CN113828276A - 一种降低污染物气体中硫含量的活性炭吸附剂 - Google Patents
一种降低污染物气体中硫含量的活性炭吸附剂 Download PDFInfo
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 28
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Abstract
本发明公开了一种降低污染物气体中硫含量的活性炭吸附剂，通过将原料颗粒预热干燥，干燥后的原料颗粒初级炭化，然后进行炭化料的碱洗浸渍联合高温焙烧，再加入碱性活化剂对炭化料表面负载金属化合物，最后，通过真空干燥去除多余的水分子得到的一种降低污染气体中硫含量的活性炭吸附剂。本发明利用活性炭独特结构和性能作为脱硫吸附剂，通过对炭化料碱洗浸渍联合高温焙烧的方法，更好的增大活性炭孔经比表面积及孔径大小；同时碱性浸渍也更好的促进金属离子的负载，在使用超声波震动状态下能更好的使负载的金属化合物均匀，通过对活性炭比表面积的改变，以及金属化合物的有效改性，增强活性炭吸附剂的吸附性能，能更好的降低污染气体中硫含量。
Description
技术领域
本发明涉及活性炭制备的技术领域，尤其涉及一种可降低污染物气体中硫含量的活性炭吸附剂。
背景技术
随着化学技术的发展，人们对天然能源物质利用的深度加大。煤、石油、天然气等原料中都含有一定量的硫化合物，对它们进行加工后含硫化合物会以不同形态存在产品中，例如矿物燃料燃烧产生的SO2气体污染物；人造丝厂、炼油厂在产生过程中产生的含有多种含硫杂质气体；也有生物腐烂生成的硫化氢在大气中氧化形成的污染气体。
目前现有技术中脱硫技术也较为成熟，但在脱硫过程中生成物的酸性液体和淤渣较难处理，并且腐蚀设备难以避免，在脱硫过程中其能耗过高，费用高等弊端。活性炭是一种成熟的碳材料，具备独特的表面物理和化学性质，活性炭在化学工业、食品工业等行业中作为重要的吸附材料，目前也有采用活性炭的脱硫技术，在工艺制备中通过对活性炭的改性包括将金属负载在活性炭表面，改变表面化学环境，达到脱硫效果，但是在负载金属化合物的同时也降低了孔隙度，特别是微孔的容积，并且金属的负载量和分布不均，导致脱硫效果不够高效。
发明内容
本发明目的是为了解决现有技术中存在的活性炭吸附剂除硫效率差，改性后的活性炭吸附剂孔隙度降低，特别是微孔的容积，以及负载量和分布不均的问题，导致脱硫效果不够高效。而提出的一种可降低污染物气体中硫含量的活性炭吸附剂。为了实现技术的优化使在脱硫过程中能更高效的降低空气中硫含量，减少污染，降低能耗，节约成本。本发明采用了如下生产工艺：
本发明涉及一种可降低污染物气体中硫含量的活性炭吸附剂，是使用碱洗浸渍联合高温焙烧得到的初级活性炭吸附剂，再通过原位合成对炭化料表面负载金属化合物的制备方法，所述的制备方法包括如下：
1)干燥阶段：将原料颗粒进行预热干燥，所述预热干燥的温度设置在 100℃～200℃，时间设置为1～3h，将原料颗粒中的水分和内在水释放出来。
2)初级炭化：将干燥后的原料颗粒进行初级炭化，所述初级炭化的温度设置在300℃～600℃，时间设置在2～4小时的环境进行炭化。
3)碱洗浸渍：将加工后的初级炭化料放入到含有碱性活化剂和水蒸气助活化剂的旋转蒸发器中浸渍，碱洗浸渍的碱炭比为2～3：1。
4)高温焙烧：将碱洗浸渍后的炭化料在温度为600℃～900℃，时间为2～ 3小时的环境中进行焙烧，得到初级活性炭吸附剂。
5)进一步活化：通过金属盐溶液浸渍使活性炭孔道表面负载金属离子，即将初级活性炭浸渍在10～30％的碱性溶液中时间设置为4～8小时；同时将金属盐加入到去离子水中，在温度60～90℃条件下加热搅拌1～2小时，得到金属离子溶液；将得到的金属离子溶液加入到含有碱性溶液的初级活性炭吸附剂中，在水浴温度设置在40～60℃，超声波中混合2～6小时后，将已经浸渍了金属化合物的载体摊开阴干2～4小时；
6)将阴干的载体在100～200℃下干燥2～5小时，然后在200～500℃氮气氛围下活化2～5小时即制得均匀负载金属化合物的活性炭吸附剂。
