CN105688798A - 一种光敏感高热稳定性柱撑粘土材料的制备方法 - Google Patents
一种光敏感高热稳定性柱撑粘土材料的制备方法 Download PDFInfo
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- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 6
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Abstract
本发明公开了一种光敏感高热稳定性柱撑粘土材料的制备方法,属于柱撑粘土材料领域。本发明制备出钠化钙基蒙脱石粉为粘土基质,将硅胶负载在钠化钙基蒙脱石粉中,不仅使柱撑粘土保持原有大的孔径和比表面积,而且还具有很高的热稳定性,在粘土矿物的层间插入分子级的二氧化钛支撑柱,得到的柱撑粘土有较强的光催化活性,即使在可见光下也具有光催化能力,使其应用更广泛。
Description
技术领域
本发明公开了一种光敏感高热稳定性柱撑粘土材料的制备方法,属于柱撑粘土材料领域。
背景技术
柱撑粘土复合材料是近几十年来受到广泛关注并得到迅速发展的一类新型类分子筛催化材料。它是利用某些具有层状结构的粘土矿物中层间所存在的可交换性阳离子通过交换反应引入外界的离子型化合物,从而在其原位生成分子级别的支撑柱,并通过干燥、烧结等手段将柱化剂转化为具有一定吸附或催化性能的大孔径和具热稳定性的复合材料。由于所合成的这类材料具有大的比表面积或催化活性的层间支撑柱,使得其能够有效吸附或转化各类有机物质,从而在环境修复、环境净化方面得到了广泛应用。
提高柱撑粘土的热稳定性。所有的柱撑粘土都会在几百摄氏度的烧结高温下发生层塌陷,致使合成材料的活性与表面积大大降低。而且目前光催化剂型柱撑粘土仍主要是在紫外线下才能够发挥其光催化活性,故限制了它在其他许多催化条件下的应用,如可开拓能够利用可见光或者不用光照射的催化剂作支撑柱制备柱撑粘土。
发明内容
本发明主要解决的技术问题:针对目前柱撑粘土在几百摄氏度的烧结高温下会发生层塌陷,致使合成材料的活性与表面积大大降低,而且光催化剂型柱撑粘土在紫外线下才能够发挥其光催化活性,限制了其应用的问题,提供了一种光敏感高热稳定性柱撑粘土材料的制备方法,本发明制备出钠化钙基蒙脱石粉为粘土基质,将硅胶负载在钠化钙基蒙脱石粉中,不仅使柱撑粘土保持原有大的孔径和比表面积,而且还具有很高的热稳定性,在粘土矿物的层间插入分子级的二氧化钛支撑柱,得到的柱撑粘土有较强的光催化活性,即使在可见光下也具有光催化能力,使其应用更广泛。
为了解决上述技术问题,本发明所采用的技术方案是:
1.(1)称取10~20g钙基蒙脱石粉和10~15g碳酸钠粉末混合后倒入200~400mL蒸馏水中,放入超声分散仪超声分散3~5min后移入水浴锅并升温至50~70℃,用磁力搅拌机搅拌1~3h,保温老化过夜,老化结束后将老化液反复离心5~7次,分离去除上清液,合并沉淀物,干燥后研磨过200目标准筛,得到钠化钙基蒙脱石粉,备用;
2.(2)量取30~50mL无水乙醇和100~150mL正硅酸乙酯一起装入500mL烧杯中,用玻璃棒搅拌均匀,在搅拌的过程中分3~5次加入15~20mL质量浓度为15%的盐酸溶液,继续搅拌15~20min后放入老化箱中,常温下静置老化2~3h,制得硅溶胶;
3.(3)将10~15g上述备用的钠化钙基蒙脱石粉加入到200~300mL蒸馏水中,搅拌形成悬浮液,再将100~200mL制得的硅溶胶逐滴滴入悬浮液中,控制滴加速度使其20~30min内滴加完毕,并继续用磁力搅拌机搅拌30~40min,过滤得滤饼,备用;
4.(4)取1~2g聚丙烯酰胺倒入50~100mL无水乙醇中,放置在磁力搅拌机上搅拌2~3min,再将15~20mL正钛酸正丁酯滴入搅拌中的混合液中,滴加完毕后将混合液放入旋涡振荡仪中,以10~20W的功率振荡分散10~20min,得混合液;
5.(5)将20~30g步骤(3)备用的滤饼倒入上述混合液中,移入冰浴锅并放置在摇床上,在4~6℃下振荡分散10~15min,振荡结束后再加入40~50mL质量浓度为30%的氨水,用磁力搅拌机室温下搅拌1~2h后将混合物倒入布氏漏斗,用去离子水洗涤抽滤3~5次得滤渣;
