CN112792099A - 一种飞灰中污染物的去除及资源化方法 - Google Patents
一种飞灰中污染物的去除及资源化方法 Download PDFInfo
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- CN112792099A CN112792099A CN202011600066.6A CN202011600066A CN112792099A CN 112792099 A CN112792099 A CN 112792099A CN 202011600066 A CN202011600066 A CN 202011600066A CN 112792099 A CN112792099 A CN 112792099A
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- fly ash
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Abstract
本发明提供了一种可在高盐和高氯水体中同步高效去除有机污染物和重金属离子的电化学氧化还原系统，并以此为基础形成整套高效飞灰资源化回收的方法，属于环境污染控制工程技术领域。本发明方法中结合淬火法(制备中间层)和等离子喷涂法(制备超薄催化层)制备具有钌‑铱中间层的Ti4O7阳极，与哈氏合金电极(阴极)构建电化学氧化还原体系，可在高盐和高氯环境下降解矿化飞灰水洗液中的二噁英等有机污染物，并在阴极通过还原作用固定重金属离子，达到降低水洗液TOC和重金属含量的目的。该方法中涉及电极制备方法简便、成本低廉、易于规模化生产。且对飞灰的无害化及资源化方法设计合理，各组分回收利用率高。
Description
技术领域
本发明属于环境工程技术领域，涉及到垃圾焚烧产生飞灰无害化 与资源化的研究，特别涉及到应用于飞灰中有毒污染物高效去除的电 极制备及电化学降解系统构建，并在此基础上形成整套飞灰中各组分 资源化回收利用方法的革新。
背景技术
随着人口增长和社会发展，我国生活垃圾的数量呈现急剧增加的 趋势，在此基础上垃圾组成结构也不断发生变化，这都严重影响我国 生态环境安全和经济的可持续发展。由于我国土地资源短缺，垃圾填 埋法正逐渐被高温焚烧技术所取代。垃圾焚烧不仅可以实现生活垃圾 减量化，而且焚烧产生的热量还可以用于发电实现部分资源循环再生。 但该过程中会产生大量的飞灰，其质量约为该技术处理总量的5％。同 时，在高温裂解过程中，生活垃圾中重金属和裂解不充分所产生的有 毒产物二噁英会在飞灰表面富集，使飞灰成为具有较大环境风险的危 险废弃物，威胁环境安全和人类健康。因此，对飞灰中有毒污染物去 除和有效资源的回收利用已经成为制约焚烧技术应用的瓶颈问题。
目前，研究者们针对飞灰无害化及资源化处理技术进行了大量研 究，可分为分离萃取、固化与稳定化、热处理三大类。其中，水泥固 化、熔融烧结、机械化学、蒸发结晶、絮凝与离子交换等方法已经被 广泛研究，但上述处理方法均无法在经济性、环保性和可行性等方面 满足飞灰无害化及资源化处理的需求。此外，对飞灰中富集的重金属 和二噁英等污染物高效、低耗去除和有效资源回收技术手段匮乏也严 重制约飞灰无害化及资源化成套处理技术的发展和应用。
发明内容
本发明根据飞灰中组成成分及含量，开发一种在高盐和高氯水体 中同步高效去除有机污染物和重金属离子的电化学氧化还原降解系 统，增强飞灰资源化过程中对二噁英去除和重金属回收能力，并以此 为基础，重组优化飞灰中各组分回收方法和顺序，简化传统飞灰资源 化过程，形成一整套高效、低耗飞灰无害化及资源化方法的革新。
本发明技术方案：
一种飞灰中污染物的去除及资源化方法，步骤如下：
步骤1：选择厚度为1-3mm的钛基板，置于0.5-2mol/L草酸水溶 液中，经60～80℃水浴反应3-8h，取出电极在去离子水中超声30-60 min，之后在60℃烘箱中干燥待用。
步骤2：取氯化钌和氯化铱(摩尔比1∶10-10∶1)溶于1L去离子水 中，超声分散1h，真空除氧30min。将步骤1的钛基板和钌铱混合溶 液置于氮气氛围手套箱中，调整平板加热器温度为700-1000℃，加热 钛基板，加热时间为1-3min，之后快速将加热后的钛基板置于钌铱混 合溶液中，静置5-30s，取出后水洗干燥，重复该过程1-10次，得到 带有Ru-Ir层的钛基板。
