CN110818417B - 一种净化空气用炭-碳化硅多孔过滤器及其制备方法 - Google Patents

一种净化空气用炭-碳化硅多孔过滤器及其制备方法 Download PDF

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CN110818417B
CN110818417B CN201911124710.4A CN201911124710A CN110818417B CN 110818417 B CN110818417 B CN 110818417B CN 201911124710 A CN201911124710 A CN 201911124710A CN 110818417 B CN110818417 B CN 110818417B
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梁雄
李亚伟
万方豪
桑绍柏
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Wuhan University of Science and Engineering WUSE
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Abstract

一种净化空气用炭‑碳化硅多孔过滤器及其制备方法。其技术方案是：以60～70wt％的椰壳炭粉、10～15wt％的活性炭粉、10～25wt％的单质硅和5～8wt％的硅微粉为原料，混合，得混合料；向混合料中加入占原料1～5wt％的氯化铁粉、0.1～0.6wt％的羧甲基纤维素和20～35wt％的水，搅拌，即得浆料。将聚氨酯海绵浸入浆料中，取出后用对辊挤压成型或甩浆成型，干燥，烘干，置于气氛烧结炉内，在埋炭气氛或惰性气氛中：以三种速率依次升温至200～220℃、600～650℃和1000～1200℃，随炉冷却，制得净化空气用炭‑碳化硅多孔过滤器。本发明工艺简单，制备的净化空气用炭‑碳化硅多孔过滤器不仅空气阻力小和PM2.5过滤效率高，且对甲醛和VOC气体去除率高。

Description

一种净化空气用炭-碳化硅多孔过滤器及其制备方法
技术领域
本发明属于多孔过滤器技术领域。尤其涉及一种净化空气用炭-碳化硅多孔过滤器及其制备方法。
背景技术
随着装修业的发展，室内空气污染成为各国广泛关注的环境问题之一。甲醛和苯系可挥发性有机物等作为常见的家装气体污染物，具有基因毒性和致癌性，严重危害人体健康。此外，室内空气中的微小颗粒物也严重威胁着身体健康，如空气中微细颗粒(PM2.5)会严重破坏人体呼吸系统和心血管系统。因此，为营造舒适健康的生活环境，必须对室内甲醛、苯系可挥发性有机物去除的同时，还需对室内PM2.5进行净化，为人体健康提供环境保障。
为解决室内甲醛等有机挥发物和PM2.5超标问题，技术人员进行了深入的研究和技术开发：
如“一种含有壳聚糖的甲醛吸附剂”(CN101327424B)的专利技术，公开了一种将壳聚糖、二氧化锰和活性炭均匀混合，制得粉末状甲醛吸附剂，或采用挤压成型工艺并涂覆二氧化锰，制得颗粒状甲醛吸附剂。所制备的甲醛吸附剂因含二氧化锰虽能有效分解甲醛等有机气体，但粉体状和颗粒状的含有壳聚糖的甲醛吸附剂通常放于布袋或纸袋中，这种呈堆积状的粉末和颗粒甲醛吸附剂的自身比表面积小，导致甲醛等有机挥发物未能充分与甲醛吸附剂接触。因而，所制得的含有壳聚糖的甲醛吸附剂仅表面能对甲醛等有机气体进行吸附-分解，其内部还存在大量甲醛吸附剂未发挥作用，故这种含有壳聚糖的甲醛吸附剂的除甲醛等有机气体的效率不高。
又如“一种陶瓷空气净化器滤芯及其空气净化器”(CN207307410U)的专利技术，公开了一种将不同粒径的炭晶颗粒组成炭晶过滤层，然后外部分别安装炭晶陶瓷颗粒层和纱布层，对空气中的甲醛和粉尘进行净化。该技术所制备的空气净化器滤芯虽同时具备甲醛和粉尘的过滤功能，但是存在过滤效率不高的问题。该滤芯仅采用炭晶颗粒对甲醛气体进行吸附，未对甲醛气体进行分解；当炭晶颗粒中甲醛浓度高于室内空气中甲醛浓度时，炭晶颗粒中的甲醛将会向空气中释放，导致室内空气的二次甲醛污染。此外，该技术采用多层纱布只对空气中的毫米级、微米级别的粉尘进行截留，无法过滤亚微米和纳米级别的微细颗粒，导致该滤芯的过滤粉尘的效果差。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种工艺简单的净化空气用炭-碳化硅多孔过滤器的制备方法，用该方法制备的净化空气用炭-碳化硅多孔过滤器不仅空气阻力小和PM2.5过滤效率高，且对甲醛和VOC气体的去除率高。
