CN107649151A - 一种硫掺杂铁酸钴催化剂的制备方法 - Google Patents
一种硫掺杂铁酸钴催化剂的制备方法 Download PDFInfo
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
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- B01J27/043—Sulfides with iron group metals or platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/39—Photocatalytic properties
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Abstract
本发明公开了一种硫掺杂铁酸钴催化剂的制备方法,步骤如下:将50g黄铁矿粉碎至10~50目,加入20~30g纯碱,用搅拌机搅拌均匀,置于马弗炉中,在800~1000℃下煅烧2~4h,煅烧结束后,加入到100~200mL浓度为0.2~0.5mol/L的氢氧化钠溶液中,剧烈搅拌下,再加入市售有效氯的质量分数为10%的次氯酸钠15~35mL,持续剧烈搅拌2~3h,最后加入1~3g氯化钴,继续搅拌2~4h,固液分离,去除上清液,蒸馏水洗涤固体3~4次,105℃烘干,再置于马弗炉中450~650℃下煅烧4~5h,冷却到室温,即得到一种硫掺杂铁酸钴催化剂。利用黄铁矿生成高铁酸盐,经过处理,得到硫掺杂铁酸钴催化剂,其中还有更多种微量的其他过度元素复合,催化效果大大提高。
Description
技术领域
本发明涉及环境污染控制新材料领域,尤其涉及一种硫掺杂铁酸钴催化剂的制备方法。
背景技术
近年来,随着工业高速发展,我国水环境受到有机物不同程度污染,其中地表河流、地下水体及土壤受到的污染尤为严重。据报道,我国90%的城市地下水遭受到了不同程度的有机和无机有害有毒污染物的污染,因此非常有必要对有机污染物进行去除。而常规的处理工艺对苯酚和苯甲酸的去除效果不尽如人意。经过科学家多年努力,逐渐开发出了很多降解水体中有机污染物的方法,主要有生物降解法、物理吸附法、化学沉淀法、化学还原法及高级氧化法。近年来,新型高效的可见光光催化剂的研制成为光催化技术中的一个重要研究内容,其中具有表面等离子共振效应的光催化材料,因其独特的表面物理化学性质和高效的可见光光催化性能,成为研究的热点之一。
高级氧化法由于其能产生氧化活性的各类自由基,能提高有机污染物的可生物降解性或将其彻底矿化,具有修复速度快、修复效果好的特点而受到广泛运用。钴铁酸盐作为ー种常用的复合氧化物已有许多研究者将其应用于可见光催化分解水反应,但其污染物降解效率较低(苯甲酸降解率小于25%),通常仅用于较易脱色的染料废水处理。
黄铁矿,主要成分是二硫化亚铁FeS2,是提取硫、制造硫酸的主要矿物原料。其特殊的形态色泽,有观赏价值。一些黄铁矿磨制成宝石也很受欢迎。黄铁矿可经由岩浆分结作用、热水溶液或升华作用中生成,也可于火成岩、沉积岩中生成。在工业上,黄铁矿用作硫和二氧化硫生成的原料。
发明内容
本发明的目的是为克服现有技术的不足,提供一种硫掺杂铁酸钴催化剂的制备方法。
本发明采用的技术方案是依次包括如下步骤:
将50g黄铁矿粉碎至10~50目,加入20~30g纯碱,用搅拌机搅拌均匀,置于马弗炉中,在800~1000℃下煅烧2~4h,煅烧结束后,加入到100~200mL浓度为0.2~0.5mol/L的氢氧化钠溶液中,剧烈搅拌下,再加入市售有效氯的质量分数为10%的次氯酸钠15~35mL,持续剧烈搅拌2~3h,最后加入1~3g氯化钴,继续搅拌2~4h,固液分离,去除上清液,蒸馏水洗涤固体3~4次,105℃烘干,再置于马弗炉中450~650℃下煅烧4~5h,冷却到室温,即得到一种硫掺杂铁酸钴催化剂。
本发明的优点是:利用黄铁矿生成高铁酸盐,经过处理,得到硫掺杂铁酸钴催化剂,其中还有更多种微量的其他过度元素复合,催化效果大大提高。
具体实施方式
以下进一步提供本发明的3个实施例:
实施例1
将50g黄铁矿粉碎至50目,加入30g纯碱,用搅拌机搅拌均匀,置于马弗炉中,在1000℃下煅烧4h,煅烧结束后,加入到200mL浓度为0.5mol/L的氢氧化钠溶液中,剧烈搅拌下,再加入市售有效氯的质量分数为10%的次氯酸钠35mL,持续剧烈搅拌3h,最后加入3g氯化钴,继续搅拌4h,固液分离,去除上清液,蒸馏水洗涤固体4次,105℃烘干,再置于马弗炉中650℃下煅烧5h,冷却到室温,即得到一种硫掺杂铁酸钴催化剂。
