CN107138145A - 一种凹凸棒土负载纳米钛酸锶的制备方法 - Google Patents
一种凹凸棒土负载纳米钛酸锶的制备方法 Download PDFInfo
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Abstract
本发明公开了一种凹凸棒土负载纳米钛酸锶的制备方法,步骤为:按照等摩尔比称取醋酸锶和钛酸四丁酯,然后将醋酸锶溶于蒸馏水中,得溶液A,将钛酸四丁酯溶于异丙醇中,得溶液B;在磁力搅拌下将溶液A逐滴加入到溶液B中,继续搅拌2‑4min,静置陈化,然后加入纯化凹凸棒土,搅拌10‑15min,过滤,放置1‑2天后烘干至恒重,烘干后在200‑250℃下预烧1‑3h,升温至380‑420℃,恒温2‑4h,再升温至590‑630℃,恒温1‑2h,再升温至770‑810℃,恒温0.5‑1h,自然冷却,次日取出即可。本发明能够高效快速地吸附并分解甲醛,苯,氨,TVOC等有害气体,达到净化,消毒,除臭,杀菌的目的。
Description
技术领域
本发明涉及涉及一种凹凸棒土负载纳米钛酸锶的制备方法,属于光触媒材料领域。
背景技术
凹凸棒土是一种层链状结构的水富镁铝硅酸粘土矿物,由于凹凸棒土特殊的结构,使其具备许多优良的特征,如具有较好的吸附能力,独特的分散性,耐高温、抗盐碱,有较高的可塑性及粘结力,矿物本身质轻、性脆、吸水性强,比面积大,干燥后收缩小,不大显裂纹,水浸泡崩散,悬浮液遇电质不絮凝、不沉淀,所以凹凸棒土具有广泛的应用领域,可用作吸附剂、催化剂、胶凝剂、填充剂、悬浮剂、增稠剂、脱色剂等。
光触媒材料是在光的照射下(自然光,灯光)会产生类似与光合作用的光催化反应,产生出氧化能力极强的氢氧自由基和活性氧,具有很强的氧化还原功能,可氧化分解各种有机化合物和部分无机物,能破坏细菌的细胞膜和病毒的蛋白质,把有机污染物分解成二氧化碳和水,因而光触媒材料具有极强的杀菌、除臭、防霉、防污自洁等功能,可广泛应用于涂料,起到净化环境的作用。
目前光触媒材料主要有TiO2、ZnO、SnO2、CdS、ZnS等。虽然光触媒材料具有广阔的应用前景,但要实现工业化还存在着一定的距离,必须首先解决光触媒材料回收困难的问题,所以需将光触媒材料固定化,负载于载体上,载体包括玻璃陶瓷类、高分子聚合物类和吸附剂类等。其中吸附剂类载体具有比表面积大、多孔、吸附性能良好、稳定性高等特点,以活性炭的吸附性能最好,也是目前研究最广泛的吸附剂载体,但其价格昂贵、再生困难,应用受到一定的限制。凹凸棒土具有比面积大,稳定性好,吸附能力强,矿藏丰富,价格较活性炭便宜,可广泛用作光触媒材料的载体。目前市场上多常见凹凸棒土负载纳米二氧化钛光触媒材料,很少见到凹凸棒土负载纳米钛酸锶光触媒材料。因此,本发明开发了一种凹凸棒土负载纳米钛酸锶的制备方法。
发明内容
本发明的目的在于提供一种凹凸棒土负载纳米钛酸锶的制备方法。本发明将纳米钛酸锶负载到凹凸棒土表面和孔隙内部,使吸附性能与光催化性能得到有机结合,从而能够高效快速地吸附并分解甲醛,苯,氨,TVOC等有害气体,达到净化,消毒,除臭,杀菌的目的。
为实现上述目的,本发明采用如下的技术方案:
一种凹凸棒土负载纳米钛酸锶的制备方法,包括以下步骤:
(1)按照等摩尔比称取醋酸锶和钛酸四丁酯,然后将醋酸锶溶于蒸馏水中,得溶液A,将钛酸四丁酯溶于异丙醇中,得溶液B;
(2)在磁力搅拌下将溶液A以每秒2-3滴的速度逐滴加入到溶液B中,继续搅拌2-4min,静置陈化24-48h,形成凝胶,然后加入相当于凝胶质量50-60%的纯化凹凸棒土,在2000-3000r/min的转速下搅拌10-15min,过滤,放置1-2天后在100-110℃下烘干至恒重,烘干后在200-250℃下预烧1-3h,升温至380-420℃,恒温2-4h,再升温至590-630℃,恒温1-2h,再升温至770-810℃,恒温0.5-1h,自然冷却,次日取出,即得所需的凹凸棒土负载纳米钛酸锶。
步骤(1)中所述的醋酸锶和蒸馏水的质量比为1:3-4。
步骤(1)中所述的钛酸四丁酯和异丙醇的体积比为1:15-20。
步骤(2)中所述的纯化凹凸棒土的制备方法如下:将凹凸棒土研磨至100目以下,然后按照固液比1:8-10将凹凸棒土加入水中,在1500-2000r/min的转速下以及70-80℃水浴温度下搅拌制浆,得到凹凸棒土悬浮液,然后对凹凸棒土悬浮液进行高压脉冲电场处理,电场强度为30-40kV/cm,脉冲电场频率为200-300Hz,处理时间为5-10s,处理完毕后向凹凸棒土悬浮液中加入相当于凹凸棒土质量5-10%的六偏磷酸钠和4-7%的丙烯酰胺-丙烯酸钠共聚物,在4000-5000r/min的转速下球磨20-30min,再超声波分散30-40min后进行低速离心分离,去除杂质,倒出剩余的悬浮液再进行高速离心分离,所得的底部物质经洗涤、干燥、研磨、过筛即得纯化凹凸棒土。