步骤3：选用真空等离子喷涂法在步骤2中得到的钛基板表面制备 Ti4O7薄层。制备条件为：喷涂电压为60-70V，喷涂电流为500-600A， 氩气流量为2000-2400L/h，氢气流量为10-30L/h，Ti4O7喷涂量为 300-400g/m2。该方法制备带有Ru-Ir中间层的Ti4O7电极作为阳极与 哈氏合金极板(与阳极相同尺寸)作为阴极构建电化学氧化还原体系， 用于飞灰水洗液中TOC和重金属去除。
步骤4：对飞灰进行二次水洗以去除二噁英和重金属。室温25℃， 搅拌水洗时间5-15min，水洗液固比为4∶1-10∶1(mL∶g)，对第一次水洗 液进行高速过滤后加入碳酸钠进行絮凝沉淀，回收得到轻质碳酸钙 (CaCO3)，可作为塑料、造纸、涂料和油墨等行业的填料。二次水洗 后的溶液再重新用于对飞灰的第一次水洗过程，即用于水洗未被水洗 的飞灰，将第二次水洗液再用于未水洗飞灰的第一次水洗步骤，以提 高出水含盐量，水洗液进行高速过滤后加入碳酸钠得到轻质CaCO3。 通过液相色谱和电感耦合等离子光谱测试，经二次水洗的飞灰其浸出 液中重金属离子成分浓度未超过《危险废物鉴别标准-浸出毒性鉴别》(GB 5085.3-2007)中危害成分浓度限值。相比于未水洗飞灰，经水洗 后的飞灰制成的水泥调料可显著提高水泥稳定性，抑制金属离子及氯 离子渗出现象。
步骤5：以步骤3中构建的电化学氧化还原系统对步骤4中分离回 收Ca2+后飞灰水洗液，用盐酸调节pH至4，进行电化学氧化还原，运 行条件为：恒电流10-15mA/cm2，电极间距1-2cm，反应时间10-120 min。相比于进水，反应出水TOC从30-40mg/L降至6-8mg/L，Pb、Cd、Mn、Cu、Sb、Cr、Hg等重金属离子去除率均在95％以上。
步骤6：经步骤5后飞灰水洗液通过纳滤膜去除剩余少量二价离 子，出水以蒸发方式将溶液体积浓缩至原溶液的0.2-0.1倍，室温下静 置，KCl晶体析出，抽滤分离得到纯度为95％-96％KCl，可作为农业用 盐。剩余的飞灰水洗液主要成分为NaCl，可直接作为氯碱厂的电解液， 用于电解制备NaOH、Cl2和H2。
针对飞灰水洗液中无机盐和氯离子含量较高从而严重影响电化学 降解过程中阳极和阴极使用效果和使用寿命的问题。本发明方法中结 合淬火法(制备中间层)和等离子喷涂法(制备超薄催化层)制备具 有Ru-Ir中间层的Ti4O7阳极。通过淬火法引入的Ru-Ir中间层，不仅 能够有效减少制备过程中氯化钌和氯化铱使用量，还能够有效控制中 间层厚度(20-200nm)和负载量(5-40g/cm2)。此外，淬火法制备的 Ru-Ir中间层会在Ti基底呈现出均匀分散的纳米岛，可作为锚定位点诱 导Ti4O7负载，强化Ti4O7氧空位表达，减少表面形貌缺陷，抑制电解 质渗透氧化Ti基底，达到提高催化层结构稳定性、耐腐蚀性和析氧电 位的作用。在中间层表面通过等离子喷涂法制备的Ti4O7超薄催化层在 较低的Ti4O7使用量情况下形成较强的电化学氧化性能。同时，鉴于飞 灰水洗液具有高盐和高氯的特点，阴极材料选择具有较高的耐酸、碱 腐蚀性能的哈氏合金，在电化学反应过程中还能有效避免氢脆对阴极 结构的破坏。采用带有Ru-Ir中间层的Ti4O7电极(阳极)与哈氏合金 电极(阴极)构建电化学氧化还原体系，可在高盐和高氯环境下降解 矿化飞灰水洗液中二噁英等有机污染物，并在阴极通过还原反应回收 重金属离子，达到降低水洗液TOC和重金属含量的目的。
以对飞灰无害化及资源化为目的，通过分析飞灰组成成分及含量， 引入可耐受高盐、高氯环境的电化学氧化还原系统对飞灰表面富集的 二噁英等有毒污染物和重金属进行有效降解矿化和还原回收，合理优 化飞灰中资源回收顺序及方法，最大程度实现资源化。
具体实施方式
以下结合技术方案详细叙述本发明的具体实施方式。
