CN110013830A - 一种铁铝复合骨炭除氟剂的制备方法及制得的除氟剂 - Google Patents
一种铁铝复合骨炭除氟剂的制备方法及制得的除氟剂 Download PDFInfo
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Abstract
本发明提供一种铁铝复合骨炭除氟剂的制备方法及制得的除氟剂,该制备方法包括如下步骤:(1)将畜骨表面洗净,在400‑450℃炭化1.5‑2h而得骨炭;(2)将步骤(1)中获得的骨炭冷却后研磨过筛,水洗后烘干得到骨炭粒;(3)将步骤(2)中获得的骨炭粒按固液比1:2.5‑1:10在质量百分比浓度为2‑8%的Fe2(SO4)3溶液中浸泡0.3‑0.7 h,水洗后烘干,然后按1:3‑1:8的固液比在质量百分比浓度为3‑10%的Al2(SO4)3溶液中浸泡0.5‑1.5h,水洗后烘干,得到Al2(SO4)3‑Fe2(SO4)3复合骨炭除氟剂。本发明的铁铝复合骨炭除氟剂吸附容量是未负载铁铝离子时的吸附容量的8.5倍,除氟效果佳。
Description
技术领域
本发明属于地下水除氟技术领域,具体涉及一种铁铝复合骨炭除氟剂的制备方法及制得的除氟剂。
背景技术
国家饮用水标准(GB5749-2006)中规定饮用水中氟最大浓度必须低于1.0 mg/L,如果长期饮用氟离子浓度超标的地下水,容易导致氟斑牙和氟骨症。由此可见,长期引用氟超标的地下水,将严重影响人体健康,为此,去除饮用水中的氟具有重要的意义。
目前去除地下水中氟的技术有吸附法、膜分离、离子交换、电渗析、絮凝等,其中,膜分离技术能有效地去除氟,但设备投资和运行成本均过高,且管理复杂,难以在实践中,特别是农村大规模的推广应用。离子交换能够去除氟,但当地下水中伴有其他阴离子如NO3-、SO4 3-、PO4 3-、Cl-等共存离子时,将降低氟的去除效果。絮凝也能有效地去除氟,但需要大量的絮凝剂,从而增加了药剂的处理费用,另外絮凝处理产生的沉淀还需过滤处理,这也增加了该工艺的处理单元和费用。吸附方法是通过吸附剂对氟的吸附作用而去除氟,吸附法具有运行管理方便,无需投加药剂等优点,而被广泛应用。
专利文献(公开号为CN101596446A)中公开了负载铝离子的骨炭除氟剂的制备方法,该方法得到的骨炭除氟剂吸附容量得到了提高,但提高幅度小,仅比一般骨炭高60%以上。因而需要吸附容量更高的骨炭除氟剂。
发明内容
本发明为了解决以往骨炭除氟剂吸附容量小的问题,而提供一种铁铝复合骨炭除氟剂的制备方法和制得的铁铝复合骨炭除氟剂。
本发明所述铁铝复合骨炭除氟剂的制备方法,包括如下步骤:
(1)将畜骨表面洗净,在400-450℃炭化1.5-2h而得骨炭;
(2)将步骤(1)中获得的骨炭冷却后研磨过筛,水洗后烘干得到骨炭粒;
(3)将步骤(2)中获得的骨炭粒按固液比1:2.5-1:10在质量百分比浓度为2-8%的Fe2(SO4)3溶液中浸泡0.3-0.7h,水洗后烘干,然后按1:3-1:8的固液比在质量百分比浓度为3-10%的Al2(SO4)3溶液中浸泡0.5-1.5h,水洗后烘干,得到Al2(SO4)3-Fe2(SO4)3复合骨炭除氟剂。
进一步地,所述畜骨为兽骨,优选牛骨。
进一步地,过筛的筛网的目数为10-80目,过筛的粒子对应的粒径为0.2~2mm。
进一步地,所述步骤(2)、步骤(3)中,水洗使用去离子水,水洗至pH显中性。
进一步地,所述步骤(2)、步骤(3)中,烘干使用烘箱进行,烘干的温度为100℃。
本发明还提供一种铁铝复合骨炭除氟剂,其使用所述铁铝复合骨炭除氟剂的制备方法制得。
有益效果:本发明通过在骨炭上负载铝离子和铁离子,使得骨炭除氟剂对氟的吸附容量是一般未负载铝铁离子的骨炭的8.5倍,除氟能力显著增强;一次、二次、三次再生效率分别为94.5%、90.4%和86.5%,循环使用性高。
附图说明
图1为本发明实施例1的铁铝复合骨炭除氟剂与其他牛骨炭的吸附平衡图。
