CN110054499A - 一种表面负载分子筛的氮化硅微球、制备方法及其应用 - Google Patents
一种表面负载分子筛的氮化硅微球、制备方法及其应用 Download PDFInfo
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Abstract
一种表面负载分子筛的氮化硅微球、制备方法及其应用,涉及分子筛化学、陶瓷化工及过滤分离技术领域。将具有甲基的ZSM‑5分子筛喷涂在氮化硅陶瓷微球表面,经干燥,即得在氮化硅陶瓷微球表面负载具有甲基的ZSM‑5分子筛。本发明工艺简单,通过喷涂,将具有甲基的ZSM‑5分子筛分布于在基材——氮化硅陶瓷微球表面,再经80℃烘干即可固化,形成的固状微球材料方便进一步包装、运输。含甲基的分子筛的修饰使得氮化硅陶瓷微球具有较强疏水性,可有效吸附有机物质,同时对水与水溶性物质产生排斥。达到优异的水中大颗粒和有机物过滤、分离作用。
Description
技术领域
本发明涉及分子筛化学、陶瓷化工及过滤分离技术领域。
技术背景
氮化硅基陶瓷由氮化硅粉料及陶瓷烧结助剂烧结制成,是一种烧结时不收缩的无机材料陶瓷,具有高强度、低密度、耐高温、耐强酸等优良性质。通过热压铸成型的氮化硅陶瓷微球材料有以下优点:化学稳定性好,耐酸碱及有机溶剂;极好的耐急热急冷性能,工作温度可高达1000℃;抗菌性能好,不易被细菌降解,较强的结构稳定性,无毒,有较大表面积,尤其适用于食品和药物的处理。但是由于裸露的氮化硅陶瓷微球作为过滤材料时,只能单纯用于分离液体中的固体大颗粒,且会大量吸附液体中的成分,会造成液体有效组成的流失。
分子筛作为一种性能优异的多孔材料,具有表面积大、水热稳定、吸附能力强等优点,在其表面修饰上甲基后更可以在对有机物产生有效吸附的同时具有良好疏水性,对水溶性物质不进行吸附,将其应用在水溶液中的有机物分离中尤高效。但分散型的分子筛成型性差,在水溶液中需通过过滤等操作除去,不仅操作麻烦,且滤纸会对溶液组成造成影响。
现有的过滤器采用漏斗作为过滤载体,在漏斗中铺设滤纸,当待过滤的混合料自漏斗上端注入时,通过滤纸的过滤作用,使滤过液自漏斗下端的出口滤出,而被滤纸截留下的物质则留在滤纸上。滤纸的耐用性较差,为了防止滤纸堵塞而造成过滤效率低下,人们需要不停地更换滤纸。另外,滤纸也无法对含大颗粒物质的混合料进行过滤,更无法选择性过滤有机物。。
发明内容
针对以上缺陷,本发明第一目的在于提出一种成形好、耐用性强、可以对大颗粒和水中有机物同时进行分离的表面负载分子筛的氮化硅微球。
本发明的特征是:在氮化硅陶瓷微球表面负载具有甲基的ZSM-5分子筛。
本发明的有益效果是:有效过滤成分为表面负载有分子筛的氮化硅微球,所负载的分子筛表面带有大量疏水的甲基,可以有效过滤、分离水溶液中的有机物成分;同时,由于过滤部分氮化硅陶瓷微球表面的疏水性分子筛结构,可以做到完全不影响水溶液中水溶性组分;同时,氮化硅陶瓷材料与分子筛材料均无毒,表面积很大,耐高温,耐用性强,该过滤器可用于多种情况下,尤其适用于制药、食品等领域。
进一步地,本发明氮化硅陶瓷微球的直径为0.5±0.002cm。该直径为氮化硅微球合成工艺中较容易成型的一种,而且,若直径过大,则总体微球表面积减小,与滤液不能充分接触;若直径过小,则会大大降低液体通过速度,影响过滤效率。
本发明的第二目的在于提出上述表面负载分子筛的氮化硅微球的制备方法。
将具有甲基的ZSM-5分子筛喷涂在氮化硅陶瓷微球表面,经干燥,即成。
所述干燥的温度环境为80℃,该温度下分子筛浆料可快速、均匀挥发,有效附着于氮化硅微球表面。