本发明提供了一种可在高盐和高氯水体中同步高效去除有机污染 物和重金属离子的电化学氧化还原系统，并以此为基础形成整套高效 飞灰资源化回收的方法，属于环境污染控制工程技术领域。本发明方 法中结合淬火法(制备中间层)和等离子喷涂法(制备超薄催化层) 制备具有钌-铱中间层的Ti4O7阳极，与哈氏合金电极(阴极)构建电 化学氧化还原体系，可在高盐和高氯环境下降解矿化飞灰水洗液中的 二噁英等有机污染物，并在阴极通过还原作用固定重金属离子，达到 降低水洗液TOC和重金属含量的目的。以对飞灰无害化及资源化为目 的，根据飞灰组成成分及含量，结合耐高盐、高氯电化学氧化还原系 统，合理优化重组水洗、絮凝沉淀、膜过滤、蒸发结晶等资源化方法， 最大程度实现资源化。该方法中涉及电极制备方法简便、成本低廉、 易于规模化生产。且对飞灰的无害化及资源化方法设计合理，各组分 回收利用率高。
本发明以带有Ru-Ir中间层的Ti4O7阳极和哈氏合金阴极构建电化 学氧化还原系统，阳极能够降解有机污染物，阴极可以还原重金属离 子，阳极不仅具有Ti4O7催化层的电化学特性还具有Ru-Ir中间层的电 化学特性，因此，纯Ti4O7电极和Ru-Ir电极作为阳极构建的电化学氧 化还原系统也在保护范围内。
实施例1
阳极电极制备：厚度为1mm、表面积为5×5cm2的钛基板，置于 0.5mol/L草酸水溶液中，80℃水浴反应6h，取出电极在去离子水中超 声60min，之后在60℃烘箱中干燥待用。取氯化钌和氯化铱(摩尔比 8∶1)溶于1L去离子水中，超声分散1h，真空除氧30min。再将钛基板和钌铱混合溶液置于氮气氛围手套箱中，调整平板加热器温度为 900℃，加热钛基板，加热时间为1min，之后快速将加热后钛基板置 于钌铱混合溶液中，静置5s，取出水洗干燥后，重复该过程4次，得 到带有Ru-Ir层的钛基板。将带有Ru-Ir层钛基板置于真空等离子喷涂 仪中，喷涂电压为60V，喷涂电流为500A，氩气流量为2000L/h，氢 气流量为15L/h，Ti4O7喷涂量为400g/m2，得到带有Ru-Ir中间层的 Ti4O7电极。
高盐、高氯环境下有机污染物去除应用：将带有Ru-Ir中间层的 Ti4O7电极(阳极)与哈氏合金极板(阴极)构建电化学氧化还原体系。 反应条件：恒电流10mA/cm2，电极间距1cm。电解质为KCl水溶液 (质量分数25％)，有机污染物为20mg/L2，4，6-三氯苯酚。反应时间 30min，出水2，4，6-三氯苯酚去除率为99％，矿化率达到75％。
实施例2
阳极电极制备：厚度为1mm、表面积为5×5cm2的钛基板，置于 1mol/L草酸水溶液中，80℃水浴反应8h，取出电极在去离子水中超 声60min，之后在60℃烘箱中干燥待用。取氯化钌和氯化铱(摩尔比 9∶1)溶于1L去离子水中，超声分散1h，真空除氧30min。再将钛 基板和钌铱混合溶液置于氮气氛围手套箱中，调整平板加热器温度为 900℃，加热钛基板，加热时间为1min，之后快速将加热后钛基板置 于钌铱混合溶液中，静置5s，取出水洗干燥后，重复该过程10次， 得到带有Ru-Ir层的钛基板。将带有Ru-Ir层钛基板置于真空等离子喷涂仪中，喷涂电压为60V，喷涂电流为500A，氩气流量为2000L/h， 氢气流量为15L/h，Ti4O7喷涂量为400g/m2，得到带有Ru-Ir中间层 的Ti4O7电极。
高盐、高氯环境下阴极还原重金属离子应用：将带有Ru-Ir中间层 的Ti4O7电极(阳极)与哈氏合金极板(阴极)构建电化学氧化还原体 系。反应条件：恒电流10mA/cm2，电极间距1cm。电解质为KCl水 溶液(质量分数25％)，重金属离子为10mg/L PbCl2。反应时间30min， 出水pb2+去除率为99.5％。
实施例3
飞灰资源化方法：取50g飞灰，对其进行二次水洗，以去除二噁 英和重金属。水洗条件为室温25℃，搅拌水洗时间10min，水洗液固 比为5∶1(mL∶g)，对第一次水洗液高速过滤后进行絮凝沉淀，加入无水 Na2CO3直至不再出现沉淀为止，过滤得到轻质CaCO3，纯度为97％， 可作为塑料、造纸、涂料和油墨等行业的填料。将第二次水洗出水重 新用于未水洗飞灰的第一次水洗步骤，水洗液进行高速过滤后加入 Na2CO3得到轻质CaCO3，将上述两阶段水洗的水洗液混合。通过液相 色谱和电感耦合等离子光谱测试，经二次水洗的飞灰其浸出液的总无 机盐离子含量均未超过《危险废物鉴别标准-浸出毒性鉴别》(GB 5085.3-2007)中危害成分浓度限值。