为实现上述目的，本发明采用的技术方案的步骤是：
步骤一、以60～70wt％的椰壳炭粉、10～15wt％的活性炭粉、10～25wt％的单质硅和5～8wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料1～5wt％的氯化铁粉、0.1～0.6wt％的羧甲基纤维素和20～35wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，用对辊挤压成型或甩浆成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在埋炭气氛或惰性气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1000～1200℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述椰壳炭的平均粒度≤20μm。
所述活性炭的制备方法是，在600～800℃和惰性气氛条件下，将微晶石墨经微波处理1～5分钟，即得活性炭；所述活性炭的平均粒径≤5μm。
所述单质硅的平均粒度≤15μm；单质硅的Si含量≥98wt％。
所述硅微粉的平均粒度≤0.5μm；硅微粉的SiO2含量≥97wt％。
所述聚氨酯海绵的孔径为40ppi～100ppi，聚氨酯海绵的开孔率≥98％。
由于采用上述技术方案，本发明与现有技术相比，具有如下积极效果：
本发明将椰壳炭粉、活性炭、硅微粉、单质硅、氯化铁、羧甲基纤维素和水混合，制得浆料；将聚氨酯海绵浸渍于浆料中，对辊挤压或甩浆成型，室温干燥和烘干，制得炭-碳化硅多孔过滤器坯体。最后于埋炭或惰性气氛下，以三种速率依次升温至200～220℃、600～650℃和1000～1200℃，经1000～1200℃热处理2～4h，制得净化空气用炭-碳化硅多孔过滤器，制备工艺简单，适用于批量生产。
本发明制备的净化空气用炭-碳化硅多孔过滤器空气阻力小、PM2.5过滤效率高、甲醛和VOC气体的去除率高。其理由是：
一方面，本发明采用椰壳炭为主要原料，通过将聚氨酯海绵浸入浆料中，对辊挤压成型或甩浆成型、烘干和高温热处理，制备具有三维网状结构的净化空气用炭-碳化硅多孔过滤器，能显著降低过滤器的空气阻力，并且还能对毫米级、微米级颗粒进行高效截留。
另一方面，本发明以椰壳炭为主要原料，制备净化空气用炭-碳化硅多孔过滤器能有效对空气中甲醛等有机挥发物进行吸附，同时引入的过滤器内的氯化铁具备强氧化性，能及时对吸附的甲醛和VOC等有毒气体进行分解，促进室内空气中甲醛等有害气体的完全去除，逐步实现空气中甲醛等有害气体的完全净化。
再者，在对炭-碳化硅多孔过滤器坯体埋碳或惰性气氛处理的过程中，以活性炭粉为碳源，以硅微粉和单质硅为硅源，利用体系内硅源形成的Si(g)、SiO(g)以及碳源产生的活性炭、CO(g)基于固-气和气-气反应机理原位形成SiC晶须，在三维孔洞内编织成晶须网络；同时，材料中引入的氯化铁能作为催化剂促进SiC晶须的大量形成，有利于净化空气用炭-碳化硅多孔过滤器内晶须网络的构筑。由于SiC晶须具备高的比表面积能高效地对空气中微、纳级颗粒进行捕捉，显著提高层级过滤精度，原位形成的SiC晶须陶瓷相还能实现净化空气用炭-碳化硅多孔过滤器的增强、增韧，运行安全可靠。
本发明制备的净化空气用炭-碳化硅多孔过滤器经检测：常温抗折强度为3.8～6.9MPa；透气度为300～368m3·cm/m2·h·mmH2O；过滤效率为99.9％～99.99％@0.1μm；甲醛和VOC气体的吸附量为165～183mg/g。
因此，本发明工艺简单，制备的净化空气用炭-碳化硅多孔过滤器不仅空气阻力小和PM2.5过滤效率高，且对甲醛和VOC气体的去除率高。
附图说明
图1是本发明制备的一种净化空气用炭-碳化硅多孔过滤器的显微结构图。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制。
为避免重复，先将本具体实施方式所涉及原料的技术参数统一描述如下：
所述椰壳炭的平均粒度≤20μm。
