CN111097383A - 一种v2o5/煤沥青基复合球形活性炭的制备方法及其应用 - Google Patents
一种v2o5/煤沥青基复合球形活性炭的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开一种V2O5/煤沥青基复合球形活性炭的制备方法及其应用，将五氧化二钒3‑5g、聚乙烯吡咯烷酮0.5‑1g、乙二醇20‑40ml、吡啶80‑120ml、无水乙醇20‑40ml和去离子水50‑200ml混合，在水浴锅中磁力搅拌并加热到80‑100℃，冷凝回流至五氧化二钒固体全部溶解，冷却至室温制得五氧化二钒溶液；采用沉浸法将五氧化二钒溶液负载到煤沥青基球形活性炭表面，将负载后的煤沥青基球形活性炭置于管式炉中，在空气条件下，从室温升至200‑500℃，用时1‑4小时，再在200‑500℃恒温1‑4小时；待自然冷却后取出即得。
Description
技术领域
本发明涉及煤焦油沥青技术领域，尤其涉及一种五氧化二钒/煤沥青基复合球形活性炭的制备方法。
背景技术
煤沥青是煤焦油蒸馏加工去除液体馏分后的残余物，约占煤焦油总量的50％-60％，属大宗产品，其组成复杂，平均分子量为300-1000，含碳量高达90％以上。
煤沥青基球形活性炭具有比表面积大、机械性能好、吸附性能优异、装填密度均匀以及孔结构丰富等优点，作为水处理过程中的吸附剂得到了广泛应用，但物理吸附只能对污染物起到暂时的消除效果，不能达到完全分解转化的目的。
发明内容
针对现有技术存在的不足，本发明提供了一种V2O5/煤沥青基复合球形活性炭的制备方法，V2O5/催化性能良好，禁带宽度Eg较小，因此将五氧化二钒与煤沥青复合制备五氧化二钒/煤沥青基复合球形活性炭将吸附技术和光催化技术的协同作用发挥到极致，吸附技术和光催化技术的协同作用可以起到良好的互补效果，将其用于废水处理，其不仅能吸附水中的悬浮物，还能杀死水中的细菌。
为了达到上述目的，本发明采用以下技术方案实现：
一种V2O5/煤沥青基复合球形活性炭的制备方法，其特征在于包括以下步骤：
1)煤沥青基球形活性炭的制备
a.取吡啶溶液对煤焦油中温沥青进行索氏抽提、冷却、抽滤收取滤液；
b.称取聚乙烯醇，无水乙醇和去离子水于烧瓶中混匀后置于水浴锅中磁力搅拌并加热，确保聚乙烯醇完全溶解后，冷却至室温；
c.将冷却好的吡啶抽提溶液倒入容器，并超声震荡；
d.将超声后的混合溶液在80-90℃下进行热搅拌，温度达80-90℃时再恒温搅拌15-35分钟；
e.将搅拌后的溶液冷却至室温、抽滤得到煤沥青球；
f.不熔化处理
将煤沥青球放入管式炉中，在空气条件下，温度从常温升至250-350℃，用时30-40小时，再在250-350℃恒温2-5小时，待自然冷却取出样品；
g.炭化处理
将装有不熔化处理后的煤沥青球的陶瓷舟放置于管式炉中，在氮气气氛下炭化；
h.活化
取KOH加入到炭化后的煤沥青基球形活性炭中，在90-120℃真空干燥，最后将干燥后的小球放入管式炉中；在氮气气氛下，先从常温升至350-450℃，用时1-3小时，再在350-450℃恒温0.5-1.5小时，再从350-450℃升温到700-800℃，用时2-4小时，再在700-800℃恒温0.5-1.5小时；待自然冷却后取出样品，用盐酸和去离子水冲洗至中性，干燥即得煤沥青基球形活性炭；
2)五氧化二钒溶液的制备
将五氧化二钒3-5g、聚乙烯吡咯烷酮0.5-1g、乙二醇20-40ml、吡啶80-120ml、无水乙醇20-40ml和去离子水50-200ml混合，在水浴锅中磁力搅拌并加热到80-100℃，冷凝回流至五氧化二钒固体全部溶解，冷却至室温制得五氧化二钒溶液；
3)V2O5/煤沥青基复合球形活性炭的制备
采用沉浸法将五氧化二钒溶液负载到煤沥青基球形活性炭表面，将负载后的煤沥青基球形活性炭置于管式炉中，在空气条件下，从室温升至200-500℃，用时1-4小时，再在200-500℃恒温1-4小时；待自然冷却后即制备了V2O5/煤沥青基复合球形活性炭。
以太阳作为光源，将V2O5/煤沥青基复合球形活性炭与锦鲤水混合，持续搅拌，用平板涂布的方法测试V2O5/煤沥青基复合球形活性炭的杀菌效果。
所述中温沥青的软化点为65～90℃。
制得的V2O5/煤沥青基复合球形活性炭是一种多孔炭材料，表面粗糙部分为负载的五氧化二钒，内部呈球形成分为煤沥青。
