CN105903272B - 一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯 - Google Patents

一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯 Download PDF

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CN105903272B
CN105903272B CN201610299967.3A CN201610299967A CN105903272B CN 105903272 B CN105903272 B CN 105903272B CN 201610299967 A CN201610299967 A CN 201610299967A CN 105903272 B CN105903272 B CN 105903272B
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carbon crystal
layer
diamond alkene
nanometer carbon
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CN105903272A (zh
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张洪涛
何本锋
王俊芝
薛胜辉
刘君丽
武艳强
杨晋中
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Henan Sino Crystal Micro Diamond Co ltd
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Abstract

本发明公开了一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，属于水处理设备领域，该陶瓷过滤芯从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层。本发明还公开了该陶瓷过滤芯的制备方法。本发明中，由于纳米钻石烯和纳米碳晶的高表面活性可以进行特定官能团或者粒子的吸附处理，加入硝酸银之后，银离子在混合处理过程中能被纳米钻石烯和纳米碳晶的表面吸附，在后期杀菌过程中可以持续作用而不会被水分子溶解带离陶瓷滤芯，从而达到了长久除菌的效果。

Description

一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯
技术领域
本发明属于水处理设备领域，具体涉及一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯。
背景技术
生活用水中污染物主要包括颗粒物质、微生物、有机溶解物以及重金属离子。自来水在处理过程中虽然可以将上述大量污染物去除，但是仍旧会残留部分有机物质，这些有机物质与游离氯结合形成致癌的诸如三氯甲烷等有机氯物质。此外，城市中的二次供水以及管网老化等原因，会导致自来水的二次污染，仍旧会带入上述污染物，从而影响了饮用水的品质，因此需要在个人家庭中加装饮用水净化器来提高水的引用品质确保人体健康。
陶瓷膜(ceramic membrane)又称无机陶瓷膜，是以无机陶瓷材料经特殊工艺制备而形成的非对称膜。陶瓷膜管壁密布微孔，在压力作用下，原料液在膜管内或膜外侧流动，小分子物质（或液体）透过膜，大分子物质（或固体）被膜截留，从而达到分离、浓缩、纯化和环保等目的。相较于传统聚合物分离膜材料，陶瓷膜具有化学稳定性好，能耐酸、耐碱、耐有机溶剂；机械强度大，可反向冲洗；抗微生物能力强；耐高温；孔径分布窄、分离效率高等优点，在食品工业、生物工程、环境工程、化学工业、石油化工、冶金工业等领域得到了广泛的应用，其市场销售额以30%的年增长率发展着。用于分离的陶瓷膜的结构通常为三明治式的：支撑层（又称载体层）、过渡层（又称中间层）、膜层（又称分离层）。其中支撑层的孔径一般为1~20μm，孔隙率为30%~65%，其作用是增加膜的机械强度；中间层的孔径比支撑层的孔径小其作用是防止膜层制备过程中颗粒向多孔支撑层的渗透，孔隙率为30%~40%；膜层具有分离功能，孔径约1μm不等，厚度约为3~10μm，孔隙率为40%~60%。整个膜的孔径分布由支撑层到膜层逐渐减小，形成不对称的结构分布。陶瓷膜根据孔径可分为微滤（孔径大于50nm）、超滤（孔径2~50nm）、纳滤（孔径小于2nm）等种类。进行分离时，在外力的作用下，小分子物质透过膜，大分子物质被膜截留，从而达到分离、浓缩、纯化、去杂、除菌等目的。陶瓷膜的不足之处在于造价较高、无机材料脆性大、弹性小、给膜的成型加工及组件装备带来一定的困难等。