6)干燥：通过对负载金属化合物的活性炭吸附剂进行干燥，在温度为 90℃～120℃，干燥时间为12h～24h，获得干燥的且能降低污染气体中硫含量的活性炭吸附剂。
进一步，所述碱性活化剂和碱性溶液包括有氢氧化钠水溶液、氢氧化钾水溶液、氨水水溶液中的至少一种。
进一步，所述水蒸气助活化中，水蒸气的用量是炭化料的1～2倍，温度为 300～600℃，活化时间为2～6小时，
进一步，所述旋转蒸发器的转速为50～160转/分。
进一步，所述金属盐包括氯化铁、氯化铜、氯化钙、氯化锌中的至少一种；利用去离子的金属盐溶液浸渍活性炭，通过原位合成使活性炭吸附剂的孔道内负载金属离子。
与现有技术相比，本发明的有益效果是：本发明的制备方法利用活性炭独特结构和性能在作为深度脱硫吸附剂，通过使用活性炭吸附剂吸附污染物气体中的硫化物，活性炭本身具有高活性、机械强度高，化学稳定性强，易于再生，可循环等优点；同时，在碱性溶液浸渍下制备活性炭可以增大活性炭孔经表面积及孔径大小，同时也能使金属负载量增加，在超声波震动下能更好的使金属化合物均匀负载，通过对活性炭比表面积的改变，表面官能团及金属化合物的有效改性，使活性炭的脱硫效果增强，能更好的降低气体中硫含量。
具体实施方式
下面对本发明作进一步说明，显然，所描述的实施例仅仅是本发明的部分实施例，而不是全部的实施例。
一种降低污染气体中硫含量的活性炭吸附剂，是通过使用碱洗浸渍联合高温焙烧得到的初级活性炭吸附剂，再通过原位合成对初级活性炭吸附剂表面负载金属化合物得到所述活性炭吸附剂，具体实施例包括如下：
实施例1
1)干燥阶段：将煤原料进行粉碎、挤压形成所需形状的原料颗粒，将原料颗粒温度设置在100℃，时间设置为3h，条件下进行预热干燥，将原料颗粒中的水分和内在水释放出来；
2)初级炭化：将干燥后的原料颗粒进行初级炭化，设置初级炭化的温度在 300℃，时间设置在4h，初级炭化后得到炭化料，此时形成初级的孔道结构，便于更好的进行后续操作；
3)碱洗浸渍：将加工后的初级炭化料放入到10％氢氧化钠的碱性活化剂中，碱洗浸渍的碱炭比为2：1，同时在水蒸气助活化剂的旋转蒸发器中浸渍，旋转蒸发器设置为100转/分，水蒸气的用量是炭化料的2倍，温度设置为300℃，活化时间为4h，得到活化后的炭化料，在氢氧化钠热解过程中炭化料会形成丰富的孔隙结构，使得炭得率降低，通过旋转蒸发器使得浸渍的更加充分；
4)高温焙烧：将碱洗浸渍后的炭化料在温度为600℃，时间为3小时的环境中进行煅烧，得到初级活性炭吸附剂，由于炭化料被碱性活化，此次高温煅烧使得炭化料孔道的比表面积进一步增大；
5)进一步活化：通过金属盐溶液浸渍使活性炭孔道表面负载金属化合物，即将初级活性炭在10％的氢氧化钠溶液中浸渍4小时；同时将氯化铁加入到去离子水中，在温度60℃条件下加热搅拌1h，得到含有铁离子的溶液；将得到的铁离子溶液加入到浸渍过氢氧化钠的初级活性炭吸附剂中，在水浴温度为40℃的超声波中混合3小时后，得到均匀负载有氢氧化铁的活性炭吸附剂；利用碱性溶液浸渍能增加金属离子的附着，由于使用超声波的震荡使得铁离子分布的更加均匀，进而使得氢氧化铁沉淀更均匀的负载在活性炭吸附剂的孔道内，便于更高效的结合污染气体中的硫物质。
6)干燥：通过对负载金属化合物的活性炭吸附剂进行加热干燥，在温度为 100℃，干燥时间为4h，获得干燥的且能降低污染气体中硫含量的活性炭吸附剂；通过干燥过程，使得原负载的金属沉淀物进一步生成稳定的化合物，使得金属化合物能更稳定的存在与活性炭的孔道内。
实施例2
1)干燥阶段：将煤原料进行粉碎、挤压形成所需形状的原料颗粒，将原料颗粒温度设置在200℃，时间设置为2h，条件下进行预热干燥，将原料颗粒中的水分和内在水释放出来；
2)初级炭化：将干燥后的原料颗粒进行初级炭化，设置初级炭化的温度在 600℃，时间设置在3h，初级炭化后得到炭化料，此时形成初级的孔道结构，便于更好的进行后续操作；