6.(6)得到滤渣后,先将滤渣放入烘箱中,在105~110℃下干燥至恒重,干燥完成后将其移入马弗炉中,以5℃/min的速率程序升温至500~600℃,保温煅烧3~4h后即得一种光敏感高热稳定性柱撑粘土材料。
本发明的应用方法:本发明制得的光敏感高热稳定性柱撑粘土材料可以应用在水体中对有机污染物的吸附和光催化降解作用,按2~3g/L加入到含有甲苯、二甲苯和乙硫醇的有机废水中,吸附3~5min后对分别对甲苯、二甲苯和乙硫醇吸附去除率均高于60%,在自然光下降解50~60min后对甲苯、二甲苯和乙硫醇的光催化降解率分别达到98.2~98.6%,99.5~99.6%,99.2~99.4%,实现了有机污染物的吸附与光催化氧化的一体化,可以有效地降解、吸附有机污染物,增强了光催化降解有机污染物的反应速率和效率。
9.本发明的有益效果是:
(1)本发明制备出硅胶负载在钠化钙基蒙脱石粉中,不仅使柱撑粘土保持原有大的孔径和比表面积,而且还具有很高的热稳定性;
(2)在粘土矿物的层间插入分子级的二氧化钛支撑柱,得到的柱撑粘土有较强的光催化活性,即使在可见光下也具有很强的光催化能力。
具体实施方式
首先称取10~20g钙基蒙脱石粉和10~15g碳酸钠粉末混合后倒入200~400mL蒸馏水中,放入超声分散仪超声分散3~5min后移入水浴锅并升温至50~70℃,用磁力搅拌机搅拌1~3h,保温老化过夜,老化结束后将老化液反复离心5~7次,分离去除上清液,合并沉淀物,干燥后研磨过200目标准筛,得到钠化钙基蒙脱石粉,备用;量取30~50mL无水乙醇和100~150mL正硅酸乙酯一起装入500mL烧杯中,用玻璃棒搅拌均匀,在搅拌的过程中分3~5次加入15~20mL质量浓度为15%的盐酸溶液,继续搅拌15~20min后放入老化箱中,常温下静置老化2~3h,制得硅溶胶;将10~15g上述备用的钠化钙基蒙脱石粉加入到200~300mL蒸馏水中,搅拌形成悬浮液,再将100~200mL制得的硅溶胶逐滴滴入悬浮液中,控制滴加速度使其20~30min内滴加完毕,并继续用磁力搅拌机搅拌30~40min,过滤得滤饼,备用;取1~2g聚丙烯酰胺倒入50~100mL无水乙醇中,放置在磁力搅拌机上搅拌2~3min,再将15~20mL正钛酸正丁酯滴入搅拌中的混合液中,滴加完毕后将混合液放入旋涡振荡仪中,以10~20W的功率振荡分散10~20min,得混合液;将20~30g备用的滤饼倒入混合液中,移入冰浴锅并放置在摇床上,在4~6℃下振荡分散10~15min,振荡结束后再加入40~50mL质量浓度为30%的氨水,用磁力搅拌机室温下搅拌1~2h后将混合物倒入布氏漏斗,用去离子水洗涤抽滤3~5次得滤渣;得到滤渣后,先将滤渣放入烘箱中,在105~110℃下干燥至恒重,干燥完成后将其移入马弗炉中,以5℃/min的速率程序升温至500~600℃,保温煅烧3~4h后即得一种光敏感高热稳定性柱撑粘土材料。
实例1
11.首先称取10g钙基蒙脱石粉和10g碳酸钠粉末混合后倒入200mL蒸馏水中,放入超声分散仪超声分散3min后移入水浴锅并升温至50℃,用磁力搅拌机搅拌1h,保温老化过夜,老化结束后将老化液反复离心5次,分离去除上清液,合并沉淀物,干燥后研磨过200目标准筛,得到钠化钙基蒙脱石粉,备用;量取30mL无水乙醇和100mL正硅酸乙酯一起装入500mL烧杯中,用玻璃棒搅拌均匀,在搅拌的过程中分3次加入15mL质量浓度为15%的盐酸溶液,继续搅拌15min后放入老化箱中,常温下静置老化2h,制得硅溶胶;将10g上述备用的钠化钙基蒙脱石粉加入到200mL蒸馏水中,搅拌形成悬浮液,再将100mL制得的硅溶胶逐滴滴入悬浮液中,控制滴加速度使其20min内滴加完毕,并继续用磁力搅拌机搅拌30min,过滤得滤饼,备用;取1g聚丙烯酰胺倒入50mL无水乙醇中,放置在磁力搅拌机上搅拌2min,再将15mL正钛酸正丁酯滴入搅拌中的混合液中,滴加完毕后将混合液放入旋涡振荡仪中,以10W的功率振荡分散10min,得混合液;将20g备用的滤饼倒入混合液中,移入冰浴锅并放置在摇床上,在4℃下振荡分散10min,振荡结束后再加入40mL质量浓度为30%的氨水,用磁力搅拌机室温下搅拌1h后将混合物倒入布氏漏斗,用去离子水洗涤抽滤3次得滤渣;得到滤渣后,先将滤渣放入烘箱中,在105℃下干燥至恒重,干燥完成后将其移入马弗炉中,以5℃/min的速率程序升温至500℃,保温煅烧3h后即得一种光敏感高热稳定性柱撑粘土材料。