制得的V2O5/煤沥青基复合球形活性炭，其特征在于：用于废水除菌处理。
本发明与现有技术相比，其显著的有益效果体现在：
通过本发明方法制备的V2O5/煤沥青复合球形活性炭具有良好的杀菌性能，解决了生活中水污染问题。
附图说明
图1是V2O5/煤沥青基球形活性炭煅烧后的XRD图；
图2是V2O5/煤沥青基球形活性炭的扫描电镜图a；
图3是V2O5/煤沥青基球形活性炭的扫描电镜图b；
图4是V2O5/煤沥青基球形活性炭的EDS分析；
图5是V2O5/煤沥青基球形活性炭的C元素EDS分析；
图6是V2O5/煤沥青基球形活性炭的O元素EDS分析；
图7是V2O5/煤沥青基球形活性炭的V元素EDS分析；
图8是V2O5/煤沥青基复合球形活性炭的杀菌性能评价图。
具体实施方式
下面结合具体实施例进行说明：
取块状煤沥青进行粉碎，过筛，用吡啶作为溶剂对煤沥青进行抽提处理，冷却后的抽滤液与1788型聚乙烯醇溶液混合，超声震荡，热搅拌(转数为300r/min)，当温度升到85℃时，恒温搅拌20分钟后，冷却，抽滤，得到固体小球并对其进行不熔化、炭化和KOH活化处理，即制得煤沥青基球形活性炭。
取3g五氧化二钒固体粉末、0.9g聚乙烯吡咯烷酮、30ml乙二醇、100ml吡啶和100ml去离子水混合，在水浴锅中磁力搅拌并加热到90℃，冷凝回流至五氧化二钒固体全部溶解，冷却至室温制得五氧化二钒溶液。
将五氧化二钒溶液用沉浸法滴入装有煤沥青基球形活性炭的坩埚中，待自然干燥后放入管式炉中，在空气气氛下400℃氧化4小时，冷却到室温即制得表面负载五氧化二钒的煤沥青基复合球形活性炭。
取两个40ml的烧杯(酒精消毒)分别放入20ml的锦鲤水和转子(酒精消毒)，将0.1gV2O5/煤沥青基球形活性炭放入其中一个烧杯中，将两只烧杯用保鲜膜封口，放置在太阳光下磁力搅拌5h，用原样锦鲤水作空白对照，每组做3个平行样，后用平板涂布法进行杀菌性能检测。
X射线衍射(XRD)技术用于材料晶体结构分析。
图1为表面负载五氧化二钒的煤沥青基球形活性炭煅烧后的XRD图，由图知，煅烧后的五氧化二钒成功与煤沥青球复合。
扫描电子显微镜(SEM)是利用入射电子束与被测样品表面发生作用而产生的二次电子成像。可以获取到样品的表面微观形貌、尺寸大小、分散情况、元素成分和含量、元素分布等信息。SEM主要被用来观测活化后的煤沥青基球形活性炭及负载后的微观形貌。
图2和图3为V2O5/煤沥青基球形活性炭的扫描电镜图。绝大部分五氧化二钒都被负载到沥青的表面，煅烧并氧化后V2O5/煤沥青基球形活性炭表面有脱落现象，这是由于煤沥青基球形活性炭浸泡在五氧化二钒的溶液中，干燥前，球表面会附载一层五氧化二钒，随着温度的升高，液体五氧化二钒逐渐变干，但是温度过高，纳米级二氧化钛就会脱落。
图4，图5、图6和图7为V2O5/煤沥青基球形活性炭的EDS分析。可以看出钒元素分布在球表面上，同时表面上还可以检测到大量的炭元素，氧元素占少部分，表明钒元素已经成功包裹在碳球表面。
图8为V2O5/煤沥青基复合球形活性炭的杀菌性能评价图。由图知，太阳光下，V2O5/煤沥青基复合球形活性炭对水中细菌的杀菌效果明显，而太阳光作为一种自然资源，被国际公认为未来最具竞争性的能源之一。
以上所述，仅为本发明较佳的具体实施方式，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 (5)
1.一种V2O5/煤沥青基复合球形活性炭的制备方法，其特征在于包括以下步骤：
1)煤沥青基球形活性炭的制备；
2)五氧化二钒溶液的制备
将五氧化二钒3-5g、聚乙烯吡咯烷酮0.5-1g、乙二醇20-40ml、吡啶80-120ml、无水乙醇20-40ml和去离子水50-200ml混合，在水浴锅中磁力搅拌并加热到80-100℃，冷凝回流至五氧化二钒固体全部溶解，冷却至室温制得五氧化二钒溶液；
3)V2O5/煤沥青基复合球形活性炭的制备
采用沉浸法将五氧化二钒溶液负载到煤沥青基球形活性炭表面，将负载后的煤沥青基球形活性炭置于管式炉中，在空气条件下，从室温升至200-500℃，用时1-4小时，再在200-500℃恒温1-4小时；待自然冷却后取出即得。
2.根据权利要求1所述V2O5/煤沥青基复合球形活性炭的制备方法，其特征在于所述煤沥青基球形活性炭的制备包括如下步骤：
a.取吡啶溶液对煤焦油中温沥青进行索氏抽提、冷却、抽滤收取滤液；
