CN115193395A - 一种硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法及其应用 - Google Patents
一种硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法及其应用 Download PDFInfo
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- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052683 pyrite Inorganic materials 0.000 title claims abstract description 74
- 239000003463 adsorbent Substances 0.000 title claims abstract description 54
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 37
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Abstract
一种硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法及其应用，本发明是为了解决现有燃煤烟气中的汞难以处理的问题。制备方法：一、将干燥的粉煤灰按质量比为1：(8～12)浸入酸液或者碱液中，持续搅拌，然后对混合液抽滤收集过滤物，经过洗涤、干燥和研磨后，得到改性粉煤灰；二、将硫铁矿矿石粉碎、过筛网；三、按照质量比为(1～3)：(1～4)将改性粉煤灰和硫铁矿粉混合均匀，得到脱汞吸附剂。本发明硫铁矿和改性粉煤灰复合的脱汞吸附剂的应用是将硫铁矿和改性粉煤灰复合的脱汞吸附剂喷入烟道中对烟气中的汞进行脱除。本发明通过将改性后的粉煤灰与磨碎过筛之后的黄铁矿石混合，提高了吸附剂材料吸附烟气中汞的能力。
Description
技术领域
本发明属于脱汞吸附剂材料领域，特别涉及一种将硫铁矿和改性粉煤灰复合之后的高效脱燃煤电厂烟气中汞的吸附剂的制备方法及其应用。
背景技术
燃煤过程中排放的汞具有高毒性、不可降解性和生物积累性，因此汞会对人类健康和生态环境健康都产生长期危害。据报道，我国大气环境中较大一部分的汞来源于燃煤电厂的排放，约占总排放的31％。正因如此，燃煤电厂必须采取更严格的排放标准，汞的污染防治被认为是继颗粒物、二氧化硫、氮氧化物之后又一热门研究课题。
燃烧后脱汞技术是目前国内外研究的主流技术，因为该技术可以充分利用目前已有的、已研究较为成熟的脱硫、脱硝、除尘设备，只需对他们进行一定程度上的改进，就可以达到脱汞的目的。这样可以尽可能地降低脱汞工艺带来的电厂运营成本和对电厂其他装置的影响。
发明内容
本发明是为了解决现有燃煤烟气中的汞难以处理的问题，而提供一种硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法及其应用。
本发明硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法按照以下步骤实现：
一、将干燥的粉煤灰按质量比为1：(8～12)浸入酸液或者碱液中，持续搅拌，然后对混合液抽滤收集过滤物，用去离子水冲洗过滤物至呈中性，经过干燥和研磨后，得到改性粉煤灰；
二、将硫铁矿矿石用粉碎研磨机磨碎后过200目的筛网，得到硫铁矿粉；
三、按照质量比为(1～3)：(1～4)将改性粉煤灰和硫铁矿粉混合均匀，得到脱汞吸附剂。
本发明硫铁矿和改性粉煤灰复合的脱汞吸附剂的应用是将硫铁矿和改性粉煤灰复合的脱汞吸附剂喷入烟道中对烟气中的汞进行脱除。
粉煤灰价格低廉，容易获得，具有较好的比表面积和吸附能力，硫铁矿作为廉价矿石，其中含有大量的Fe和S元素，本发明提供了一种将改性粉煤灰和硫铁矿结合的高效脱汞吸附剂制备方法，该硫铁矿-改性粉煤灰的脱汞原理如下：
首先，Hg0被吸附在吸附剂的表面，
其次，Hg0和硫铁矿-改性粉煤灰中的活性组分FeS2反应，
最终大部分的汞以HgS的形式附着在复合吸附剂表面。
本发明的制备方法简单，工序简洁、所用的原材料易得廉价。通过将改性后的粉煤灰与磨碎过筛之后的黄铁矿石混合，提高了吸附剂材料吸附烟气中汞的能力。通过实验，本发明确定了最佳的改性粉煤灰与黄铁矿石粉末的混合比例，最佳的过筛目数以及改性粉煤灰所需酸的浓度大小等制备条件。最终在本发明最佳制备条件所制得的硫铁矿-改性粉煤灰吸附汞的效果较好，使得电厂脱汞更加简单，成本更低。
本发明提出了粉煤灰综合利用的新用途，为燃煤电厂提供了一种成本低廉，高效的脱汞吸附剂。
附图说明
