CN114887610B - 一种金属改性活性炭及其制备方法和应用 - Google Patents
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Abstract
本发明公开了一种金属改性活性炭及其制备方法和应用，其中，本发明的一种金属改性活性炭的制备方法，包括：盐溶液的配制：将金属盐与水混合配置成盐溶液；活性炭改性：将活性炭与盐溶液混合，超声处理后，采用电磁搅拌，静置、过滤后获得改性活性炭；干燥：将过滤获得的改性活性炭进行清洗并干燥获得成品。本发明的方法能有效提高制备得到的一种金属改性活性炭的氨气去除效率，效果显著。
Description
技术领域
本发明涉及催化剂领域，具体涉及一种金属改性活性炭及其制备方法和应用。
背景技术
NH3是一种极具毒性、污染性、腐蚀性、刺激性和危险性的碱性气体，广泛存在于各种工业流程中，如制冷剂、肥料、医药中间体、炸药、清洁剂等。NH3与大气中的酸性气体反应生成铵盐，被认为是PM2.5形成的一个重要原因。如果NH3直接排放到大气中，将会给人类健康带来严重的问题，并导致各种环境问题。短期暴露在NH3环境中即可影响呼吸道功能，并引起眼部、皮肤不适。长时间暴露于高浓度的NH3环境中将引发暂时性失明、肺水肿、水疱等，严重时会威胁人的生命安全。
NH3产生途径有两类，自然产生与人类生产实践活动产生。自然产生包括火山喷发、动植物等有机体腐烂分解、雷电等自然现象。对于人类生产实践活动产生的NH3，目前，工业上NH3脱除与回收方法主要有吸收法、吸附法、膜分离法、氧化法和生物法。吸收法主要分物理吸收和化学吸收，物理吸收利用NH3在水中有较高溶解度的特性，而化学法主要利用NH3的碱性与酸性吸收剂的化学反应来吸收NH3。物理吸收法是目前废气脱除NH3最常用、最成熟的方法。
吸附法是利用吸附材料的选择性吸附来达到NH3脱除的目的，既有物理性质的吸附，如分子筛、活性炭吸附等，也有化学性质的吸附，如酸改性的吸附材料。吸附分离具有节能高效的特点，而有效的吸附剂是该方法应用效果的关键。
目前，现有的达到NH3脱除的吸附剂，大部分都是金属改性后的活性炭，但该改性后的活性炭对氨气的去除率并不显著，需要对其进行进一步优化以提高其对氨气的去除率；并且，现有金属改性后的活性炭大部分都只适用于高浓度氨气的去除，对于低浓度的氨气的去除难度极大，尤其是1h内氨气的去除率普遍都在60％以下，去除效果并不理想。
发明内容
因此，本发明的目的在于，解决现有的制备方法获得的金属改性活性炭吸附剂在去除氨气时，对氨气的去除效率并不显著的问题，提供一种能有效提高氨气去除效率的一种金属改性活性炭的制备方法，以及该制备方法制备得到的一种金属改性活性炭及其应用。
一种金属改性活性炭的制备方法，包括：
盐溶液的配制：将金属盐与水混合配置成盐溶液；
活性炭改性：将活性炭与盐溶液混合，超声处理后，采用电磁搅拌，静置、过滤后获得改性活性炭；
干燥：将过滤获得的改性活性炭进行清洗并干燥获得成品。
所述金属盐为铜盐和铁盐，其中，铜盐和铁盐的摩尔比为2:1，所述铜盐和铁盐总质量与活性炭的质量之比为1:(5-6)。
所述铜盐为可溶性铜盐，优选为硝酸铜、硫酸铜中的至少一种。
所述铁盐为可溶性铁盐，优选为氯化铁、硫酸亚铁、硫酸铁中的至少一种。
所述盐溶液中铜盐浓度为0.005-0.01mol/L。
所述活性炭改性步骤中，所述超声处理的参数为：超声能量密度为2.0W/mL，超声频率为35Hz，超声时间为5-30min。
所述干燥步骤中，干燥的温度为105℃，干燥时间为12h。
本发明还包括上述制备方法制备得到的一种金属改性活性炭。
本发明还包括上述制备方法制备得到的一种金属改性活性炭在氨气催化中的应用。