所述活性炭的制备方法是，在600～800℃和惰性气氛条件下，将微晶石墨经微波处理1～5分钟，即得活性炭；所述活性炭的平均粒径≤5μm。
所述单质硅的平均粒度≤15μm；单质硅的Si含量≥98wt％。
所述硅微粉的平均粒度≤0.5μm；硅微粉的SiO2含量≥97wt％。
所述聚氨酯海绵的开孔率≥98％。
实施例1
一种净化空气用炭-碳化硅多孔过滤器及其制备方法。所述制备方法的步骤是：
步骤一、以60～65wt％的椰壳炭粉、12～15wt％的活性炭粉、10～18wt％的单质硅和6～8wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料3～5wt％的氯化铁粉、0.3～0.6wt％的羧甲基纤维素和30～35wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，用对辊挤压成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在埋炭气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1000～1100℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述聚氨酯海绵的孔径为40～60ppi。
本实施例制备的净化空气用炭-碳化硅多孔过滤器，经检测：常温抗折强度为3.8～4.2MPa；透气度为350～368m3·cm/m2·h·mmH2O；过滤效率为99.9％～99.92％@0.1μm；甲醛和VOC气体吸附量为165～172mg/g。
实施例2
一种净化空气用炭-碳化硅多孔过滤器及其制备方法。所述制备方法的步骤是：
步骤一、以65～70wt％的椰壳炭粉、10～13wt％的活性炭粉、17～25wt％的单质硅和5～7wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料1～3wt％的氯化铁粉、0.1～0.3wt％的羧甲基纤维素和20～25wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，用对辊挤压成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在埋炭气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1100～1200℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述聚氨酯海绵的孔径为50～70ppi。
本实施例制备的净化空气用炭-碳化硅多孔过滤器，经检测：常温抗折强度为4.0～5.2MPa；透气度为341～360m3·cm/m2·h·mmH2O；过滤效率为99.9％～99.92％@0.1μm；甲醛和VOC气体吸附量为165～173mg/g。
实施例3
一种净化空气用炭-碳化硅多孔过滤器及其制备方法。所述制备方法的步骤是：
步骤一、以65～70wt％的椰壳炭粉、10～13wt％的活性炭粉、17～25wt％的单质硅和6～8wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料1～3wt％的氯化铁粉、0.3～0.6wt％的羧甲基纤维素和23～27wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，甩浆成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在埋炭气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1080～1150℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述聚氨酯海绵的孔径为80～100ppi。
本实施例制备的净化空气用炭-碳化硅多孔过滤器，经检测：常温抗折强度为5.2～6.0MPa；透气度为300～321m3·cm/m2·h·mmH2O；过滤效率为99.92％～99.98％@0.1μm；甲醛和VOC气体吸附量为170～183mg/g。
实施例4
一种净化空气用炭-碳化硅多孔过滤器及其制备方法。所述制备方法的步骤是：