图1是实施例1和实施例2所制备的酸碱改性粉煤灰脱汞效率对比图，其中◆代表酸改性粉煤灰，■代表碱改性粉煤灰；
图2是实施例3制备硫铁矿和改性粉煤灰复合的脱汞吸附剂的SEM表征图，其中左图放大500倍，右图放大2000倍；
图3是实施例4制备硫铁矿和改性粉煤灰复合的脱汞吸附剂的SEM表征图，其中左图放大500倍，右图放大2000倍；
图4是实施例5制备硫铁矿和改性粉煤灰复合的脱汞吸附剂的SEM表征图，其中左图放大500倍，右图放大2000倍；
图5是实施例6制备硫铁矿和改性粉煤灰复合的脱汞吸附剂的SEM表征图，其中左图放大500倍，右图放大2000倍；
图6是实施例3-6制备硫铁矿和改性粉煤灰复合的脱汞吸附剂的XRD表征图，其中1代表实施例5，2代表实施例3，3代表实施例4，4代表实施例6；
图7是实施例3-6制备硫铁矿和改性粉煤灰复合的脱汞吸附剂在反应条件相同时脱汞效率对比图。
具体实施方式
具体实施方式一：本实施方式硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法按照以下步骤实施：
一、将干燥的粉煤灰按质量比为1：(8～12)浸入酸液或者碱液中，持续搅拌，然后对混合液抽滤收集过滤物，用去离子水冲洗过滤物至呈中性，经过干燥和研磨后，得到改性粉煤灰；
二、将硫铁矿矿石用粉碎研磨机磨碎后过200目的筛网，得到硫铁矿粉；
三、按照质量比为(1～3)：(1～4)将改性粉煤灰和硫铁矿粉混合均匀，得到脱汞吸附剂。
具体实施方式二：本实施方式与具体实施方式一不同的是步骤一所述的酸液为1mol/L的硫酸，所述的碱液为1mol/L的氢氧化钠溶液。
具体实施方式三：本实施方式与具体实施方式二不同的是将干燥的粉煤灰按质量比为1：10浸入酸液或者碱液中。
具体实施方式四：本实施方式与具体实施方式一至三之一不同的是步骤一中在常温下持续搅拌30～50min。
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是步骤一中干燥的温度为110℃。
具体实施方式六：本实施方式与具体实施方式一至五之一不同的是步骤三中改性粉煤灰和硫铁矿粉过200目筛网。
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是步骤三中改性粉煤灰和硫铁矿粉的质量比为1：3～5。
具体实施方式八：本实施方式与具体实施方式七不同的是步骤三中改性粉煤灰和硫铁矿粉的质量比为1：4。
具体实施方式九：本实施方式硫铁矿和改性粉煤灰复合的脱汞吸附剂的应用是将硫铁矿和改性粉煤灰复合的脱汞吸附剂喷入烟道中对烟气中的汞进行脱除。
本实施方式在空气预热器之后，静电除尘器或布袋除尘器之前向烟道中喷入吸附剂对烟气汞进行脱除，脱汞吸附剂颗粒由静电除尘器或者布袋除尘器进行收集。
具体实施方式十：本实施方式与具体实施方式九不同的是烟道中的温度为120～180℃。
实施例1：本实施例酸改性粉煤灰的制备方法按照以下步骤实施：
将洗涤干净并在烘箱中干燥好过200目筛网的粉煤灰按质量比为1：10浸入1mol/L的硫酸溶液中，在常温下搅拌30min，然后对混合液抽滤收集过滤物，用去离子水冲洗过滤物至呈中性，放入110℃的烘箱中干燥3h，干燥后研细，得到酸改性粉煤灰。
实施例2：本实施例碱改性粉煤灰的制备方法按照以下步骤实施：
将洗涤干净并在烘箱中干燥好过200目筛网的粉煤灰按质量比为1：10浸入1mol/L的氢氧化钠溶液中，在常温下搅拌30min，然后对混合液抽滤收集过滤物，用去离子水冲洗过滤物至呈中性，放入110℃的烘箱中干燥3h，干燥后研细，得到碱改性粉煤灰。
由图1中所示的结果可知，通过实施例1和实施例2所制备的酸改性粉煤灰和碱改性粉煤灰中酸改性粉煤灰脱汞的效率较高。
实施例3：本实施例硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法按照以下步骤实施：
一、将洗涤干净并在烘箱中干燥好过200目筛网的粉煤灰按质量比为1：10浸入1mol/L的硫酸溶液中，在常温下搅拌30min，然后对混合液抽滤收集过滤物，用去离子水冲洗过滤物至呈中性，放入110℃的烘箱中干燥3h，干燥后研细，得到酸改性粉煤灰；
二、将硫铁矿矿石用粉碎研磨机磨碎后过200目的筛网，得到硫铁矿粉；
三、按照质量比为1：4将改性粉煤灰和硫铁矿粉混合均匀，得到脱汞吸附剂。
脱汞实验过程：汞蒸汽由U型管中的汞渗透管发出，将U型管置于水浴锅中。当外界温度恒定时，U型管中的汞达到汽液平衡，汞蒸汽以一定的速率稳定逸散出来，再由N2吹至气路中，气路连接固定床反应器(由石英反应管和温控伴热带组成)。石英反应管(D:20mm，L:120mm)水平放置于实验台上，外壁缠绕温控伴热带和热电偶，确保热电偶不与空气接触。反应器中的吸附剂由上下两层玻璃棉夹着放置，本实验采用KMnO4/H2SO4吸收法测经过吸附剂后汞的浓度，通过QM201测汞仪测定样品中的汞离子浓度，为确保实验准确性，样品每次实验完就立刻检测其汞浓度。为保证实验的安全与环保，实验最终尾气在通过第一个酸性高锰酸钾吸收瓶后需要再通过活性炭吸附处理，最后被通风橱排至大气中。