将其作为水泥填料，相比于未水 洗飞灰，可显著提高水泥稳定性，抑制金属离子及氯离子渗出现象。 将经过Ca2+分离回收后的飞灰水洗液，用盐酸调节pH至4，再置于本 发明构建的电化学氧化还原系统中进行电化学氧化还原过程，运行条 件为：恒电流10mA/cm2，电极间距1cm，反应时间10min。相比于 进水，反应出水TOC下降了82％，降至6mg/L，Pb、Cd、Mn、Cu、 Sb、Cr、Hg等重金属离子去除率均在95％以上。选择纳滤膜过滤电化学降解系统的出水，去除剩余的少量二价离子，出水以蒸发方式将溶 液体积浓缩至原溶液的0.2-0.1倍，室温下静置，KCl晶体析出，抽滤 分离得到纯度为95％-96％KCl，可作为农业用盐。剩余的飞灰水洗液 主要成分为NaCl，可直接作为氯碱厂的电解液，用于电解制备NaOH、 Cl2和H2。
Claims (5)
1.一种飞灰中污染物的去除及资源化方法，其特征在于，步骤如下：
步骤1：厚度为1-3mm的钛基板，置于0.5-2mol/L草酸水溶液中，60～80℃水浴反应3-8h，取出电极在去离子水中超声30-60min，之后在60℃烘箱中干燥待用；
步骤2：取氯化钌和氯化铱(摩尔比1∶10-10∶1)溶于1L去离子水中，超声分散1h，真空除氧30min，将步骤1的钛基板和钌铱混合溶液置于氮气氛围手套箱中，调整平板加热器温度为700-1000℃，加热钛基板，加热时间为1-3min，之后快速将加热后的钛基板置于钌铱混合溶液中，静置5-30s，取出水洗干燥后，重复该过程1-10次，得到带有Ru-Ir层的钛基板；
步骤3：选用真空等离子喷涂法在步骤2中得到的钛基板表面制备Ti4O7薄层，制备条件为：喷涂电压为60-70V，喷涂电流为500-600A，氩气流量为2000-2400L/h，氢气流量为10-30L/h，Ti4O7喷涂量为300-400g/m2，该方法制备带有Ru-Ir中间层的Ti4O7电极作为阳极与哈氏合金极板(与阳极相同尺寸)作为阴极构建电化学氧化还原体系，用于飞灰水洗液中TOC和重金属去除；
步骤4：对飞灰进行二次水洗以去除二噁英和重金属，室温25℃，搅拌水洗时间5-15min，水洗液固比为4∶1-10∶1(mL∶g)，对第一次水洗液进行高速过滤后加入碳酸钠进行絮凝沉淀，回收得到轻质碳酸钙(CaCO3)，将第二次水洗液再用于未水洗飞灰的第一次水洗步骤，以提高出水含盐量，水洗液进行高速过滤后加入碳酸钠得到轻质CaCO3；
步骤5：以步骤3中构建的电化学氧化还原系统对步骤4中分离回收Ca2+后飞灰水洗液进行电化学氧化还原，运行条件为：恒电流10-15mA/cm2，电极间距1-2cm，反应时间10-120min；
步骤6：经步骤5后飞灰水洗液通过纳滤膜去除剩余的少量二价离子，出水以蒸发方式将溶液体积浓缩至原溶液的0.2-0.1倍，室温下静置，KCl晶体析出，抽滤分离得到纯度为95％-96％KCl，剩余的飞灰水洗液主要成分为NaCl，可直接作为氯碱厂的电解液，用于电解制备NaOH、Cl2和H2。
2.根据权利要求1所述的方法，其特征在于，通过淬火法在钛基材料表面制备中间层，选自多孔状钛板、平板状钛或箔片状钛；不锈钢板等金属基底材料。
3.根据权利要求1所述的方法，其特征在于，通过淬火法制备中间层的方法，选自Ru-Ir中间层，金属氧化物中间层。
4.根据权利要求1所述的方法，其特征在于，结合淬火法和真空等离子喷涂法制备带有中间层和超薄催化层的电催化材料。
5.根据权利要求1所述的方法，其特征在于，以带有Ru-Ir中间层的Ti4O7阳极和哈氏合金阴极构建电化学氧化还原系统，阳极能够降解有机污染物，阴极可以还原重金属离子，阳极不仅具有Ti4O7催化层的电化学特性还具有Ru-Ir中间层的电化学特性。
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| CN114147053A (zh) * | 2021-10-11 | 2022-03-08 | 北京建筑材料科学研究总院有限公司 | 一种从垃圾焚烧飞灰中同时去除氯和重金属的方法 |
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