CN111389347B - 一种废水除氟吸附剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种废水除氟吸附剂及其制备方法,所述吸附剂包括:拜耳法赤泥、粉煤灰、CaO;拜耳法赤泥与粉煤灰质量比为1:5‑1:2,CaO的加入量为经柠檬酸改性的拜耳法赤泥和粉煤灰混合物重量的5%‑20%。本发明公开的废水除氟吸附剂的制备方法,包括:先将拜耳法赤泥与粉煤灰按上述质量比混合均匀,将得到混合物进行酸改性后,经过滤得到的滤饼中配入CaO,再次混合均匀后,进行高温固相改性后,冷却至室温,得到吸附剂。本发明可使废水除氟吸附剂的比表面积达到17.00m2/g以上,适用于任何氟含量、任何pH值的含氟废水除氟治理,对废水中氟的去除率在1h时可达到99.0%以上。
Description
技术领域
本发明涉及除氟吸附剂技术领域,具体涉及一种废水除氟吸附剂及其制备方法。
背景技术
吸附法除氟是目前应用最广泛的含氟废水除氟方法。常用的吸附剂有活性氧化铝、沸石、骨炭等。近年来研究者们趋向于将工农业废弃物如砖粉、赤泥、铝酸钙矿渣、漂白土、竹炭、稻草、果壳及树皮制活性炭等用作水处理除氟吸附剂。李建萍等将取自电厂的粉煤灰经200目筛后,在300℃下烘3h。直接用于除氟。结果表明,其对F-质量浓度<500mg/L的含氟废水具有很好的脱氟效果。薛金凤等用50%粉煤灰,48%黏土和2%无机造孔剂在900℃下烧制2h,制得比表面积为15.91m2/g的除氟滤料。Y.Cengeloglu等将从工厂收集而来的碱性赤泥,用水彻底冲洗直至呈现中性,然后用20%的盐酸处理活化,经过滤、反复冲洗、干燥后用于处理含氟水,除氟率可达85%。陈涛等利用废弃羊骨制成的骨炭吸附剂具有再生容易、使用寿命长的特点,处理含氟地下水效果令人满意。梁丽珍等利用城市建筑垃圾(主成分为废砖)为主要原料制得改性废砖,研究发现在pH=1~3时改性废砖对F-的吸附效果很好。专利201710724164.2,将废渣赤泥焙烧,得到焙烧产物,再将焙烧产物用硫酸进行酸浸,得到改性赤泥,对废水中氟的去除率在1h时即可达到99%以上。专利201610209508.1采用水热法,以白云石和粉煤灰为原料,合成除氟用钙基吸附剂,可以在低pH条件下有效吸附氟污染物。
目前来看,单一的吸附材料吸附容量都不大,存在较多的缺陷和局限性,无法满足水污染治理的要求。通过不同吸附材料的复合,实现不同复合材料之间的优势互补,是发展趋势。在各种材料复合之前一般会采用酸浸改性提升材料的活性,常用的是硫酸、盐酸、硝酸中一种或几种的混合物,这几种酸均很不容易被自然环境降解,给后续吸附剂的使用和酸浸废水的处理带来了困难。
此外,一般的除氟吸附剂均具有特定的使用条件如特定pH、特定的废水浓度范围等,在废水处理方面具有加大局限性。
发明内容
针对上述已有技术存在的不足,本发明提供一种以柠檬酸改性多种工业固废制备的废水除氟吸附剂及其方法。
本发明是通过以下技术方案实现的。
一种废水除氟吸附剂,其特征在于,所述吸附剂包括:拜耳法赤泥、粉煤灰、CaO;所述拜耳法赤泥与粉煤灰质量比为1:5-1:2,所述CaO的加入量为经柠檬酸改性的拜耳法赤泥和粉煤灰混合物重量的5%-20%。
进一步地,所述拜耳法赤泥、粉煤灰混合后采用浓度按质量百分比计为20%-40%柠檬酸溶液进行改性。