所述的超声波功率为150-200W。
所述的低速离心分离中离心转速为500-800r/min,离心时间为30-40min。
所述的高速离心分离中离心转速为6000-8000r/min,离心时间为10-20min。
本发明的有益效果:
本发明采用溶胶-凝胶法将纳米钛酸锶光触媒材料固定在具有优良吸附性能的载体凹凸棒土表面和孔隙内部,可以增加光催化反应的比表面积,将凹凸棒土的吸附作用与纳米钛酸锶的光催化性能紧密结合,以增强光催化反应速率和效率,从而提高光催化性能,能够高效快速地吸附并分解甲醛,苯,氨,TVOC等有害气体,达到净化,消毒,除臭,杀菌的目的。
具体实施方式
实施例1
一种凹凸棒土负载纳米钛酸锶的制备方法,包括以下步骤:
(1)按照等摩尔比称取醋酸锶和钛酸四丁酯,然后将醋酸锶溶于蒸馏水中,得溶液A,将钛酸四丁酯溶于异丙醇中,得溶液B;
(2)在磁力搅拌下将溶液A以每秒2滴的速度逐滴加入到溶液B中,继续搅拌2min,静置陈化24h,形成凝胶,然后加入相当于凝胶质量50%的纯化凹凸棒土,在2000r/min的转速下搅拌15min,过滤,放置1天后在100℃下烘干至恒重,烘干后在200℃下预烧3h,升温至380℃,恒温4h,再升温至590℃,恒温2h,再升温至770℃,恒温1h,自然冷却,次日取出,即得所需的凹凸棒土负载纳米钛酸锶。
步骤(1)中所述的醋酸锶和蒸馏水的质量比为1:3。
步骤(1)中所述的钛酸四丁酯和异丙醇的体积比为1:15。
步骤(2)中所述的纯化凹凸棒土的制备方法如下:将凹凸棒土研磨至100目以下,然后按照固液比1:8将凹凸棒土加入水中,在1500r/min的转速下以及70℃水浴温度下搅拌制浆,得到凹凸棒土悬浮液,然后对凹凸棒土悬浮液进行高压脉冲电场处理,电场强度为30kV/cm,脉冲电场频率为200Hz,处理时间为10s,处理完毕后向凹凸棒土悬浮液中加入相当于凹凸棒土质量5%的六偏磷酸钠和4%的丙烯酰胺-丙烯酸钠共聚物,在4000r/min的转速下球磨30min,再超声波分散30min后进行低速离心分离,去除杂质,倒出剩余的悬浮液再进行高速离心分离,所得的底部物质经洗涤、干燥、研磨、过筛即得纯化凹凸棒土。
所述的超声波功率为200W。
所述的低速离心分离中离心转速为500r/min,离心时间为40min。
所述的高速离心分离中离心转速为6000r/min,离心时间为20min。
实施例2
一种凹凸棒土负载纳米钛酸锶的制备方法,包括以下步骤:
(1)按照等摩尔比称取醋酸锶和钛酸四丁酯,然后将醋酸锶溶于蒸馏水中,得溶液A,将钛酸四丁酯溶于异丙醇中,得溶液B;
(2)在磁力搅拌下将溶液A以每秒2滴的速度逐滴加入到溶液B中,继续搅拌3min,静置陈化36h,形成凝胶,然后加入相当于凝胶质量55%的纯化凹凸棒土,在2500r/min的转速下搅拌12min,过滤,放置2天后在105℃下烘干至恒重,烘干后在220℃下预烧2h,升温至400℃,恒温3h,再升温至610℃,恒温1.5h,再升温至790℃,恒温0.5h,自然冷却,次日取出,即得所需的凹凸棒土负载纳米钛酸锶。
步骤(1)中所述的醋酸锶和蒸馏水的质量比为1:3。
步骤(1)中所述的钛酸四丁酯和异丙醇的体积比为1:18。
步骤(2)中所述的纯化凹凸棒土的制备方法如下:将凹凸棒土研磨至100目以下,然后按照固液比1:9将凹凸棒土加入水中,在1800r/min的转速下以及75℃水浴温度下搅拌制浆,得到凹凸棒土悬浮液,然后对凹凸棒土悬浮液进行高压脉冲电场处理,电场强度为35kV/cm,脉冲电场频率为250Hz,处理时间为8s,处理完毕后向凹凸棒土悬浮液中加入相当于凹凸棒土质量8%的六偏磷酸钠和5%的丙烯酰胺-丙烯酸钠共聚物,在4500r/min的转速下球磨25min,再超声波分散35min后进行低速离心分离,去除杂质,倒出剩余的悬浮液再进行高速离心分离,所得的底部物质经洗涤、干燥、研磨、过筛即得纯化凹凸棒土。
所述的超声波功率为180W。
所述的低速离心分离中离心转速为700r/min,离心时间为35min。
所述的高速离心分离中离心转速为7000r/min,离心时间为15min。
实施例3
一种凹凸棒土负载纳米钛酸锶的制备方法,包括以下步骤:
(1)按照等摩尔比称取醋酸锶和钛酸四丁酯,然后将醋酸锶溶于蒸馏水中,得溶液A,将钛酸四丁酯溶于异丙醇中,得溶液B;