本发明制得的光敏感高热稳定性柱撑粘土材料可以应用在水体中对有机污染物的吸附和光催化降解作用,按2g/L加入到含有甲苯、二甲苯和乙硫醇的有机废水中,吸附3min后对分别对甲苯、二甲苯和乙硫醇吸附去除率为65%、68%、63%,在自然光下降解50min后对甲苯、二甲苯和乙硫醇的光催化降解率分别达到98.2%,99.5%,99.2%,实现了有机污染物的吸附与光催化氧化的一体化,可以有效地降解、吸附有机污染物,增强了光催化降解有机污染物的反应速率和效率。
实例2
12.首先称取15g钙基蒙脱石粉和13g碳酸钠粉末混合后倒入300mL蒸馏水中,放入超声分散仪超声分散4min后移入水浴锅并升温至60℃,用磁力搅拌机搅拌2h,保温老化过夜,老化结束后将老化液反复离心6次,分离去除上清液,合并沉淀物,干燥后研磨过200目标准筛,得到钠化钙基蒙脱石粉,备用;量取40mL无水乙醇和125mL正硅酸乙酯一起装入500mL烧杯中,用玻璃棒搅拌均匀,在搅拌的过程中分4次加入17mL质量浓度为15%的盐酸溶液,继续搅拌17min后放入老化箱中,常温下静置老化2.5h,制得硅溶胶;将13g上述备用的钠化钙基蒙脱石粉加入到250mL蒸馏水中,搅拌形成悬浮液,再将150mL制得的硅溶胶逐滴滴入悬浮液中,控制滴加速度使其25min内滴加完毕,并继续用磁力搅拌机搅拌35min,过滤得滤饼,备用;取1.5g聚丙烯酰胺倒入75mL无水乙醇中,放置在磁力搅拌机上搅拌2.5min,再将17mL正钛酸正丁酯滴入搅拌中的混合液中,滴加完毕后将混合液放入旋涡振荡仪中,以15W的功率振荡分散15min,得混合液;将25g备用的滤饼倒入混合液中,移入冰浴锅并放置在摇床上,在5℃下振荡分散13min,振荡结束后再加入45mL质量浓度为30%的氨水,用磁力搅拌机室温下搅拌1.5h后将混合物倒入布氏漏斗,用去离子水洗涤抽滤4次得滤渣;得到滤渣后,先将滤渣放入烘箱中,在108℃下干燥至恒重,干燥完成后将其移入马弗炉中,以5℃/min的速率程序升温至550℃,保温煅烧3.5h后即得一种光敏感高热稳定性柱撑粘土材料。
本发明制得的光敏感高热稳定性柱撑粘土材料可以应用在水体中对有机污染物的吸附和光催化降解作用,按2.5g/L加入到含有甲苯、二甲苯和乙硫醇的有机废水中,吸附4min后对分别对甲苯、二甲苯和乙硫醇吸附去除率为66%、69%、65%,在自然光下降解55min后对甲苯、二甲苯和乙硫醇的光催化降解率分别达到98.4%,99.5%,99.3%,实现了有机污染物的吸附与光催化氧化的一体化,可以有效地降解、吸附有机污染物,增强了光催化降解有机污染物的反应速率和效率。
实例3
13.首先称取20g钙基蒙脱石粉和15g碳酸钠粉末混合后倒入400mL蒸馏水中,放入超声分散仪超声分散5min后移入水浴锅并升温至70℃,用磁力搅拌机搅拌3h,保温老化过夜,老化结束后将老化液反复离心7次,分离去除上清液,合并沉淀物,干燥后研磨过200目标准筛,得到钠化钙基蒙脱石粉,备用;量取50mL无水乙醇和150mL正硅酸乙酯一起装入500mL烧杯中,用玻璃棒搅拌均匀,在搅拌的过程中分5次加入20mL质量浓度为15%的盐酸溶液,继续搅拌20min后放入老化箱中,常温下静置老化3h,制得硅溶胶;将15g上述备用的钠化钙基蒙脱石粉加入到300mL蒸馏水中,搅拌形成悬浮液,再将200mL制得的硅溶胶逐滴滴入悬浮液中,控制滴加速度使其30min内滴加完毕,并继续用磁力搅拌机搅拌40min,过滤得滤饼,备用;取2g聚丙烯酰胺倒入100mL无水乙醇中,放置在磁力搅拌机上搅拌3min,再将20mL正钛酸正丁酯滴入搅拌中的混合液中,滴加完毕后将混合液放入旋涡振荡仪中,以20W的功率振荡分散20min,得混合液;将30g备用的滤饼倒入混合液中,移入冰浴锅并放置在摇床上,在6℃下振荡分散15min,振荡结束后再加入50mL质量浓度为30%的氨水,用磁力搅拌机室温下搅拌2h后将混合物倒入布氏漏斗,用去离子水洗涤抽滤5次得滤渣;得到滤渣后,先将滤渣放入烘箱中,在110℃下干燥至恒重,干燥完成后将其移入马弗炉中,以5℃/min的速率程序升温至600℃,保温煅烧4h后即得一种光敏感高热稳定性柱撑粘土材料。