所述氨气为浓度低于10mg/m3的低浓度氨气。
本发明技术方案，具有如下优点：
1.通过本发明的制备方法，尤其是通过本方法中超声步骤和电磁搅拌步骤的配合，可以明显提高制备得到的成品对氨气的去除率，尤其是在低浓度氨气中1h内的氨气去除效率，达到在低浓度氨气中短时间内处理的目的，效果明显。
2.本发明中金属盐优选为铜盐和铁盐，通过铜盐和铁盐的相互配合，可以产生协同增效的作用，提高在氨气处理中氨气的去除率，通过实施例数据可知，两者相互配合，可以将氨气去除率提高到60％以上，高于现有公开的金属处理后的活性炭吸附剂。
3.本发明方法制备得到的成品可在常温下处理氨气，无需加热至高温，节约了用电成本；同时，本申请方法简单易操作，反应条件温和，氨气去除效果明显，制备过程无有毒有害副产物产生，不会对环境造成二次污染。
附图说明
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本发明实验例中实施例的氨气去除率结果示意图。
具体实施方式
提供下述实施例是为了更好地进一步理解本发明，并不局限于所述最佳实施方式，不对本发明的内容和保护范围构成限制，任何人在本发明的启示下或是将本发明与其他现有技术的特征进行组合而得出的任何与本发明相同或相近似的产品，均落在本发明的保护范围之内。
实施例中未注明具体实验步骤或条件者，按照本领域内的文献所描述的常规实验步骤的操作或条件即可进行。
实施例1
一种金属改性活性炭的制备方法，本实施例中制备的是Cu(NO3)2-AC，具体过程如下：
称取2.416g Cu(NO3)2·3H2O溶解于水中，配制成0.01moL/L的硝酸铜溶液。称取20g活性炭，水洗烘干后加入硝酸铜溶液，超声10min后将其进行多相柔性磁力搅拌4h；超声条件为：能量密度为2.0W/mL，超声频率为35Hz。静置8h，过滤、洗净后于干燥箱中105℃干燥12h，制备成Cu(NO3)2-AC样品。
实施例2
一种金属改性活性炭的制备方法，本实施例中制备的是FeCl3-AC，具体过程如下：
称取2.702g FeCl3·6H2O溶解于水中，配制成0.01moL/L的氯化铁溶液，称取20g活性炭，水洗烘干后加入氯化铁溶液，超声10min后将其进行多相柔性磁力搅拌4h；超声条件为：能量密度为2.0W/mL，超声频率为35Hz。静置8h，过滤、洗净后于干燥箱中105℃干燥12h，制备成FeCl3-AC样品。
实施例3
一种金属改性活性炭的制备方法，本实施例中制备的是Cu(NO3)2/FeCl3-AC，具体过程如下：
称取1.351g FeCl3·6H2O、2.416g Cu(NO3)2·3H2O溶解于水中，配制成浓度为0.01moL/L的盐溶液，称取20g活性炭，水洗烘干后加入盐溶液，超声10min后将其进行多相柔性磁力搅拌4h；超声条件为：能量密度为2.0W/mL，超声频率为35Hz。静置8h，过滤、洗净后于干燥箱中105℃干燥12h，制备成Cu(NO3)2/FeCl3-AC样品。
实施例4
一种金属改性活性炭的制备方法，本实施例中制备的是CuSO4/FeSO4-AC，具体过程如下：
称取2.500g CuSO4·5H2O、1.390g FeSO4·7H2O溶解于水中，配制成硫酸铜浓度为0.01moL/L的盐溶液，称取20g活性炭，水洗烘干后加入盐溶液，超声30min后将其进行多相柔性磁力搅拌4h；超声条件为：能量密度为2.0W/mL，超声频率为35Hz。静置8h，过滤、洗净后于干燥箱中105℃干燥12h，制备成CuSO4/FeSO4-AC样品。
实施例5
一种金属改性活性炭的制备方法，本实施例中制备的是CuSO4/FeSO4-AC，具体过程如下：