(2)在磁力搅拌下将溶液A以每秒3滴的速度逐滴加入到溶液B中,继续搅拌4min,静置陈化48h,形成凝胶,然后加入相当于凝胶质量60%的纯化凹凸棒土,在2500r/min的转速下搅拌12min,过滤,放置2天后在110℃下烘干至恒重,烘干后在250℃下预烧1h,升温至420℃,恒温2h,再升温至630℃,恒温1h,再升温至810℃,恒温0.5h,自然冷却,次日取出,即得所需的凹凸棒土负载纳米钛酸锶。
步骤(1)中所述的醋酸锶和蒸馏水的质量比为1:4。
步骤(1)中所述的钛酸四丁酯和异丙醇的体积比为1:20。
步骤(2)中所述的纯化凹凸棒土的制备方法如下:将凹凸棒土研磨至100目以下,然后按照固液比1:10将凹凸棒土加入水中,在2000r/min的转速下以及80℃水浴温度下搅拌制浆,得到凹凸棒土悬浮液,然后对凹凸棒土悬浮液进行高压脉冲电场处理,电场强度为40kV/cm,脉冲电场频率为300Hz,处理时间为5s,处理完毕后向凹凸棒土悬浮液中加入相当于凹凸棒土质量10%的六偏磷酸钠和7%的丙烯酰胺-丙烯酸钠共聚物,在5000r/min的转速下球磨20min,再超声波分散40min后进行低速离心分离,去除杂质,倒出剩余的悬浮液再进行高速离心分离,所得的底部物质经洗涤、干燥、研磨、过筛即得纯化凹凸棒土。
所述的超声波功率为150W。
所述的低速离心分离中离心转速为800r/min,离心时间为30min。
所述的高速离心分离中离心转速为8000r/min,离心时间为10min。
Claims (7)
1.一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,包括以下步骤:
(1)按照等摩尔比称取醋酸锶和钛酸四丁酯,然后将醋酸锶溶于蒸馏水中,得溶液A,将钛酸四丁酯溶于异丙醇中,得溶液B;
(2)在磁力搅拌下将溶液A以每秒2-3滴的速度逐滴加入到溶液B中,继续搅拌2-4min,静置陈化24-48h,形成凝胶,然后加入相当于凝胶质量50-60%的纯化凹凸棒土,在2000-3000r/min的转速下搅拌10-15min,过滤,放置1-2天后在100-110℃下烘干至恒重,烘干后在200-250℃下预烧1-3h,升温至380-420℃,恒温2-4h,再升温至590-630℃,恒温1-2h,再升温至770-810℃,恒温0.5-1h,自然冷却,次日取出,即得所需的凹凸棒土负载纳米钛酸锶。
2.根据权利要求1所述的一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,步骤(1)中所述的醋酸锶和蒸馏水的质量比为1:3-4。
3.根据权利要求1所述的一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,步骤(1)中所述的钛酸四丁酯和异丙醇的体积比为1:15-20。
4.根据权利要求1所述的一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,步骤(2)中所述的纯化凹凸棒土的制备方法如下:将凹凸棒土研磨至100目以下,然后按照固液比1:8-10将凹凸棒土加入水中,在1500-2000r/min的转速下以及70-80℃水浴温度下搅拌制浆,得到凹凸棒土悬浮液,然后对凹凸棒土悬浮液进行高压脉冲电场处理,电场强度为30-40kV/cm,脉冲电场频率为200-300Hz,处理时间为5-10s,处理完毕后向凹凸棒土悬浮液中加入相当于凹凸棒土质量5-10%的六偏磷酸钠和4-7%的丙烯酰胺-丙烯酸钠共聚物,在4000-5000r/min的转速下球磨20-30min,再超声波分散30-40min后进行低速离心分离,去除杂质,倒出剩余的悬浮液再进行高速离心分离,所得的底部物质经洗涤、干燥、研磨、过筛即得纯化凹凸棒土。
5.根据权利要求4所述的一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,所述的超声波功率为150-200W。
6.根据权利要求4所述的一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,所述的低速离心分离中离心转速为500-800r/min,离心时间为30-40min。
7.根据权利要求4所述的一种凹凸棒土负载纳米钛酸锶的制备方法,其特征在于,所述的高速离心分离中离心转速为6000-8000r/min,离心时间为10-20min。
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