具体实施方式
下面通过实施例对本发明技术方案进行详细说明,但是本发明的保护范围不局限于所述实施例。
实施例1
将洗净的牛骨900g放入马弗炉(箱式电阻炉SX-5-12,天津泰斯特有限公司)中,在450℃炭化2h而得骨炭。将骨炭冷却至室温后,使用研磨机(天津泰斯特,FW100研磨机)磨碎通过目数为80目(粒径约0.2mm)的筛网,再用去离子水清洗至水澄清,在100℃的烘箱(上海精宏,DHG-9030A 9070A,电热恒温鼓风干燥箱,以下相同)中烘干得到骨炭粒(未改性骨炭)。
将骨炭粒(未改性骨炭)50g加入250ml质量百分比浓度为4%的Fe2(SO4)3溶液中浸泡0.5h,用去离子水洗至pH显中性,在100℃的烘箱中烘干得到Fe2(SO4)3改性牛骨炭。然后将Fe2(SO4)3改性牛骨炭50g加入250ml质量百分比浓度为8%的Al2(SO4)3溶液中浸泡1h,用去离子水洗至pH显中性,在100℃烘箱中烘干,得到Al2(SO4)3-Fe2(SO4)3-牛骨炭1。
实施例2
将洗净的牛骨900g放入马弗炉中,在450℃炭化2h而得骨炭。将骨炭冷却后,使用研磨机磨碎通过目数为80目(粒径约0.2mm)的筛网,再用去离子水清洗至水澄清,在100℃烘箱中烘干得到骨炭粒(未改性骨炭)。
将骨炭粒(未改性骨炭)50g加入150ml质量百分比浓度为8%的Fe2(SO4)3溶液中浸泡0.3h,用去离子水洗至pH显中性,在100℃烘箱中烘干得到Fe2(SO4)3改性牛骨炭。然后将Fe2(SO4)3改性牛骨炭50g加入200ml质量百分比浓度为10%的Al2(SO4)3溶液中浸泡0.5h,用去离子水洗至pH显中性,在100℃烘箱中烘干,得到Al2(SO4)3-Fe2(SO4)3-牛骨炭2。
实施例3
将洗净的牛骨900g放入马弗炉中,在450℃炭化2h而得骨炭。将骨炭冷却后,使用研磨机磨碎通过目数为10目(粒径约2mm)的筛网,再用去离子水清洗至水澄清,在100℃烘箱中烘干得到骨炭粒(未改性骨炭)。
将骨炭粒(未改性骨炭)50g加入450ml质量百分比浓度为2%的Fe2(SO4)3溶液中浸泡0.7h,用去离子水洗至pH显中性,在100℃烘箱中烘干得到Fe2(SO4)3改性牛骨炭。然后将Fe2(SO4)3改性牛骨炭50g加入350ml质量百分比浓度为3%的Al2(SO4)3溶液中浸泡1.5h,用去离子水洗至pH显中性,在100℃烘箱中烘干,得到Al2(SO4)3-Fe2(SO4)3-牛骨炭3。
对比例1
将牛骨900g放入马弗炉中,在450℃炭化2h而得骨炭。将骨炭冷却后,使用研磨机磨碎通过目数为80目(粒径约0.2mm)的筛网,再用去离子水清洗至水澄清,在100℃烘箱中烘干得到骨炭粒(未改性骨炭)。
对比例2
将上述骨炭粒(未改性骨炭)50g加入250ml质量百分比浓度为4%的Fe2(SO4)3溶液中浸泡0.5h,用去离子水洗至pH显中性,在100℃烘箱中烘干得到Fe2(SO4)3改性牛骨炭。
对比例3
将上述骨炭粒(未改性骨炭)50g加入250mL质量百分比浓度为8%的Al2(SO4)3溶液中浸泡1h,用去离子水洗至pH显中性,在100℃烘箱中烘干,得到Al2(SO4)3改性牛骨炭。
吸附容量测定
取未改性牛骨炭0.5g、Fe2(SO4)3改性牛骨炭0.5g、Al2(SO4)3改性牛骨炭0.5g和0.5g的Al2(SO4)3-Fe2(SO4)3-牛骨炭1、2、3,分别浸泡在初始浓度为60mg/L、120mg/L、180mg/L、240mg/L、300mg/L的氟化钠溶液40mL中,在24h后测定溶液浓度,并计算吸附量。通过Langmuir方程模拟不同牛骨炭对氟的吸附过程,得到不同牛骨炭对氟的最大吸附量(吸附容量)如表1所示,由表1可知,Al2(SO4)3-Fe2(SO4)3-牛骨炭1、2、3中,Al2(SO4)3-Fe2(SO4)3-牛骨炭1的吸附容量最大,且三者均高于未改性牛骨炭、Fe2(SO4)3改性牛骨炭和Al2(SO4)3改性牛骨炭的吸附容量。其中Al2(SO4)3-Fe2(SO4)3-牛骨炭1对氟的吸附容量为45.5mg•g-1,是未改性牛骨炭的8.5倍。