本发明工艺简单,通过喷涂,将具有甲基的ZSM-5分子筛分布于在基材——氮化硅陶瓷微球表面,再经80℃烘干即可固化,形成的固状微球材料方便进一步包装、运输和应用。
进一步地,本发明中,基材——氮化硅陶瓷微球的具体制备方法是:将氮化硅粉末、氧化铝粉末、氧化钇粉末、分散剂和去离子水混合,取得混合坯料,再将混合坯料经球形模具制得球形坯体,然后在1650℃~1700℃和压强为0.5MPa的条件下煅烧0.5h~3h,取得氮化硅陶瓷微球。该方法制作的氮化硅微球形状规整,且机械强度优异,有良好水热稳定性。
上述氮化硅粉末的粒径为0.5μm~2.5μm,氧化铝粉末的粒径为0.3μm~5.0μm,氧化钇粉末的粒径为0.1μm~5.0μm;所述氮化硅粉末占混合坯料总质量的65~90%,氧化铝粉末占混合坯料总质量的2~4%,氧化钇粉末占混合坯料总质量的6~8%。该方法中材料所选的粒径、用量、配比均为反复实验所得合成氮化硅微球最佳选用范围。
所述分散剂为木质素磺酸盐等可调节氮化硅粉末表面电位的阴离子表面活性剂。
另外,本发明还进一步公开了具有甲基的ZSM-5分子筛的制备方法:先将氯酸钠、四丙基氢氧化铵和水混合均匀后,再混入甲基硅脂和四甲氧基硅脂,取得分子筛前驱体,然后将分子筛前驱体在180℃陈化4天,取得具有甲基的ZSM-5分子筛。本方法可有效制取具有优异疏水亲油型的分子筛,且所的分子筛孔道结构规整,吸附、过滤效率高。
所述氯酸钠占分子筛前驱体总质量的0.2%,四丙基氢氧化铵占分子筛前驱体总质量的14%,四甲氧基硅脂占分子筛前驱体总质量的21%,甲基硅脂占分子筛前驱体总质量的5%,其余为水。该方法中材料所选的配比均为多次实验所得合成具有甲基的ZSM-5分子筛的最佳选用值。
本发明第三目的是提出以上表面负载分子筛的氮化硅微球的应用。
即,将表面负载分子筛的氮化硅微球作为滤料装填在漏斗中。
采用以上表面负载分子筛的氮化硅微球作为滤料,替代漏斗的滤纸等过滤用材料,可以在不影响水溶液中水溶性组分的情况下,有效吸附过滤混合体系中的大颗粒和有机物成分。
附图说明
图1为本发明的一种应用结构示意图。
具体实施方式
一、制备氮化硅陶瓷微球:
将氮化硅粉末、氧化铝粉末、氧化钇粉末与分散剂、去离子水进行混合,制备出混合坯料。
以上原料中,氮化硅粉末粒径0.5μm~2.5μm,添加量为总粉体重量的65~90%;氧化铝粉末粒径0.3μm~5.0μm,添加量为总粉体重量的2~4%;氧化钇粉末粒径为0.1μm~5.0μm,添加量为总粉体重量的6~8%;分散剂为总粉体重量的12.8%;其余为去离子水,合计量为100%。
以上分散剂的为木质素磺酸盐等可调节氮化硅粉末表面电位的阴离子表面活性剂。
将以上混合坯料挤入微球模具中,在1650℃至1700℃之间进行煅烧,保温0.5h~3h,压强0.5MPa,形成直径为0.5±0.002cm的氮化硅陶瓷微球。
二、制备具有甲基的ZSM-5分子筛:
将氯酸钠、四丙基氢氧化铵和水混合均匀后,再加入甲基硅脂和四甲氧基硅脂,取得分子筛前驱体,然后将分子筛前驱体在180℃陈化4天,取得具有甲基的ZSM-5分子筛,硅铝比为30~40∶1。
其中,所述氯酸钠占分子筛前驱体总质量的0.2%,四丙基氢氧化铵占分子筛前驱体总质量的14%,四甲氧基硅脂占分子筛前驱体总质量的21%,甲基硅脂占分子筛前驱体总质量的5%,其余为去离子水,合计量为100%。
三、制备表面负载分子筛的氮化硅微球:
将具有甲基的ZSM-5分子筛喷涂在氮化硅陶瓷微球表面,在温度环境为80℃的条件下干燥固化,即得表面负载分子筛的氮化硅微球。
四、应用:
1、过滤器的制作:
将表面负载分子筛的氮化硅微球装入球状玻璃腔室中,该腔室的上、下两端各自开有一个小于该微球粒径的通孔。
在一个通孔上焊接喇叭形玻璃漏斗,在另一个通孔上焊接直形玻璃出液管。