3)碱洗浸渍：将加工后的初级炭化料放入到10％氢氧化钾的碱性活化剂中，碱洗浸渍的碱炭比为2：1，同时在水蒸气助活化剂的旋转蒸发器中浸渍，旋转蒸发器设置为100转/分，水蒸气的用量是炭化料的2倍，温度设置为300℃，活化时间为4h，得到活化后的炭化料，在氢氧化钾热解过程中炭化料会形成丰富的孔隙结构，使得炭得率降低，通过旋转蒸发器使得浸渍的更加充分；
4)高温焙烧：将碱洗浸渍后的炭化料在温度为900℃，时间为2小时的环境中进行煅烧，得到初级活性炭吸附剂，由于炭化料被碱性活化，此次高温煅烧使得炭化料孔道的比表面积进一步增大；
5)进一步活化：通过金属盐溶液浸渍使活性炭孔道表面负载金属化合物，即将初级活性炭在25％的氨水中浸渍4小时；同时将氯化铝加入到去离子水中，在温度90℃条件下加热搅拌1h，得到含有铝离子的溶液；将得到的铝离子溶液加入到浸渍过氨水的初级活性炭吸附剂中，在水浴温度为60℃的超声波中混合 2小时后，得到均匀负载有氢氧化铝的活性炭吸附剂；利用碱性溶液浸渍能增加金属离子的附着，由于使用超声波的震荡使得铁离子分布的更加均匀，进而使得氢氧化铝沉淀更均匀的负载在活性炭吸附剂的孔道内，便于更高效的结合污染气体中的硫物质。
6)干燥：通过对负载金属化合物的活性炭吸附剂进行加热干燥，在温度为 100℃，干燥时间为6h，获得干燥的且能降低污染气体中硫含量的活性炭吸附剂；通过干燥过程，使得原负载的金属沉淀物进一步生成稳定的化合物，使得金属化合物能更稳定的存在与活性炭的孔道内。
实施例3
通过将本发明改进后的活性炭吸附剂与市场上其他活性炭进行对比，比较不同吸附剂降低污染气体中硫含量的实验：仪器：干燥器、水浴锅、气体流量计、电子天平、扫描电子显微镜等。
1)比表面积和孔径的测定
通过全自动比表面积及孔隙度分析仪，用BET测定法测定不同种类的活性炭比表面积以及孔径，使用检测材料分别为普通活性炭吸附剂、NaOH碱洗后的活性炭吸附剂、负载Fe金属化合物的活性炭吸附剂、NaOH碱洗后再负载金属化合物的活性炭吸附剂各20g。
比表面积和孔径的测定，比表面积是指单位质量固体所具有的总表面积，BET吸附等温线方程式是现在公认的测量固体比表面积的标准方法，公式： P/[V(Pо-P)]＝1/(Vm×C)﹢[﹙C-1)/(Vm×C﹚]×﹙P/Pо﹚
式中:P:氮气分压
P0:吸附温度下，氮气的饱和蒸汽压
V:样品表面氮气的实际吸附量
Vm:氮气单层饱和吸附量
C:与样品吸附能力相关的常数
2)脱硫效率的测定
为了检验改进后的活性炭吸附剂的效果，通过设置对照进行比较，相同的硫浓度，在不同的活性炭吸附剂下进行测试，首先把脱硫入口和出口的二氧化硫都折算到6％的氧量下，用入口二氧化硫浓度减去出口二氧化硫浓度，再比上入口二氧化硫浓度乘以100％。脱硫效率是单位时间内脱硫***脱除的二氧化硫量占进入脱硫***烟气中二氧化硫量的百分比。公式：脱硫效率＝(原来的二氧化硫浓度-脱硫后的二氧化硫浓度)/原来的二氧化硫浓度*100％
3)饱和硫容测定方法：
用纯水洗净后，放在120℃干燥箱中干燥，将气体预热装置调节为20℃，同时使吸附剂柱外层通入水的温度设置为20℃，将干燥过的活性炭放入吸附柱，连接好实验装置后，打开气瓶旋钮和减压阀，调节气体流速，使气体通过流量计的流速为500ml/min，在常压下测定四种活性炭的饱和硫容。
当出气口与进气口中硫化氢含量的比值小于0.05时，脱硫剂已经穿透，这时，每隔一个小时称量吸附剂柱一次，直至两次称量的质量差不大于0.0005g，实验结束后将饱和的活性炭取出，放入100℃干燥箱中干燥2h后，冷却后精确称重至0.0002g，得到脱硫剂在脱硫饱和后的质量，据此计算吸附量，饱和硫容计算：饱和硫容量w表示，单位是毫克每克(mg/g)：
W＝(m-m0)/m(m0：表示实验前干燥脱硫剂的质量(g),M表示实验后干燥脱硫剂的之质量(g))
不同吸附剂降低污染气体中硫含量的实验，通过将改进后的活性炭吸附剂与其他不同类型的活性炭吸附剂进行对比，比较不同类型活性炭的比表面积、孔径大小、脱硫率、饱和硫容量来判断活性炭的吸附效果，具体测量数据如下表：