本发明制得的光敏感高热稳定性柱撑粘土材料应用在水体中对有机污染物的吸附和光催化降解作用,按3g/L加入到含有甲苯、二甲苯和乙硫醇的有机废水中,吸附5min后对分别对甲苯、二甲苯和乙硫醇吸附去除率为67%、70%、66%,在自然光下降解60min后对甲苯、二甲苯和乙硫醇的光催化降解率分别达到98.6%,99.6%,99.4%,实现了有机污染物的吸附与光催化氧化的一体化,可以有效地降解、吸附有机污染物,增强了光催化降解有机污染物的反应速率和效率。
Claims (1)
1.一种光敏感高热稳定性柱撑粘土材料的制备方法,其特征在于具体制备步骤为:
(1)称取10~20g钙基蒙脱石粉和10~15g碳酸钠粉末混合后倒入200~400mL蒸馏水中,放入超声分散仪超声分散3~5min后移入水浴锅并升温至50~70℃,用磁力搅拌机搅拌1~3h,保温老化过夜,老化结束后将老化液反复离心5~7次,分离去除上清液,合并沉淀物,干燥后研磨过200目标准筛,得到钠化钙基蒙脱石粉,备用;
(2)量取30~50mL无水乙醇和100~150mL正硅酸乙酯一起装入500mL烧杯中,用玻璃棒搅拌均匀,在搅拌的过程中分3~5次加入15~20mL质量浓度为15%的盐酸溶液,继续搅拌15~20min后放入老化箱中,常温下静置老化2~3h,制得硅溶胶;
(3)将10~15g上述备用的钠化钙基蒙脱石粉加入到200~300mL蒸馏水中,搅拌形成悬浮液,再将100~200mL制得的硅溶胶逐滴滴入悬浮液中,控制滴加速度使其20~30min内滴加完毕,并继续用磁力搅拌机搅拌30~40min,过滤得滤饼,备用;
(4)取1~2g聚丙烯酰胺倒入50~100mL无水乙醇中,放置在磁力搅拌机上搅拌2~3min,再将15~20mL正钛酸正丁酯滴入搅拌中的混合液中,滴加完毕后将混合液放入旋涡振荡仪中,以10~20W的功率振荡分散10~20min,得混合液;
(5)将20~30g步骤(3)备用的滤饼倒入上述混合液中,移入冰浴锅并放置在摇床上,在4~6℃下振荡分散10~15min,振荡结束后再加入40~50mL质量浓度为30%的氨水,用磁力搅拌机室温下搅拌1~2h后将混合物倒入布氏漏斗,用去离子水洗涤抽滤3~5次得滤渣;
(6)得到滤渣后,先将滤渣放入烘箱中,在105~110℃下干燥至恒重,干燥完成后将其移入马弗炉中,以5℃/min的速率程序升温至500~600℃,保温煅烧3~4h后即得一种光敏感高热稳定性柱撑粘土材料。
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CN106732466A (zh) * | 2017-02-27 | 2017-05-31 | 安徽埃克利环境工程有限公司 | 一种吸附反应型甲醛消除剂及其制备方法 |
WO2019000349A1 (zh) * | 2017-06-29 | 2019-01-03 | 黄玉倩 | 一种硅胶粘土的制备工艺 |
CN114259982A (zh) * | 2021-12-31 | 2022-04-01 | 南宁师范大学 | 氧化锌硅基柱撑伊蒙黏土复合材料及其制备方法与应用 |
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CN106732466A (zh) * | 2017-02-27 | 2017-05-31 | 安徽埃克利环境工程有限公司 | 一种吸附反应型甲醛消除剂及其制备方法 |
WO2019000349A1 (zh) * | 2017-06-29 | 2019-01-03 | 黄玉倩 | 一种硅胶粘土的制备工艺 |
CN114259982A (zh) * | 2021-12-31 | 2022-04-01 | 南宁师范大学 | 氧化锌硅基柱撑伊蒙黏土复合材料及其制备方法与应用 |
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