发明内容
本发明的目的在于提供一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯。
基于上述目的，本发明采用以下技术方案：一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层。
进一步地，所述支撑层由硅藻土、碳化硅、纳米碳晶和水按照质量比1︰（0.8~1）︰（0.1~0.3）︰（0.5~0.9）制备而成。
进一步地，所述硅藻土由纳米级硅藻土和微米级硅藻土按质量比1︰（8~9）混合而成，硅藻土是构建陶瓷滤芯的基体材料，主要作用是支撑，同时兼有过滤的功能。分别选用微米级和纳米级硅藻土，可以在支撑层中形成非对称的渐进式孔隙，从支撑层表面向第二过滤层的内孔隙逐渐变小，提高支撑层的过滤精度。
进一步地，所述过滤层由纳米级硅藻土、碳化硅、纳米碳晶和水按照质量比1︰（0.5~0.8）︰（0.2~0.5）︰（0.6~1）制备而成。
进一步地，所述第一分离层由纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水按照质量比1︰1︰（0.05~0.08）︰（0.2~0. 5）︰（0.1~0.5）︰（0.6~1）制备而成。
进一步地，所述第二分离层由纳米碳晶、纳米钻石烯、纳米级硅藻土和水按照质量比1︰1︰（0.1~0.3）︰（0.5~0.7）制备而成。
进一步地，所述纳米级硅藻土的粒径为50~200nm，微米级硅藻土的的粒径为20~30μm。
进一步地，支撑层的厚度为10mm，孔隙率为30%~60%，孔径为1~20μm；过滤层的厚度为5mm，孔隙率为30%~50%，孔径为0.5~1μm；第一分离层的厚度为1mm，孔隙率为30%~40%，孔径为0.15~0.2μm；第二分离层的的厚度为30μm，孔隙率为40%~50%，孔径为0.1~0.15μm。
纳米钻石烯特殊的层状结构结合其高比表面积从而具有极佳的吸附性能；同时化学性质稳定，使其在加工过程中不会发生物质性质的变化。
上述含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯的制备方法，包括以下步骤：
（1）将硅藻土、碳化硅、纳米碳晶和水混合、搅拌0.5~3h制得泥料，泥料经熟化、成型后制得生坯，在100~120℃下烘干得到支撑层；
（2）将纳米级硅藻土、碳化硅、纳米碳晶和水混合、搅拌1~4h制得浆料，将熟化处理后是我浆料涂覆在步骤（1）所得的支撑层上，100~120℃烘干，在支撑层表面形成过滤层；
（3）将纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水混合、搅拌1~4h得浆料，将熟化后的浆料涂覆在过滤层表面，100~120℃烘干，在过滤层表面形成第一分离层；
（4）将纳米碳晶、纳米钻石烯、纳米级硅藻土和水混合、搅拌1~4h得浆料，将熟化后的浆料涂覆在第一分离层表面，100~120℃烘干，在第一分离层表面形成第二分离层，得到陶瓷过滤芯生坯；
（5）将陶瓷过滤芯生坯在氮气保护下，以3~7℃/min的升温速度加热到800~950℃，在800~950℃下烧结 2.5~3.5h，制得陶瓷过滤芯。
本发明提供的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯具有以下优点：
1、传统支撑层选用原料颗粒较粗，以过滤较粗颗粒杂质为主，主要起陶瓷滤芯的结构支撑作用，本发明在支撑层中加入纳米碳晶，从支撑层开始就能吸附过滤较细的颗粒；
2、因纳米碳晶具有颗粒细、硬度高、耐磨性好、极高的比表面积、吸附性能极好、稳定的物理化学性能等优点，掺杂在硅藻土中可以增加陶瓷芯的耐磨度以及耐热性能，能够替代传统材料碳化硅，降低碳化硅的用量，纳米碳晶和纳米钻石烯还提高了各层的韧性以及力学性能；