一种废水除氟吸附剂的制备方法,其特征在于,所述方法包括:先将拜耳法赤泥与粉煤灰按上述质量比混合均匀,将得到的混合物经柠檬酸进行酸改性后配入CaO,再次混合均匀后,进行高温固相改性后,冷却至室温,得到吸附剂。
进一步地,所述酸改性条件为:采用浓度为20%-40%的柠檬酸溶液浸渍拜耳法赤泥与粉煤灰的混合物,浸渍时间为12h-14h,浸渍温度为40℃-60℃,所述柠檬酸溶液的加入质量是拜尔法赤泥与粉煤灰质量之和的10-30倍。
进一步地,所述CaO的加入量为经柠檬酸改性的拜耳法赤泥和粉煤灰混合物重量的5%-20%。
进一步地,所述高温固相改性具体为:在600℃-850℃条件下,在马弗炉中高温焙烧6h-8h。
进一步地,对混合物酸改性后进行过滤,并用去离子水反复冲洗滤饼,直至洗液呈中性。
进一步地,冲洗后的滤饼在80℃条件下烘干至恒重。
进一步地,经烘干至恒重的滤饼经研磨后过200目标准筛,取筛下物后配入CaO。
本发明的有益技术效果,本发明利用工业固废赤泥和粉煤灰(燃煤电厂或锅炉)及价廉易得的石灰作为除氟吸附剂制备的原料,一方面可减少工业固废处理处置过程带来的环境压力,另一方面利用工业固废中的有用成分用于废水除氟,可达到废治废的目的。以柠檬酸作为酸改性试剂,使得吸附剂制备过程更加绿色环保。同时,本发明所述的一种废水除氟吸附剂可用于各种浓度的含氟废水治理,可在各种pH条件下使用,具有广泛的适用性。本发明可使废水除氟吸附剂的比表面积达到17.00m2/g以上,适用于任何氟含量、任何pH值的含氟废水除氟治理,对废水中氟的去除率在1h时可达到99.0%以上。
附图说明
图1为本发明的一种废水除氟吸附剂的制备流程示意图。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
一种废水除氟吸附剂制备方法,用拜耳法赤泥、粉煤灰及CaO作为原料,先将拜耳法赤泥与粉煤灰按质量比1:5-1:2的比例混合均匀后,对其进行酸改性,改性条件为:采用浓度为20%-40%柠檬酸溶液浸渍拜耳法赤泥与粉煤灰的混合物,浸渍时间为12h-14h,浸渍温度为40℃-60℃,浸渍时柠檬酸溶液加入质量与拜耳法赤泥和粉煤灰质量之和的比例为10:1-30:1。酸改性后过滤,并用去离子水反复冲洗滤饼,直至洗液呈中性,在80℃条件下烘干至恒重,研磨后过200目标准筛,取筛下物配入筛下物总重5%-20%的CaO,再次混合均匀后,在600℃-850℃条件下,在马弗炉中高温焙烧6h-8h,进行高温固相改性,改性后冷却至室温即可制得所述的一种废水除氟吸附剂。
实施例1
用拜耳法赤泥、燃煤电厂的粉煤灰及CaO作为原料,先将拜耳法赤泥与燃煤电厂粉煤灰按1:5的比例混合均匀,用浓度为20%柠檬酸,在液固比为10:1条件下,40℃浸渍12h,过滤,用去离子水反复冲洗滤饼至洗液呈中性,在80℃条件下烘干至恒重,研磨后过200目标准筛,取筛下物配入筛下物总重5%的CaO,再次混合均匀后,在600℃条件下,在马弗炉中高温焙烧6h,进行高温固相改性,改性后冷却至室温即可制得所述的一种废水除氟吸附剂,比表面积为18.20m2/g。用该吸附剂处理含氟废水(氟离子浓度2000mg/L,pH=2),氟离子去除率1h可达99.5%。
实施例2