形成的产品如图1所示:在喇叭形玻璃漏斗1和直形玻璃出液管2之间连通有球状玻璃腔室3,在球状玻璃腔室3内装填有表面负载分子筛的氮化硅微球4。
2、过滤使用及效果:
在直形玻璃出液管2下方放置接收皿,向过滤器的喇叭形玻璃漏斗1内加入待过滤的混合体系,通过球状玻璃腔室3内的表面负载分子筛的氮化硅微球4即可实现有效过滤。
表面粗糙的氮化硅陶瓷微球由热压铸法成型,用作过滤器基材,既有较大比表面积,又稳定耐腐蚀,提供可过滤水溶液中有机物的有效成分——含甲基的分子筛固载支持。含甲基的分子筛由水热法合成,通过胶质与表面粗糙的氮化硅微球紧密结合。含甲基的分子筛的修饰使得氮化硅陶瓷微球具有较强疏水性,可有效吸附有机物质,同时对水与水溶性物质产生排斥。达到优异的水中大颗粒和有机物过滤、分离作用。
以上所述实施例仅是对本发明的优选方式进行描述,并非对本发明范围的限定,在不脱离本发明设计精神前提下,本领域普通技术人员对本发明的技术方案作出的各种变形与改进,均应落入本发明权利要求书确定的保护范围。
Claims (10)
1.一种表面负载分子筛的氮化硅微球,其特征在于:在氮化硅陶瓷微球表面负载具有甲基的ZSM-5分子筛。
2.根据权利要求1所述表面负载分子筛的氮化硅微球,其特征在于:所述氮化硅陶瓷微球的直径为0.5±0.002cm。
3.如权利要求1所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:将具有甲基的ZSM-5分子筛喷涂在氮化硅陶瓷微球表面,经干燥,即成。
4.根据权利要求3所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:所述干燥的温度环境为80℃。
5.根据权利要求3所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:将氮化硅粉末、氧化铝粉末、氧化钇粉末、分散剂和去离子水混合,取得混合坯料,再将混合坯料经球形模具制得球形坯体,然后在1650℃~1700℃和压强为0.5MPa的条件下煅烧0.5h~3h,取得氮化硅陶瓷微球。
6.根据权利要求5所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:所述氮化硅粉末的粒径为0.5μm~2.5μm,氧化铝粉末的粒径为0.3μm~5.0μm,氧化钇粉末的粒径为0.1μm~5.0μm;所述氮化硅粉末占混合坯料总质量的65~90%,氧化铝粉末占混合坯料总质量的2~4%,氧化钇粉末占混合坯料总质量的6~8%。
7.根据权利要求5所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:所述分散剂的为木质素磺酸盐。
8.根据权利要求3所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:先将氯酸钠、四丙基氢氧化铵和水混合均匀后,再混入甲基硅脂和四甲氧基硅脂,取得分子筛前驱体,然后将分子筛前驱体在180℃陈化4天,取得具有甲基的ZSM-5分子筛。
9.根据权利要求8所述表面负载分子筛的氮化硅微球的制备方法,其特征在于:所述氯酸钠占分子筛前驱体总质量的0.2 %,四丙基氢氧化铵占分子筛前驱体总质量的14 %,四甲氧基硅脂占分子筛前驱体总质量的21%,甲基硅脂占分子筛前驱体总质量的5%,其余为去离子水,合计量为100%。
10.如权利要求1所述表面负载分子筛的氮化硅微球的应用,其特征在于:将表面负载分子筛的氮化硅微球作为滤料装填在漏斗中。
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