b.称取聚乙烯醇，无水乙醇和去离子水于烧瓶中混匀后置于水浴锅中磁力搅拌并加热，确保聚乙烯醇完全溶解后，冷却至室温；
c.将冷却好的吡啶抽提溶液倒入容器，并超声震荡；
d.将超声后的混合溶液在80-90℃下进行热搅拌，温度达80-90℃时再恒温搅拌15-35分钟；
E.将搅拌后的溶液冷却至室温、抽滤得到煤沥青球；
F.不熔化处理
将煤沥青球放入管式炉中，在空气条件下，温度从常温升至250-350℃，用时30-40小时，再在250-350℃恒温2-5小时，待自然冷却取出样品；
g.炭化处理
将装有不熔化处理后的煤沥青球的陶瓷舟放置于管式炉中，在氮气气氛下炭化；
h.活化
取KOH加入到炭化后的煤沥青基球形活性炭中，在90-120℃真空干燥，最后将干燥后的小球放入管式炉中；在氮气气氛下，先从常温升至350-450℃，用时1-3小时，再在350-450℃恒温0.5-1.5小时，再从350-450℃升温到700-800℃，用时2-4小时，再在700-800℃恒温0.5-1.5小时；待自然冷却后取出样品，用盐酸和去离子水冲洗至中性，干燥即得煤沥青基球形活性炭。
3.根据权利要求1所述V2O5/煤沥青基复合球形活性炭的制备方法，其特征在于：所述中温沥青的软化点为65～90℃。
4.一种根据权利要求1-3任意一项所述V2O5/煤沥青基复合球形活性炭的制备方法制得的V2O5/煤沥青基复合球形活性炭，特特征在于：为多孔炭材料，表面粗糙部分为负载的五氧化二钒，内部呈球形的成分为煤沥青。
5.一种根据权利要求1-3任意一项所述V2O5/煤沥青基复合球形活性炭的制备方法制得的V2O5/煤沥青基复合球形活性炭的应用，其特征在于：用于废水除菌处理。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112791699A (zh) * | 2021-01-20 | 2021-05-14 | 辽宁科技大学 | 一种ZrO2/煤沥青基复合活性炭球的制备方法 |
| CN113209959A (zh) * | 2021-05-12 | 2021-08-06 | 昆明理工大学 | 一种负载型棒状氧化镁复合抗菌剂的制备方法 |
| CN113528174A (zh) * | 2021-07-28 | 2021-10-22 | 辽宁科技大学 | 一种直径为15～80μm的V2O5/复合煤沥青球的制备方法 |
| CN113955802A (zh) * | 2021-09-22 | 2022-01-21 | 辽宁科技大学 | 三维多级结构锂离子电池v2o5@c正极材料的制备方法 |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006110470A (ja) * | 2004-10-14 | 2006-04-27 | Ueda Shikimono Kojo:Kk | 水質浄化剤 |
| KR20060104346A (ko) * | 2005-03-30 | 2006-10-09 | 유은영 | 목탄필터 |
| CN104194758A (zh) * | 2014-09-23 | 2014-12-10 | 兰州熙瑞化工科技有限公司 | 油田采油井中性解堵剂组合物及其制备方法 |
| CN104307473A (zh) * | 2014-10-21 | 2015-01-28 | 同济大学 | 一种用于空气污染治理的吸附可见光催化材料的制备方法 |
| CN104474552A (zh) * | 2014-11-24 | 2015-04-01 | 浙江大学 | 多功能多层微/纳米核壳结构的制备方法 |
| CN106084817A (zh) * | 2016-06-13 | 2016-11-09 | 山东交通学院 | 一种具有光催化降解尾气排放物功能的沥青材料及其制备方法 |
| CN106242136A (zh) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | 一种含吡啶类废水的处理方法 |
| CN106955650A (zh) * | 2017-04-01 | 2017-07-18 | 东华大学 | 一种三维多孔框架增强纤维气凝胶材料及其制备方法 |
| CN108832078A (zh) * | 2018-05-16 | 2018-11-16 | 辽宁科技大学 | 一种Fe3O4/Fe-煤沥青基复合球形活性炭的制备方法 |
