CN107349879B - 原位合成蜂窝状c-a-s-h凝胶膜复合多孔集料的方法 - Google Patents

原位合成蜂窝状c-a-s-h凝胶膜复合多孔集料的方法 Download PDF

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CN107349879B
CN107349879B CN201710539135.9A CN201710539135A CN107349879B CN 107349879 B CN107349879 B CN 107349879B CN 201710539135 A CN201710539135 A CN 201710539135A CN 107349879 B CN107349879 B CN 107349879B
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胡曙光
赵都
王发洲
聂帅
刘鹏
高衣宁
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Abstract

本发明公开了一种原位合成蜂窝状C‑A‑S‑H凝胶膜复合多孔集料的方法。还公开了应用于负载纳米Ag/AgBr可见光催化剂。包括以下步骤：配置过饱和Ca(OH)2悬浊液，再加入NaOH调节溶液的碱性至pH为13～14；加入洗涤烘干后的多孔集料，超声处理，使过饱和Ca(OH)2悬浊液分布均匀并进入集料的孔隙中；在80～120℃加热处理6～12h；过滤分离，洗涤除去表面附着的Ca(OH)2；烘干制得蜂窝状C‑A‑S‑H凝胶膜复合多孔集料。本发明大大增加了多孔集料的比表面积，优化了孔结构，能够大大提高纳米功能性吸附剂或催化剂的负载量。同时，C‑A‑S‑H凝胶本身的链状结构也有固化重金属、与功能性纳米粒子成键的作用。