表1 不同牛骨炭对氟的吸附容量
种类 | 吸附容量mg•g<sup>-1</sup> |
未改性牛骨炭 | 5.3 |
Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-牛骨炭 | 13.3 |
Al<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-牛骨炭 | 34.5 |
Al<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-牛骨炭1 | 45.5 |
Al<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-牛骨炭2 | 43.7 |
Al<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>-牛骨炭3 | 42.8 |
吸附平衡
取未改性牛骨炭0.5g、Fe2(SO4)3改性牛骨炭0.5g、Al2(SO4)3改性牛骨炭0.5g和0.5g的Al2(SO4)3-Fe2(SO4)3-牛骨炭1,分别浸泡在初始浓度为17mg/L的氟化钠溶液中,测定吸附容量趋于稳定所需要的时间。结果如图1所示。根据图1可知,4种牛骨炭对氟的吸附容量逐渐增大,10h后吸附逐渐趋于平衡。其中未改性牛骨炭和Fe2(SO4)3-牛骨炭吸附8h左右就基本达到平衡状态,而Al2(SO4)3-牛骨炭和Al2(SO4)3-Fe2(SO4)3-牛骨炭1达到吸附平衡的时间较长,这也意味着吸附容量会更大,在达到吸附平衡时,Al2(SO4)3-Fe2(SO4)3-牛骨炭1的吸附容量最大。
Al2(SO4)3-Fe2(SO4)3-牛骨炭1的再生
再生方法如下:将5g的Al2(SO4)3-Fe2(SO4)3-牛骨炭1在饱和吸附后在150ml质量百分比浓度为1%的NaOH溶液中浸泡9h后,用滤纸(双圈定性滤纸,通用电气生物科技有限公司)过滤,将滤纸上的Al2(SO4)3-Fe2(SO4)3-牛骨炭1放入100ml烧瓶中,并加入20ml去离子水,然后用0.05mol·L-1盐酸调节溶液至pH显中性。将Al2(SO4)3-Fe2(SO4)3-牛骨炭1在中性溶液中浸泡0.5h后过滤,放入烧杯中用去离子水清洗,然后在100℃烘箱中烘干后,得到再生的Al2(SO4)3-Fe2(SO4)3-牛骨炭1。
再生效率测定
按上述再生方法进行再生,其中取质量百分比浓度为0.5%、1%、1.5%、2%、3%、4%、5%的NaOH溶液100ml进行再生,再生后得到不同浓度NaOH再生的Al2(SO4)3-Fe2(SO4)3-牛骨炭1,然后测定再生后的吸附容量,将结果表示于下表2。
表2 经不同浓度NaOH再生的再生效率
NaOH浓度/% | 再生前吸附容量/ mg·g<sup>-1</sup> | 再生后吸附容量/ mg·g<sup>-1</sup> | 再生效率/% |
0.5% | 13.148 | 12.18537 | 92.7 |
1% | 13.148 | 12.41907 | 94.5 |
1.5% | 13.148 | 12.43462 | 94.6 |
2% | 13.148 | 12.43764 | 94.6 |
3% | 13.148 | 12.46046 | 94.8 |
4% | 13.148 | 12.45806 | 94.8 |
5% | 13.148 | 12.47781 | 94.9 |
由表2可知,在1%~5%浓度的范围内NaOH溶液对再生骨炭吸附氟的量影响比较小,且再生效率均为94.5%以上。
固液比对骨炭再生效率的影响