| CN109250716A (zh) * | 2018-12-05 | 2019-01-22 | 宁波设会物联网科技有限公司 | 一种沥青基空心球形活性炭的制备方法 |
-
2019
- 2019-12-09 CN CN201911251210.7A patent/CN111097383B/zh active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006110470A (ja) * | 2004-10-14 | 2006-04-27 | Ueda Shikimono Kojo:Kk | 水質浄化剤 |
| KR20060104346A (ko) * | 2005-03-30 | 2006-10-09 | 유은영 | 목탄필터 |
| CN104194758A (zh) * | 2014-09-23 | 2014-12-10 | 兰州熙瑞化工科技有限公司 | 油田采油井中性解堵剂组合物及其制备方法 |
| CN104307473A (zh) * | 2014-10-21 | 2015-01-28 | 同济大学 | 一种用于空气污染治理的吸附可见光催化材料的制备方法 |
| CN104474552A (zh) * | 2014-11-24 | 2015-04-01 | 浙江大学 | 多功能多层微/纳米核壳结构的制备方法 |
| CN106084817A (zh) * | 2016-06-13 | 2016-11-09 | 山东交通学院 | 一种具有光催化降解尾气排放物功能的沥青材料及其制备方法 |
| CN106242136A (zh) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | 一种含吡啶类废水的处理方法 |
| CN106955650A (zh) * | 2017-04-01 | 2017-07-18 | 东华大学 | 一种三维多孔框架增强纤维气凝胶材料及其制备方法 |
| CN108832078A (zh) * | 2018-05-16 | 2018-11-16 | 辽宁科技大学 | 一种Fe3O4/Fe-煤沥青基复合球形活性炭的制备方法 |
| CN109250716A (zh) * | 2018-12-05 | 2019-01-22 | 宁波设会物联网科技有限公司 | 一种沥青基空心球形活性炭的制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| TAIPING XIE ET AL: ""Synthesis of multifunctional photocatalyst vanadium oxide/activated carbon via in situ utilization of stone coal ore"", 《CERAMICS INTERNATIONAL》 * |
| 廖婷: ""石煤提制活性炭及五氧化二钒/活性炭复合光催化剂的性能研究"", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112791699A (zh) * | 2021-01-20 | 2021-05-14 | 辽宁科技大学 | 一种ZrO2/煤沥青基复合活性炭球的制备方法 |
| CN113209959A (zh) * | 2021-05-12 | 2021-08-06 | 昆明理工大学 | 一种负载型棒状氧化镁复合抗菌剂的制备方法 |
| CN113209959B (zh) * | 2021-05-12 | 2023-01-24 | 昆明理工大学 | 一种负载型棒状氧化镁复合抗菌剂的制备方法 |
| CN113528174A (zh) * | 2021-07-28 | 2021-10-22 | 辽宁科技大学 | 一种直径为15～80μm的V2O5/复合煤沥青球的制备方法 |
| CN113955802A (zh) * | 2021-09-22 | 2022-01-21 | 辽宁科技大学 | 三维多级结构锂离子电池v2o5@c正极材料的制备方法 |
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