步骤一、以65～70wt％的椰壳炭粉、10～13wt％的活性炭粉、17～25wt％的单质硅和5～7wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料3～5wt％的氯化铁粉、0.2～0.4wt％的羧甲基纤维素和24～28wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，甩浆成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在惰性气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1050～1130℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述聚氨酯海绵的孔径为60～80ppi。
本实施例制备的净化空气用炭-碳化硅多孔过滤器，经检测：常温抗折强度为4.8～5.4MPa；透气度为320～331m3·cm/m2·h·mmH2O；过滤效率为99.92％～99.96％@0.1μm；甲醛和VOC气体吸附量为168～179mg/g。
实施例5
一种净化空气用炭-碳化硅多孔过滤器及其制备方法。所述制备方法的步骤是：
步骤一、以60～65wt％的椰壳炭粉、12～15wt％的活性炭粉、10～18wt％的单质硅和6～8wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料3～5wt％的氯化铁粉、0.3～0.5wt％的羧甲基纤维素和25～30wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，用对辊挤压成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在惰性气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1050～1130℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述聚氨酯海绵的孔径为70～90ppi。
本实施例制备的净化空气用炭-碳化硅多孔过滤器，经检测：常温抗折强度为4.9～5.3MPa；透气度为328～356m3·cm/m2·h·mmH2O；过滤效率为99.91％～99.95％@0.1μm；甲醛和VOC气体吸附量为170～175mg/g。
实施例6
一种净化空气用炭-碳化硅多孔过滤器及其制备方法。所述制备方法的步骤是：
步骤一、以65～70wt％的椰壳炭粉、10～13wt％的活性炭粉、17～25wt％的单质硅和5～7wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料2～4wt％的氯化铁粉、0.3～0.6wt％的羧甲基纤维素和27～33wt％的水，搅拌45～60min，即得浆料。
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，用对辊挤压成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体。
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在惰性气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1150～1200℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
所述聚氨酯海绵的孔径为60～80ppi。
本实施例制备的净化空气用炭-碳化硅多孔过滤器，经检测：常温抗折强度为3.9～4.9MPa；透气度为320～341m3·cm/m2·h·mmH2O；过滤效率为99.9％～99.97％@0.1μm；甲醛和VOC气体吸附量为172～180mg/g。
本具体实施方式与现有技术相比，具有如下积极效果：
本具体实施方式将椰壳炭粉、活性炭、硅微粉、单质硅、氯化铁、羧甲基纤维素和水混合，制得浆料；将聚氨酯海绵浸渍于浆料中，对辊挤压或甩浆成型，室温干燥和烘干，制得炭-碳化硅多孔过滤器坯体。最后于埋炭或惰性气氛下，以三种速率依次升温至200～220℃、600～650℃和1000～1200℃，经1000～1200℃热处理2～4h，制得净化空气用炭-碳化硅多孔过滤器，制备工艺简单，适用于批量生产。