称取2.500g CuSO4·5H2O、1.390g FeSO4·7H2O溶解于水中，配制成硫酸铜浓度为0.005moL/L的盐溶液，称取20g活性炭，水洗烘干后加入盐溶液，超声5min后将其进行多相柔性磁力搅拌4h；超声条件为：能量密度为2.0W/mL，超声频率为35Hz。静置8h，过滤、洗净后于干燥箱中105℃干燥12h，制备成CuSO4/FeSO4-AC样品。
对比例1
一种金属改性活性炭，其与实施例1的区别在于，本实施例中制备工艺不同，本实施例中，不进行超声处理，采用常规机械搅拌方法搅拌4h。
对比例2
一种金属改性活性炭，其与实施例2的区别在于，本实施例中制备工艺不同，本实施例中，不进行超声处理，采用常规机械搅拌方法搅拌4h。
对比例3
一种金属改性活性炭，其与实施例3的区别在于，本实施例中制备工艺不同，本实施例中，不进行超声处理，采用常规机械搅拌方法搅拌4h。
试验例
采用实施例和对比例制备得到样品进行氨气去除实验，实验过程如下：
氨气标准曲线绘制：于各加入了氨水标准液和稀硫酸吸收液的比色管中，加入0.5mL 5％水杨酸溶液，再加入0.1mL 1％亚硝基铁氰化钠溶液和0.1mL 0.05mol/L次氯酸钠溶液，混匀，室温下显色1h后，用紫外-可见分光光度计测定各管溶液的吸光度。以氨含量(μg)为横坐标，吸光度为纵坐标，绘制标准曲线。
金属改性活性炭效果测试：将制备好的样品20g放置于一个反应容器中，通入浓度为1.00mg/m3的氨气，空速为1500mL/(g·h)，分别在30min、60min和180min对氨气浓度进行检测，反应后的氨气浓度采用靛酚蓝分光光度法进行定量测定，进而换算得到氨气的去除效率。
氨气去除结果如图1和表1所示。
表1
图1中AC为水洗烘干后的活性炭。
通过上述表1和图1中的结果可知：仅仅只是活性炭对氨气几乎没有去除作用；通过实施例1和对比例1、实施例2和对比例2、实施例3和对比例3的对比结果可知，采用超声处理和电磁搅拌的方式可以显著提高金属改性活性炭对低浓度氨气的去除效率；通过实施例1-2与实施例3的对比可知，铜盐和铁盐相互配合可以达到相互协同增效的作用，使金属改性活性炭在1h内氨气的去除率提高到60％以上，效果显著。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (8)
1.一种用于去除氨气的金属改性活性炭的制备方法，其特征在于，包括：
盐溶液的配制：将金属盐与水混合配置成盐溶液；
活性炭改性：将活性炭与盐溶液混合，超声处理后，采用电磁搅拌，静置、过滤后获得改性活性炭；
干燥：将过滤获得的改性活性炭进行清洗并干燥获得成品；
所述金属盐为铜盐和铁盐，其中，铜盐和铁盐的摩尔比为2:1；所述铜盐和铁盐总质量与活性炭的质量之比为1:（5-6）；
所述活性炭改性步骤中，所述超声处理的参数为：超声能量密度为2.0 W/mL，超声频率为35 Hz，超声时间为10-30 min。
2.根据权利要求1所述的制备方法，其特征在于，所述铜盐为硝酸铜、硫酸铜中的至少一种。
3.根据权利要求1所述的制备方法，其特征在于，所述铁盐为氯化铁、硫酸亚铁、硫酸铁中的至少一种。
4.根据权利要求1-3任一项所述的制备方法，其特征在于，所述盐溶液中盐的摩尔浓度为0.005-0.01mol/L。
5.根据权利要求1-3任一项所述的制备方法，其特征在于，所述干燥步骤中，干燥的温度为105℃，干燥时间为12 h。
6.权利要求1-5任一项所述的制备方法制备得到的一种金属改性活性炭。
7.权利要求1-5任一项所述的制备方法制备得到的一种金属改性活性炭在氨气去除中的应用。
8.根据权利要求7所述的应用，其特征在于，所述氨气为浓度低于10 mg/m³的低浓度氨气。
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