3、纳米钻石烯和纳米碳晶的粒径在纳米级别，将其作为过渡层和分离层的主要原料，可以提高过滤精度；同时纳米钻石烯和纳米碳晶的高比表面和高吸附性不仅可以有效吸附固体颗粒，还可以吸附各种分子和离子等杂质粒子；
4、纳米钻石烯和纳米碳晶的高表面活性可以进行特定官能团或者粒子的吸附处理，加入硝酸银之后，银离子在混合处理过程中能被纳米钻石烯和纳米碳晶的表面吸附，在后期杀菌过程中可以持续作用而不会被水分子溶解带离陶瓷滤芯，从而达到了长久除菌的效果。
附图说明
图1是含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯的结构示意图。
具体实施方式
下面结合实施例对本发明进行详细说明。
纳米碳晶的制备参考专利CN2015107503345，制备出的纳米碳晶为类球形形貌，C含量为99-100%，晶格间距为0.21nm；该纳米碳晶表面的C原子与内层金刚石相的C原子构成C原子的二聚体结构，C原子的二聚体结构中的两个碳原子为非对称分布；平均粒径为R，0＜R≤10nm。纳米碳晶具有颗粒细、硬度高、耐磨性好、极高的比表面积、吸附性能极好、稳定的物理化学性能等优点。
纳米钻石烯的制备参考专利CN2015107492073，制备出的纳米钻石烯为层片状单晶结构，同一片层的碳原子之间为sp3轨道杂化碳键连接，层与层之间的碳原子之间为sp2杂化碳键连接，C含量为99～100%，晶格间距为0.21nm；粒径为R，20≤R≤500nm。纳米钻石烯特殊的层状结构结合其高比表面积从而具有极佳的吸附性能；同时化学性质稳定，使其在加工过程中不会发生物质性质的变化。
实施例1
一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，采用以下方法制备，步骤为：
（1）将硅藻土（由纳米级硅藻土和微米级硅藻土按质量比1︰8混合而成）、碳化硅、纳米碳晶和水按照质量比1︰0.8︰0.1︰0.5混合、搅拌0.5h制得泥料，泥料经熟化、成型后制得生坯，在100℃下烘干得到支撑层；
（2）将纳米级硅藻土、碳化硅、纳米碳晶和水按照质量比1︰0.5︰0.2︰0.6混合、搅拌1h制得浆料，将熟化处理后是我浆料涂覆在步骤（1）所得的支撑层上，100℃烘干，在支撑层表面形成过滤层；
（3）将纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水按照质量比1︰1︰0.05︰0.2︰0.1︰0.6混合、搅拌1h得浆料，将熟化后的浆料涂覆在过滤层表面，100℃烘干，在过滤层表面形成第一分离层；
（4）将纳米碳晶、纳米钻石烯、纳米级硅藻土和水按照质量比1︰1︰0.1︰0.5混合、搅拌1h得浆料，将熟化后的浆料涂覆在第一分离层表面，100℃烘干，在第一分离层表面形成第二分离层，得到陶瓷过滤芯生坯；
（5）将陶瓷过滤芯生坯在氮气保护下，以3℃/min的升温速度加热到800℃，在800℃下烧结2.5h，制得陶瓷过滤芯。
所述纳米级硅藻土的粒径为50~200nm，微米级硅藻土的的粒径为20~30μm。硅藻土是构建陶瓷滤芯的基体材料，主要作用是支撑，同时兼有过滤的功能。分别选用微米级和纳米级硅藻土，可以在支撑层中形成非对称的渐进式孔隙，从支撑层表面向第二过滤层的内孔隙逐渐变小，提高支撑层的过滤精度。
采用上述方法制备的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层；支撑层的厚度为10mm，孔隙率为45%，孔径为20μm；过滤层的厚度为5mm，孔隙率为35%，孔径为1μm；第一分离层的厚度为1mm，孔隙率为30%，孔径为0.2μm；第二分离层的的厚度为30μm，孔隙率为43%，孔径为0.13μm。
实施例2
一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，采用以下方法制备，步骤为：
（1）将硅藻土（由纳米级硅藻土和微米级硅藻土按质量比1︰9混合而成）、碳化硅、纳米碳晶和水按照质量比1︰1︰0.3︰0.9混合、搅拌3h制得泥料，泥料经熟化、成型后制得生坯，在120℃下烘干得到支撑层；
（2）将纳米级硅藻土、碳化硅、纳米碳晶和水按照质量比1︰0.8︰0.5︰1混合、搅拌4h制得浆料，将熟化处理后是我浆料涂覆在步骤（1）所得的支撑层上 120℃烘干，在支撑层表面形成过滤层；