本具体实施方式制备的净化空气用炭-碳化硅多孔过滤器空气阻力小、PM2.5过滤效率高、甲醛和VOC气体的去除率高。其理由是：
一方面，本具体实施方式采用椰壳炭为主要原料，通过将聚氨酯海绵浸入浆料中，对辊挤压成型或甩浆成型、烘干和高温热处理，制备具有三维网状结构的净化空气用炭-碳化硅多孔过滤器，能显著降低过滤器的空气阻力，并且还能对毫米级、微米级颗粒进行高效截留。
另一方面，本具体实施方式以椰壳炭为主要原料，制备净化空气用炭-碳化硅多孔过滤器能有效对空气中甲醛等有机挥发物进行吸附，同时引入的过滤器内的氯化铁具备强氧化性，能及时对吸附的甲醛和VOC等有毒气体进行分解，促进室内空气中甲醛等有害气体的完全去除，逐步实现空气中甲醛等有害气体的完全净化。
再者，在对炭-碳化硅多孔过滤器坯体埋碳或惰性气氛处理的过程中，以活性炭粉为碳源，以硅微粉和单质硅为硅源，利用体系内硅源形成的Si(g)、SiO(g)以及碳源产生的活性炭、CO(g)，基于固-气和气-气反应机理原位形成SiC晶须，在三维孔洞内编织成如图1所示的晶须网络，图1是实施例4制备的净化空气用炭-碳化硅多孔过滤器的显微结构图，从图1可以看出，SiC晶须相互交织，在微纳孔内呈晶须编织状，形成具有三维网状结构的SiC晶须网络；同时，材料中引入的氯化铁能作为催化剂促进SiC晶须的大量形成，有利于净化空气用炭-碳化硅多孔过滤器内晶须网络的构筑。由于SiC晶须具备高的比表面积能高效地对空气中微、纳级颗粒进行捕捉，显著提高层级过滤精度，原位形成的SiC晶须陶瓷相还能实现净化空气用炭-碳化硅多孔过滤器的增强、增韧，运行安全可靠。
本具体实施方式制备的净化空气用炭-碳化硅多孔过滤器经检测：透气度为常温抗折强度为3.8～6.9MPa；300～368m3·cm/m2·h·mmH2O；过滤效率为99.9％～99.99％@0.1μm；甲醛和VOC气体的吸附量为165～183mg/g。
因此，本具体实施方式工艺简单，制备的净化空气用炭-碳化硅多孔过滤器不仅空气阻力小和PM2.5过滤效率高，且对甲醛和VOC气体的去除率高。

Claims (7)

1.一种净化空气用炭-碳化硅多孔过滤器的制备方法，其特征在于所述制备方法的步骤是：
步骤一、以60～70wt％的椰壳炭粉、10～15wt％的活性炭粉、10～25wt％的单质硅和5～8wt％的硅微粉为原料，混合均匀，即得混合料；再向所述混合料中加入占所述原料1～5wt％的氯化铁粉、0.1～0.6wt％的羧甲基纤维素和20～35wt％的水，搅拌45～60min，即得浆料；
步骤二、将聚氨酯海绵浸入所述浆料中，浸渍5～10min，用对辊挤压成型或甩浆成型，室温干燥，90～110℃条件下烘干24～48h，即得炭-碳化硅多孔过滤器坯体；
步骤三、将所述炭-碳化硅多孔过滤器坯体置于气氛烧结炉内，在埋炭气氛或惰性气氛中：先以0.5～2℃/min的速率升温至200～220℃，再以1～1.5℃/min的速率升温至600～650℃，然后以2～3℃/min的速率升温至1000～1200℃，保温2～4h，最后随炉冷却至室温，制得净化空气用炭-碳化硅多孔过滤器。
2.如权利要求1所述的净化空气用炭-碳化硅多孔过滤器的制备方法，其特征在于所述椰壳炭的平均粒度≤20μm。
3.如权利要求1所述的净化空气用炭-碳化硅多孔过滤器的制备方法，其特征在于所述活性炭的制备方法是，在600～800℃和惰性气氛条件下，将微晶石墨经微波处理1～5分钟，即得活性炭；所述活性炭的平均粒径≤5μm。
4.如权利要求1所述的净化空气用炭-碳化硅多孔过滤器的制备方法，其特征在于所述单质硅的平均粒度≤15μm；单质硅的Si含量≥98wt％。
5.如权利要求1所述的净化空气用炭-碳化硅多孔过滤器的制备方法，其特征在于所述硅微粉的平均粒度≤0.5μm；硅微粉的SiO2含量≥97wt％。
6.如权利要求1所述的净化空气用炭-碳化硅多孔过滤器的制备方法，其特征在于所述聚氨酯海绵的孔径为40ppi～100ppi，聚氨酯海绵的开孔率≥98％。
7.一种净化空气用炭-碳化硅多孔过滤器，其特征在于所述净化空气用炭-碳化硅多孔过滤器是根据权利要求1～6项中任一项所述净化空气用炭-碳化硅多孔过滤器的制备方法所制备的净化空气用炭-碳化硅多孔过滤器。
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