经实验，实施例3制备的硫铁矿和改性粉煤灰复合的脱汞吸附剂的脱汞(效)率为91.92％。
实施例4：本实施例与实施例3不同的是按照质量比为1：2将改性粉煤灰和硫铁矿粉混合均匀。
本实施例制备的硫铁矿和改性粉煤灰复合的脱汞吸附剂的脱汞效率为91.38％。
实施例5：本实施例与实施例3不同的是按照质量比为1：1将改性粉煤灰和硫铁矿粉混合均匀。
本实施例制备的硫铁矿和改性粉煤灰复合的脱汞吸附剂的脱汞效率为84.70％。
实施例6：本实施例与实施例3不同的是按照质量比为3：1将改性粉煤灰和硫铁矿粉混合均匀。
本实施例制备的硫铁矿和改性粉煤灰复合的脱汞吸附剂的脱汞效率为70.89％。
由图2-5可知，在酸改性粉煤灰的掺杂下，×500的SEM图像显示与掺杂前相比，吸附剂颗粒物间的孔隙增加，孔洞直径增大，颗粒物多为块状和球型。×2000倍下的SEM图像显示酸改性粉煤灰的颗粒表面附着了些许硫铁矿颗粒。20wt％掺杂比下的吸附剂只有少数颗粒物为球型，这也与掺杂比相符。颗粒物间的孔隙更大，推挤也更为松散。×2000倍下的SEM图像显示，相比于50wt％的掺杂比，20wt％掺杂比下的酸改性粉煤灰颗粒物的表面吸附了更多的絮状物和硫铁矿粉末。33.3wt％掺杂比下的吸附剂的孔隙没有20wt％掺杂比中的大，但该吸附剂颗粒表面吸附了最多的颗粒物和硫铁矿。掺杂75wt％酸改性粉煤灰的吸附剂的颗粒物多为球型，颗粒物间孔隙较大，少数颗粒物表面吸附有硫铁矿颗粒。
下表1为不同酸改性粉煤灰掺杂比条件下吸附剂的比表面积测试结果：
表1
上述比表面测试结果结合图7的脱汞效率结果可知，酸改性粉煤灰与硫铁矿掺杂可提高硫铁矿的比表面积和孔隙体积从而提高其脱汞效率，但是并非掺杂比越高，比表面提升越大，脱汞效率最佳，酸改性粉煤灰的最佳掺杂比为20wt％。
本发明采用X射线衍射仪对硫铁矿-改性粉煤灰吸附剂的晶型进行测试，测试结果如下图6所示。由图可知，该吸附剂的主要衍射峰为莫来石和FeS2。两种物质的衍射峰的高度和多少随着改性粉煤灰占比的变化而变化，与实际相符。
Claims (10)
1.硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于该制备方法按照以下步骤实现：
一、将干燥的粉煤灰按质量比为1：(8～12)浸入酸液或者碱液中，持续搅拌，然后对混合液抽滤收集过滤物，用去离子水冲洗过滤物至呈中性，经过干燥和研磨后，得到改性粉煤灰；
二、将硫铁矿矿石用粉碎研磨机磨碎后过200目的筛网，得到硫铁矿粉；
三、按照质量比为(1～3)：(1～4)将改性粉煤灰和硫铁矿粉混合均匀，得到脱汞吸附剂。
2.根据权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于步骤一所述的酸液为1mol/L的硫酸，所述的碱液为1mol/L的氢氧化钠溶液。
3.根据权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于将干燥的粉煤灰按质量比为1：10浸入酸液或者碱液中。
4.根据权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于步骤一中在常温下持续搅拌30～50min。
5.根据权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于步骤一中干燥的温度为110℃。
6.根据权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于步骤三中改性粉煤灰和硫铁矿粉过200目筛网。
7.根据权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于步骤三中改性粉煤灰和硫铁矿粉的质量比为1：3～5。
8.根据权利要求7所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的制备方法，其特征在于步骤三中改性粉煤灰和硫铁矿粉的质量比为1：4。
9.如权利要求1所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的应用，其特征在于将硫铁矿和改性粉煤灰复合的脱汞吸附剂喷入烟道中对烟气中的汞进行脱除。
10.根据权利要求9所述的硫铁矿和改性粉煤灰复合的脱汞吸附剂的应用，其特征在于烟道中的温度为120～180℃。
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