用拜耳法赤泥、燃煤电厂粉煤灰及CaO作为原料,先将拜耳法赤泥与燃煤电厂粉煤灰按1:3的比例混合均匀,用浓度为30%柠檬酸,在液固比为20:1条件下,50℃浸渍12h,过滤,用去离子水反复冲洗滤饼至洗液呈中性,在80℃条件下烘干至恒重,研磨后过200目标准筛,取筛下物配入筛下物总重10%的CaO,再次混合均匀后,在700℃条件下,在马弗炉中高温焙烧7h,进行高温固相改性,改性后冷却至室温即可制得所述的一种废水除氟吸附剂,比表面积为17.42m2/g。用该吸附剂处理含氟废水(氟离子浓度900mg/L,pH=7),氟离子去除率1h可达99.3%。
实施例3
用拜耳法赤泥、燃煤电厂粉煤灰及CaO作为原料,先将拜耳法赤泥与燃煤电厂粉煤灰按1:2的比例混合均匀,用浓度为40%柠檬酸,在液固比为30:1条件下,60℃浸渍12h,过滤,用去离子水反复冲洗滤饼至洗液呈中性,在80℃条件下烘干至恒重,研磨后过200目标准筛,取筛下物配入筛下物总重20%的CaO,再次混合均匀后,在850℃条件下,在马弗炉中高温焙烧8h,进行高温固相改性,改性后冷却至室温即可制得所述的一种废水除氟吸附剂,比表面积为17.02m2/g。用该吸附剂处理含氟废水(氟离子浓度50mg/L,pH=12),氟离子去除率1h可达99.1%。
实施例4
用拜耳法赤泥、燃煤电厂粉煤灰及CaO作为原料,先将拜耳法赤泥与燃煤电厂粉煤灰按1:4的比例混合均匀,用浓度为35%柠檬酸,在液固比为25:1条件下,55℃浸渍14h,过滤,用去离子水反复冲洗滤饼至洗液呈中性,在80℃条件下烘干至恒重,研磨后过200目标准筛,取筛下物配入筛下物总重15%的CaO,再次混合均匀后,在800℃条件下,在马弗炉中高温焙烧7h,进行高温固相改性,改性后冷却至室温即可制得所述的一种废水除氟吸附剂,比表面积为17.55m2/g。用该吸附剂处理含氟废水(氟离子浓度50mg/L,pH=12),氟离子去除率1h可达99.4%。
以上所述的仅是本发明的较佳实施例,并不局限发明。应当指出对于本领域的普通技术人员来说,在本发明所提供的技术启示下,还可以做出其它等同改进,均可以实现本发明的目的,都应视为本发明的保护范围。
Claims (6)
1.一种废水除氟吸附剂的制备方法,其特征在于,所述吸附剂原料包括:拜耳法赤泥、粉煤灰、CaO;所述方法包括:先将拜耳法赤泥与粉煤灰按质量比1:5-1:2混合均匀,将得到的混合物经浓度按质量百分比计为20%-40%柠檬酸进行酸改性后配入CaO,所述CaO的加入量为经柠檬酸改性的拜耳法赤泥和粉煤灰混合物重量的5%-20%,再次混合均匀后,进行高温固相改性后,所述高温固相改性具体为:在600℃-850℃条件下,在马弗炉中高温焙烧6h-8h,冷却至室温,得到吸附剂。
2.根据权利要求1所述的制备方法,其特征在于,所述酸改性条件为:采用浓度为20%-40%的柠檬酸溶液浸渍拜耳法赤泥与粉煤灰的混合物,浸渍时间为12h -14h,浸渍温度为40℃-60℃,所述柠檬酸溶液的加入质量是拜尔法赤泥与粉煤灰质量之和的10-30倍。
3.根据权利要求1所述的制备方法,其特征在于,所述CaO的加入量为经柠檬酸改性的拜耳法赤泥和粉煤灰混合物重量的5%-20%。
4.根据权利要求1所述的制备方法,其特征在于,对混合物酸改性后进行过滤,并用去离子水反复冲洗滤饼,直至洗液呈中性。
5.根据权利要求4所述的制备方法,其特征在于,冲洗后的滤饼在80℃条件下烘干至恒重。
6.根据权利要求5所述的制备方法,其特征在于,经烘干至恒重的滤饼经研磨后过200目标准筛,取筛下物后配入CaO。
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