（3）将纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水按照质量比1︰1︰0.08︰0.5︰0.5︰1混合、搅拌4h得浆料，将熟化后的浆料涂覆在过滤层表面，120℃烘干，在过滤层表面形成第一分离层；
（4）将纳米碳晶、纳米钻石烯、纳米级硅藻土和水按照质量比1︰1︰0.3︰0.7混合、搅拌4h得浆料，将熟化后的浆料涂覆在第一分离层表面，120℃烘干，在第一分离层表面形成第二分离层，得到陶瓷过滤芯生坯；
（5）将陶瓷过滤芯生坯在氮气保护下，以7℃/min的升温速度加热到950℃，在950℃下烧结3.5h，制得陶瓷过滤芯。
所述纳米级硅藻土的粒径为50~200nm，微米级硅藻土的的粒径为20~30μm。
采用上述方法制备的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层；支撑层的厚度为10mm，孔隙率为50%，孔径为5μm；过滤层的厚度为5mm，孔隙率为45%，孔径为0.7μm；第一分离层的厚度为1mm，孔隙率为38%，孔径为0.15μm；第二分离层的的厚度为30μm，孔隙率为48%，孔径为0.1μm。
实施例3
一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，采用以下方法制备，步骤为：
（1）将硅藻土（由纳米级硅藻土和微米级硅藻土按质量比1︰9混合而成）、碳化硅、纳米碳晶和水按照质量比1︰0.9︰0.2︰0.7混合、搅拌2h制得泥料，泥料经熟化、成型后制得生坯，在110℃下烘干得到支撑层；
（2）将纳米级硅藻土、碳化硅、纳米碳晶和水按照质量比1︰0.7︰0.3︰0.8混合、搅拌3h制得浆料，将熟化处理后是我浆料涂覆在步骤（1）所得的支撑层上，110℃烘干，在支撑层表面形成过滤层；
（3）将纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水按照质量比1︰1︰0.06︰0.4︰0.3︰0.8混合、搅拌3h得浆料，将熟化后的浆料涂覆在过滤层表面，110℃烘干，在过滤层表面形成第一分离层；
（4）将纳米碳晶、纳米钻石烯、纳米级硅藻土和水按照质量比1︰1︰0.2︰0.6混合、搅拌3h得浆料，将熟化后的浆料涂覆在第一分离层表面，110℃烘干，在第一分离层表面形成第二分离层，得到陶瓷过滤芯生坯；
（5）将陶瓷过滤芯生坯在氮气保护下，以5℃/min的升温速度加热到900℃，在900℃下烧结3.0h，制得陶瓷过滤芯。
所述纳米级硅藻土的粒径为50~200nm，微米级硅藻土的的粒径为20~30μm。
采用上述方法制备的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层；支撑层的厚度为10mm，孔隙率为47%，孔径为10μm；过滤层的厚度为5mm，孔隙率为37%，孔径为0.9μm；第一分离层的厚度为1mm，孔隙率为36%，孔径为0.18μm；第二分离层的的厚度为30μm，孔隙率为45%，孔径为0.12μm。
实施例4
一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，采用以下方法制备，步骤为：
（1）将硅藻土（由纳米级硅藻土和微米级硅藻土按质量比1︰8混合而成）、碳化硅、纳米碳晶和水按照质量比1︰0.9︰0.3︰0.7混合、搅拌1h制得泥料，泥料经熟化、成型后制得生坯，在110℃下烘干得到支撑层；
（2）将纳米级硅藻土、碳化硅、纳米碳晶和水按照质量比1︰0.7︰0.4︰0.8混合、搅拌2h制得浆料，将熟化处理后是我浆料涂覆在步骤（1）所得的支撑层上，110℃烘干，在支撑层表面形成过滤层；
（3）将纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水按照质量比1︰1︰0.07︰0.4︰0.3︰0.9混合、搅拌2h得浆料，将熟化后的浆料涂覆在过滤层表面，110℃烘干，在过滤层表面形成第一分离层；
（4）将纳米碳晶、纳米钻石烯、纳米级硅藻土和水按照质量比1︰1︰0.2︰0.6混合、搅拌2h得浆料，将熟化后的浆料涂覆在第一分离层表面，110℃烘干，在第一分离层表面形成第二分离层，得到陶瓷过滤芯生坯；
（5）将陶瓷过滤芯生坯在氮气保护下，以6℃/min的升温速度加热到850℃，在850℃下烧结3.0h，制得陶瓷过滤芯。