从上表可以看出，通过相比较其他种类的活性炭吸附剂，本发明所改进的碱洗后负载金属化合物的活性炭吸附剂比表面积和孔径更大，同时脱硫率相对其他活性炭吸附剂更高，饱和硫容量也较高，因此具有更好的吸附气体中硫物质的效果，
本实施例的制备方法利用活性炭本身具有高活性、机械强度高，化学稳定性强，易于再生，可循环等优点，通过对炭化料碱洗浸渍联合高温焙烧的方法，更好的增大活性炭孔经比表面积及孔径大小；同时碱性浸渍也更好的促进金属离子的负载，在使用超声波震动状态下能更好的使负载的金属化合物均匀，利用旋转蒸发器使得浸渍的更加充分，这种通过原位合成对初级活性炭吸附剂表面负载金属化合物得到所述活性炭吸附剂，使得活性炭比表面积的增大，表面官能团及金属化合物得到有效改性，增强活性炭吸附剂的吸附性能，能更好的降低气体中硫含量。
以上所述，仅为本发明有较佳的具体实施效果，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，通过使用碱洗浸渍联合高温焙烧得到的初级活性炭吸附剂，再通过原位合成对初级活性炭吸附剂表面负载金属化合物得到所述活性炭吸附剂，具体制备方法包括如下：
1)干燥阶段：将原料颗粒进行预热干燥，所述预热干燥的温度设置在100℃～200℃，时间设置为1～3小时，将原料颗粒中的水分和内在水释放出来；
2)初级炭化：将干燥后的原料颗粒进行初级炭化，所述初级炭化的温度设置在300℃～600℃，时间设置在2～4小时；
3)碱洗浸渍：将加工后的初级炭化料放入到含有碱性活化剂和水蒸气助活化剂的旋转蒸发器中浸渍，碱洗浸渍的碱炭比为2～3：1；
4)高温焙烧：将碱洗浸渍后的炭化料在温度为600℃～900℃，时间为2～3小时的环境中进行焙烧，得到初级活性炭吸附剂；
5)进一步活化：通过金属盐溶液浸渍使活性炭孔道表面负载金属离子，即将初级活性炭浸渍在10-30％的碱性溶液中4～8小时；同时将金属盐加入到去离子水中，在温度60～90℃条件下加热搅拌1～2小时，得到金属离子溶液；将得到的金属离子溶液加入到含有碱性溶液的初级活性炭吸附剂中，在水浴温度为40～60℃，超声波中混合2～6小时后，得到均匀负载金属化合物的活性炭吸附剂；
6)进一步干燥：通过高温对负载金属化合物的活性炭吸附剂进行干燥。
2.根据权利要求1所述的一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，所述碱性活化剂和碱性溶液包括有氢氧化钠水溶液、氢氧化钾水溶液、氨水水溶液中的至少一种。
3.根据权利要求2所述的一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，所述水蒸气助活化中，水蒸气的用量是炭化料的1～2倍，温度设置为300～600℃，活化时间设置为2～6小时。
4.根据权利要求3所述的一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，所述旋转蒸发器的转速为50～160转/分。
5.根据权利要求4所述的一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，所述金属盐包括氯化铁、氯化铜、氯化钙、氯化锌中的至少一种。
6.根据权利要求5所述的一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，所述进一步干燥温度为90℃～180℃，干燥时间为2h～8h。
7.根据权利要求6所述的一种降低污染气体中硫含量的活性炭吸附剂，其特征在于，所述金属盐为氯化铁时，在进一步活化中，通过将初级活性炭浸渍在10-30％的碱性溶液中4～8小时；同时将氯化铁加入到去离子水中，在温度60～90℃条件下加热搅拌1～2小时，得到含有铁离子的溶液；再将得到的铁离子溶液加入到浸渍过碱性溶液的初级活性炭吸附剂中，在水浴温度为40～60℃，超声波中混合2～6小时后，得到均匀负载有氢氧化铁的活性炭吸附剂。
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