0.5g硫掺杂铁酸钴催化剂加入到100mL浓度为18mg/L的苯酚废水中,在120W的LED灯照射下,反应120min,降解率为95.1%。
相比市售的铁酸钴,在同样的条件下,苯酚的去除率仅为21.4%。
实施例2
将50g黄铁矿粉碎至10目,加入20g纯碱,用搅拌机搅拌均匀,置于马弗炉中,在800℃下煅烧2h,煅烧结束后,加入到100mL浓度为0.2mol/L的氢氧化钠溶液中,剧烈搅拌下,再加入市售有效氯的质量分数为10%的次氯酸钠15mL,持续剧烈搅拌2h,最后加入1g氯化钴,继续搅拌2h,固液分离,去除上清液,蒸馏水洗涤固体3次,105℃烘干,再置于马弗炉中450℃下煅烧4h,冷却到室温,即得到一种硫掺杂铁酸钴催化剂。
0.5g硫掺杂铁酸钴催化剂加入到150mL浓度为15mg/L的亚甲基蓝废水中,在120W的LED灯照射下,反应90min,脱色率为95.2%。
实施例3
将50g黄铁矿粉碎至40目,加入25g纯碱,用搅拌机搅拌均匀,置于马弗炉中,在800℃下煅烧3h,煅烧结束后,加入到200mL浓度为0.4mol/L的氢氧化钠溶液中,剧烈搅拌下,再加入市售有效氯的质量分数为10%的次氯酸钠25mL,持续剧烈搅拌3h,最后加入3g氯化钴,继续搅拌4h,固液分离,去除上清液,蒸馏水洗涤固体4次,105℃烘干,再置于马弗炉中550℃下煅烧5h,冷却到室温,即得到一种硫掺杂铁酸钴催化剂。
0.5g硫掺杂铁酸钴催化剂加入到100mL浓度为18mg/L的罗丹明B废水中,在120W的LED灯照射下,反应90min,脱色率为97.9%。
Claims (1)
1.一种硫掺杂铁酸钴催化剂的制备方法,其特征是依次包括如下步骤:
将50g黄铁矿粉碎至10~50目,加入20~30g纯碱,用搅拌机搅拌均匀,置于马弗炉中,在800~1000℃下煅烧2~4h,煅烧结束后,加入到100~200mL浓度为0.2~0.5mol/L的氢氧化钠溶液中,剧烈搅拌下,再加入市售有效氯的质量分数为10%的次氯酸钠15~35mL,持续剧烈搅拌2~3h,最后加入1~3g氯化钴,继续搅拌2~4h,固液分离,去除上清液,蒸馏水洗涤固体3~4次,105℃烘干,再置于马弗炉中450~650℃下煅烧4~5h,冷却到室温,即得到一种硫掺杂铁酸钴催化剂。
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Citations (5)
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CN101073774A (zh) * | 2007-05-30 | 2007-11-21 | 北京科技大学 | 一种利用锡铁矿制备铁酸锌光催化材料的方法 |
CN101913680A (zh) * | 2010-08-07 | 2010-12-15 | 太原市恒远化工环保科技有限公司 | 磁稳流化床光催化反应器及其处理难降解有机废水的方法 |
CN102553595A (zh) * | 2011-12-22 | 2012-07-11 | 南京理工大学 | 一种纳米铁酸盐/碳纳米管复合材料的制备方法 |
CN103611577A (zh) * | 2013-12-17 | 2014-03-05 | 江南大学 | 一种高效降解有机染料废水的可见光催化剂及其制备方法 |
CN103990476A (zh) * | 2014-06-04 | 2014-08-20 | 常州大学 | 一种硫掺杂磷酸银催化剂的制备方法 |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101073774A (zh) * | 2007-05-30 | 2007-11-21 | 北京科技大学 | 一种利用锡铁矿制备铁酸锌光催化材料的方法 |
CN101913680A (zh) * | 2010-08-07 | 2010-12-15 | 太原市恒远化工环保科技有限公司 | 磁稳流化床光催化反应器及其处理难降解有机废水的方法 |
CN102553595A (zh) * | 2011-12-22 | 2012-07-11 | 南京理工大学 | 一种纳米铁酸盐/碳纳米管复合材料的制备方法 |
CN103611577A (zh) * | 2013-12-17 | 2014-03-05 | 江南大学 | 一种高效降解有机染料废水的可见光催化剂及其制备方法 |
CN103990476A (zh) * | 2014-06-04 | 2014-08-20 | 常州大学 | 一种硫掺杂磷酸银催化剂的制备方法 |
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