按上述再生方法进行再生,其中取5g的Al2(SO4)3-Fe2(SO4)3-牛骨炭1按固液比为1:20、1:30、1:40、1:50在质量百分比浓度为1%的NaOH溶液中进行再生,再生后得到不同固液比条件下的Al2(SO4)3-Fe2(SO4)3-牛骨炭1,然后测定再生后的吸附容量,将结果表示于下表3。
表3 固液比对骨炭再生效率的影响
固液比 | 再生前吸附容量/ mg·g<sup>-1</sup> | 再生后吸附容量/ mg·g<sup>-1</sup> | 再生效率/% |
1:20 | 13.148 | 12.15337 | 92.4 |
1:30 | 13.148 | 12.49974 | 95.1 |
1:40 | 13.148 | 12.53971 | 95.4 |
1:50 | 13.148 | 12.54252 | 95.4 |
由表3可知,随着再生液用量的增加,再生后Al2(SO4)3-Fe2(SO4)3-牛骨炭1的再生效率呈上升趋势。考虑实际应用中的经济因素,优选Al2(SO4)3-Fe2(SO4)3-牛骨炭1与NaOH溶液的固液比为1∶30。
二次、三次再生效率的测定
按照上述再生方法,将一次再生的Al2(SO4)3-Fe2(SO4)3-牛骨炭1在饱和吸附后进行再生,得到二次再生的Al2(SO4)3-Fe2(SO4)3-牛骨炭1,按照同样的方式得到三次再生的Al2(SO4)3-Fe2(SO4)3-牛骨炭1,然后测定二次、三次再生后的吸附容量,所得结果如表4所示。
表4 三次再生的再生效率
再生次数 | 再生前吸附容量/ mg·g<sup>-1</sup> | 再生后吸附容量/ mg·g<sup>-1</sup> | 再生效率/% |
1 | 13.15 | 12.50 | 95.10 |
2 | 13.15 | 11.89 | 90.42 |
3 | 13.15 | 11.38 | 86.54 |
如表4所示,Al2(SO4)3-Fe2(SO4)3-牛骨炭1在最佳再生条件下,再生后的吸附容量为12.50mg·g-1,可达到原先吸附容量的95.10%,且经过第二次和第三次再生后的吸附容量仍然能够达到原先吸附容量的90.42%和86.54%,实验结果表明Al2(SO4)3-Fe2(SO4)3-牛骨炭具有良好的可再生性,是一种可以实际应用的除氟材料。
如上所述,尽管参照特定的优选实施例已经表示和表述了本发明,但其不得解释为对本发明自身的限制。在不脱离所附权利要求定义的本发明的精神和范围前提下,可对其在形式上和细节上作出各种变化。
Claims (6)
1.一种铁铝复合骨炭除氟剂的制备方法,其特征在于,包括如下步骤:
(1)将畜骨表面洗净,在400-450℃炭化1.5-2h而得骨炭;
(2)将步骤(1)中获得的骨炭冷却后研磨过筛,水洗后烘干得到骨炭粒;
(3)将步骤(2)中获得的骨炭粒按固液比1:2.5-1:10在质量百分比浓度为2-8%的Fe2(SO4)3溶液中浸泡0.3-0.7 h,水洗后烘干,然后按1:3-1:8的固液比在质量百分比浓度为3-10%的Al2(SO4)3溶液中浸泡0.5-1.5h,水洗后烘干,得到Al2(SO4)3-Fe2(SO4)3复合骨炭除氟剂。
2.根据权利要求1所述的铁铝复合骨炭除氟剂的制备方法,其特征在于,步骤(1)中,所述畜骨为兽骨。
3.根据权利要求1所述的铁铝复合骨炭除氟剂的制备方法,其特征在于,步骤(2)中,过筛的筛网的目数为10-80目。
4.根据权利要求1所述的铁铝复合骨炭除氟剂的制备方法,其特征在于,所述步骤(2)、步骤(3)中,水洗使用去离子水,水洗至pH显中性。
5.根据权利要求1所述的铁铝复合骨炭除氟剂的制备方法,其特征在于,所述步骤(2)、步骤(3)中,烘干使用烘箱进行,烘干的温度为100℃。
6.一种铁铝复合骨炭除氟剂,其特征在于,使用权利要求1至5中任一项所述的铁铝复合骨炭除氟剂的制备方法制得。
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