所述纳米级硅藻土的粒径为50~200nm，微米级硅藻土的的粒径为20~30μm。
采用上述方法制备的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层；支撑层的厚度为10mm，孔隙率为46%，孔径为15μm；过滤层的厚度为5mm，孔隙率为38%，孔径为0.8μm；第一分离层的厚度为1mm，孔隙率为34%，孔径为0.16μm；第二分离层的的厚度为30μm，孔隙率为45%，孔径为0.12μm。
试验例1 性能测试实验
实验过程：选取试实施例1~4制备的试样，依次将试样表面以0.5μm金刚石研磨膏抛光，然后在HV-120型维氏硬度仪上，采用不同的载荷p在试样抛光面上压出压痕，保持时间为15秒。用XJL-02型立式金相显微镜观察压痕，准确测量出材料的大小压痕的对角线尺寸d1、 d2及裂纹尺寸l，并求得相应的压痕对角线平均值d=（d1+ d2）/2、切口深度a=d /2及裂纹半长c=a+l，将d带入相应的维氏硬度计算公式HV=0.1891F /d,求出维氏硬度值HV；同理，将不同的载荷p以及c带入断裂韧性计算公式K=0.0752p·c-1.5，求出断裂韧性值。具体结果见表1。
试验例2 抗菌实验
实验过程：因为自来水中含有细菌较少，为了达到预期的实验效果，先培养一定量的大肠杆菌、伤寒菌、金黄色葡萄球菌以及白色念珠菌。用金相显微镜挑选30个大肠杆菌、10个伤寒菌、80个金黄色葡萄球菌、20个白色念珠菌放到100mL无菌蒸馏水中，用加压微滤装置，经实施例1~4所制得的陶瓷过滤芯过滤，制得样品。把滤出样品装入已灭菌的瓶中，并对应标注样品号1、2、3、4，最后对滤出样品1、2、3、4进行检测，每组试验进行三次并记录处理前后细菌个数求得平均值，具体结果见表2。

Claims (9)

1.一种含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，所述陶瓷过滤芯从内到外依次设置有支撑层、过滤层、第一分离层和第二分离层；所述支撑层由硅藻土、碳化硅、纳米碳晶和水按照质量比1︰（0.8~1）︰（0.1~0.3）︰（0.5~0.9）制备而成。
2.根据权利要求1所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，支撑层采用的硅藻土由纳米级硅藻土和微米级硅藻土按质量比1︰（8~9）混合而成。
3.根据权利要求1所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，所述过滤层由纳米级硅藻土、碳化硅、纳米碳晶和水按照质量比1︰（0.5~0.8）︰（0.2~0.5）︰（0.6~1）制备而成。
4.根据权利要求1所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，所述第一分离层由纳米碳晶、纳米钻石烯、硝酸银、纳米级硅藻土、碳化硅和水按照质量比1︰1︰（0.05~0.08）︰（0.2~0. 5）︰（0.1~0.5）︰（0.6~1）制备而成。
5.根据权利要求1所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，所述第二分离层由纳米碳晶、纳米钻石烯、纳米级硅藻土和水按照质量比1︰1︰（0.1~0.3）︰（0.5~0.7）制备而成。
6.根据权利要求1-5任一所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，支撑层的厚度为10mm，孔隙率为30%~60%，孔径为1~20μm。
7.根据权利要求1-5任一所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，过滤层的厚度为5mm，孔隙率为30%~50%，孔径为0.5~1μm。
8.根据权利要求1-5任一所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，第一分离层的厚度为1mm，孔隙率为30~40%，孔径为0.15~0.2μm。
9.根据权利要求1-5任一所述的含有纳米碳晶和纳米钻石烯共混物的陶瓷过滤芯，其特征在于，第二分离层的的厚度为30μm，孔隙率为40%~50%，孔径为0.1~0.15μm。
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