Description

原位合成蜂窝状C-A-S-H凝胶膜复合多孔集料的方法
技术领域
本发明属于功能陶瓷材料技术领域，具体涉及一种原位合成蜂窝状C-A-S-H凝胶膜复合多孔集料的方法。
背景技术
一些多孔负载材料(如陶粒、粉煤灰、活性炭、沸石、MnO2、γ-Al2O3等)因比表面积大、吸附能力强、疏松多孔、热稳定性好等特性可以用于纳米催化剂、吸附剂的稳定化和负载。其中，多孔陶砂、陶粒等煅烧页岩、粘土类集料具有价格低廉、来源广泛、耐高温、耐腐蚀等特点的同时，集料本身也具有相当的吸附性能，能够对空气中的污染物、污染水中的重金属等进行吸附。由于主要原料天然页岩或陶土，与微生物也具有相当的亲和性，易于微生物的吸附生长。目前，多孔集料已被广泛应用于空气污染处理、水污染处理等领域。
目前多孔集料在污染领域的应用方法有直接应用和催化剂、吸附剂负载两种方式。直接应用主要是直接充当水污染处理过程中的填料。另外，多孔集料作为载体负载催化剂、吸附剂现在也得到了广泛的研究，主要负载方式有直接负载、碱激发法、真空超声、化学键合等。但相对于其它多孔负载材料，多孔集料的比表面积较小、孔径偏大，对于纳米尺度来说表面比较平滑，使其对于纳米功能性颗粒的负载量大大降低。因此，集料的表面改性和活化对于它作为载体应用过程中尤为关键。
发明内容
本发明目的在于旨在针对多孔集料作为纳米吸附剂催化剂载体比表面积较小、孔径较大、表面平滑等缺陷，制备出一种制备过程简便，对纳米功能性颗粒负载方式简单、负载量大的原位合成蜂窝状C-A-S-H凝胶膜复合多孔集料载体材料。
为达到上述目的，采用技术方案如下：
原位合成蜂窝状C-A-S-H凝胶膜复合多孔集料的方法，包括以下步骤：
1)配置过饱和Ca(OH)2悬浊液，再加入NaOH调节溶液的碱性至pH为13～14；
2)加入超声洗涤并烘干后的多孔集料，超声处理，使过饱和Ca(OH)2悬浊液分布均匀并进入集料的孔隙中；
3)在80～120℃加热处理6～12h；
4)过滤分离，洗涤除去表面附着的Ca(OH)2；烘干制得蜂窝状C-A-S-H凝胶膜复合多孔集料。
按上述方案，过饱和Ca(OH)2悬浊液Ca(OH)2的投加量为0.5～1g/100mL水。
按上述方案，多孔集料加入量为3～8g/100mL。
按上述方案，所述多孔集料为陶粒、陶砂或多孔陶瓷的任意一种或者任意混合。
按上述方案，所述陶粒为页岩陶粒、黏土陶粒、粉煤灰陶粒、垃圾陶粒、煤矸石陶粒、生物污泥陶粒或河底泥陶粒。
按上述方案，所述陶砂为页岩陶砂、黏土陶砂、粉煤灰陶砂、垃圾陶砂、煤矸石陶砂、生物污泥陶砂或河底泥陶砂。
一种蜂窝状C-A-S-H凝胶膜复合多孔集料，按上述方法制备而来。
所述蜂窝状C-A-S-H凝胶膜复合多孔集料应用于功能性载体负载催化剂和吸附剂或直接应用于水污染处理和空气污染处理。
本发明所得蜂窝状C-A-S-H凝胶膜复合多孔集料大大增加了多孔集料的比表面积，优化了集料的孔结构，能够大大提高纳米功能性吸附剂或催化剂的负载量。同时，由于C-A-S-H的结构特性，重金属颗粒可以替代Si进入C-A-S-H的链状结构中，结构中的SiO2也可以与纳米催化剂和吸附剂颗粒成键，具有广泛的应用前景。
本发明有益效果如下：
(1)制备方法简便高效，能够一步合成材料，制备周期短，成本低，效果好；
(2)制备过程中通过控制条件如：加热温度、时间、PH值、Ca(OH)2量、集料投加量等，有效控制了C-A-S-H凝胶的生长，使其生长至蜂窝状结构阶段；
(3)通过负载这层蜂窝状C-A-S-H凝胶，提高了集料的比表面积达50倍，优化了集料的孔结构，大大增加了集料作为功能材料载体的负载量；
(4)C-A-S-H凝胶本身的链状结构也有固化重金属、与功能性纳米粒子成键的作用。
附图说明
图1：普通陶砂表面的扫描电子显微镜图；
图2、3：实施例1所得蜂窝状C-A-S-H凝胶膜复合多孔集料的扫描电子显微镜图；
图4：实施例2所得蜂窝状C-A-S-H凝胶膜复合多孔集料的扫描电子显微镜图；
图5、6：实施例3普通陶砂负载Ag/AgBr可见光催化剂的扫描电子显微镜图；
图7、8：实施例3蜂窝状C-A-S-H凝胶膜复合多孔集料负载Ag/AgBr可见光催化剂的扫描电子显微镜图；
图9：普通陶砂与蜂窝状C-A-S-H凝胶膜复合多孔集料负载光催化剂催化效果对比图。
具体实施方式
以下实施例进一步阐释本发明的技术方案，但不作为对本发明保护范围的限制。
实施例1
原位合成蜂窝状C-A-S-H凝胶膜复合多孔陶砂的制备
(1)陶砂预处理：将900级页岩陶砂超声洗涤3次，每次30min，105℃下烘干，备用；
(2)配置反应溶液：称取0.5g Ca(OH)2置入100ml去离子水中，再称取NaOH调节其碱度，使NaOH浓度为0.5mol/L，超声30min，使其均匀分散。
