制备得到，所述陶瓷浆料包括以下质量分数的各组分：
2.根据权利要求1所述的抗菌泡沫陶瓷，其特征在于，所述硅溶胶中二氧化硅颗粒的粒径为80-150nm，固含量≥40％。
3.根据权利要求1所述的抗菌泡沫陶瓷，其特征在于，NaOH溶液的质量百分浓度为1-1.5％。
4.根据权利要求1所述的抗菌泡沫陶瓷，其特征在于，所述石墨烯分散液中石墨烯的固含量为20-30％。
5.根据权利要求1所述的抗菌泡沫陶瓷，其特征在于，所述填料包括煅烧高岭土、重钙、云母粉、气相二氧化硅、硅微粉、纳米氧化铝中的一种或几种；所述颜料包括钛白粉、铜铬黑、氧化铁黄、氧化铁红、钴蓝中的一种或几种。
6.根据权利要求1所述的抗菌泡沫陶瓷，其特征在于，所述弱酸包括甲酸、乙酸中的一种或多种。
7.一种如权利要求1所述的抗菌泡沫陶瓷的制备方法，其特征在于，所述制备方法包括如下步骤：
S1、陶瓷浆料的制备：
S1-1、制备色浆：按照质量分数称取各组分原料，将硅溶胶、NaOH溶液、填料、颜料、去离子水混合，研磨、过滤后，滤液中加入石墨烯分散液，混合均匀后得到色浆；
S1-2、将甲基三甲氧基硅烷、γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷混合后加入弱酸混合均匀，然后倒入所得色浆中混合均匀，得陶瓷浆料；
S2、泡沫塑料溶胀预处理：
将泡沫塑料放入丙酮溶液中，浸泡后冲洗、烘干后待用；
S3、浸渍吸浆：
将预处理后的泡沫塑料浸渍于所得陶瓷浆料中，然后取出自然风干、烘干，得吸浆泡沫塑料；
S4、热解除去泡沫塑料：
将所得吸浆泡沫塑料高温热解，待泡沫塑料完全热解后，得到所述抗菌泡沫陶瓷。
8.根据权利要求7所述的抗菌泡沫陶瓷的制备方法，其特征在于，步骤S1-2中，色浆的混合是在10-35℃的温度下，以100-180转/分的转速反应4-5小时。
9.根据权利要求7所述的抗菌泡沫陶瓷的制备方法，其特征在于，步骤S3中，自然风干是时间为24-48小时；烘干的温度为150-200℃，时间为8-12小时。
10.根据权利要求7所述的抗菌泡沫陶瓷的制备方法，其特征在于，步骤S4中，高温热解是升温至500℃，并保温1-2小时。
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