(3)原位合成蜂窝状结构C-A-S-H凝胶膜复合多孔陶砂功能性载体材料的制备：陶砂洗涤完成后，将5g陶砂置于100ml所配置的溶液中。超声30min，使过饱和析出的Ca(OH)2悬浊液分布均匀并进入集料的孔隙中。密封，置于90℃烘箱中，加热8h。取出，将加热后的陶砂超声洗涤3次每次30min，将表面附着的Ca(OH)2洗去，在105℃下烘干，制得原位合成蜂窝状结构C-A-S-H凝胶膜复合多孔陶砂功能材料。
所用页岩陶砂表面的扫描电子显微镜图如图1所示。图2和图3是本实施例制备的原位合成蜂窝状C-A-S-H凝胶膜复合多孔陶砂的扫描电镜图片，材料中的蜂窝状结构为C-A-S-H凝胶。与图1中普通陶砂的形貌相比，可以看出这种原位合成蜂窝状凝胶膜已经均匀覆盖在了陶砂的整个表面。
普通多孔陶砂与本实施例所得C-A-S-H凝胶膜复合多孔陶砂氮吸附比表面积分析结果见表1所示。
表1
Figure BDA0001341420080000031
本实施例所得原位合成蜂窝状C-A-S-H凝胶膜复合多孔陶砂具有蜂窝状结构，比表面积相较于普通多孔陶砂增加50倍左右。
实施例2
原位合成蜂窝状C-A-S-H凝胶膜复合多孔陶粒的制备
(1)陶粒预处理：将700级页岩陶粒超声洗涤3次，每次30min，105℃下烘干，备用；
(2)配置反应溶液：称取2.5g Ca(OH)2置入500ml去离子水中，再称取NaOH调节其碱度，使NaOH浓度为0.5mol/L，超声30min，使其均匀分散。
(3)原位合成蜂窝状结构C-A-S-H凝胶膜复合多孔陶粒功能性载体材料的制备：陶粒洗涤完成后，将50g陶粒置于500ml所配置的溶液中。超声30min，使过饱和析出的Ca(OH)2悬浊液分布均匀并进入集料的孔隙中。密封，置于90℃烘箱中，加热8h。取出，将加热后的陶粒超声洗涤3次每次30min，将表面附着的Ca(OH)2洗去，在105℃下烘干，制得原位合成蜂窝状结构C-A-S-H凝胶膜复合多孔陶粒功能性载体材料。
图4是本实施例原位合成蜂窝状结构C-A-S-H凝胶膜复合多孔陶粒功能性载体材料的扫描电镜图片，材料中的蜂窝状结构为C-A-S-H凝胶，可以看出这种原位合成蜂窝状凝胶膜已经均匀覆盖在了陶粒的整个表面。
实施例3
原位合成蜂窝状C-A-S-H凝胶膜复合多孔陶砂负载可见光催化剂Ag/AgBr的制备及其与普通陶砂负载可见光催化剂的对比：
(1)C-A-S-H凝胶膜复合多孔陶砂载体的制备同实施例1中所述。
(2)纳米AgBr的制备：调制50mL 0.015M的CTAB溶液，磁力搅拌30min，待用；调制50mL0.015M的AgNO3溶液在磁力搅拌下慢滴1～2h加入配好的CTAB溶液中，在8000转转速下离心洗涤3次，每次5min，将上清液移除，得到纳米AgBr。
(3)将一次所得到的纳米AgBr加入60ml去离子水中，得到纳米AgBr悬浊液，将3g普通多孔陶砂与3g原位合成蜂窝状结构C-A-S-H凝胶膜复合多孔陶砂分别加入两个培养皿中，分别向两个培养皿中加入30mlAgBr悬浊液；将培养皿放入通风橱中，静置晾干。
(4)将得到的负载有AgBr的普通陶砂和凝胶陶砂置于紫外光下还原30min，即得到Ag/AgBr/C-A-S-H复合光催化陶砂。
从图5、6、7、8可以看出，Ag/AgBr/C-A-S-H复合光催化陶砂的负载量远大于普通陶砂，且没有团聚现象，纳米Ag/AgBr颗粒很好的镶嵌在了C-A-S-H的蜂窝状结构中。从图9可以看出，Ag/AgBr/C-A-S-H复合光催化陶砂的效果比普通陶砂提高了40％。

Claims (4)

1.原位合成蜂窝状C-A-S-H凝胶膜复合多孔集料的方法，其特征在于包括以下步骤：
1)配置过饱和Ca(OH)2悬浊液，再加入NaOH调节溶液的碱性至pH为13～14；过饱和Ca(OH)2悬浊液Ca(OH)2的投加量为0.5～1g/100mL水；
2)加入多孔集料，超声处理，使过饱和Ca(OH)2悬浊液分布均匀并进入集料的孔隙中；多孔集料加入量为3～8g/100mL；
3)在80～120℃加热处理6～12h；
4)过滤分离，洗涤除去表面附着的Ca(OH)2；烘干制得蜂窝状C-A-S-H凝胶膜复合多孔集料。
2.如权利要求1所述原位合成蜂窝状C-A-S-H凝胶膜复合多孔集料的方法，其特征在于所述多孔集料为陶粒、陶砂或多孔陶瓷的任意一种或者任意混合。
3.一种蜂窝状C-A-S-H凝胶膜复合多孔集料，采用权利要求1所述方法制备而来。
4.权利要求3所述蜂窝状C-A-S-H凝胶膜复合多孔集料应用于功能性载体负载催化剂和吸附剂或者直接应用于水污染处理和空气污染处理。
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