CN116651400A - 一种改性烟蒂活性炭微球的制备方法及其在吸附氨中的应用 - Google Patents
一种改性烟蒂活性炭微球的制备方法及其在吸附氨中的应用 Download PDFInfo
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- CN116651400A CN116651400A CN202310785490.XA CN202310785490A CN116651400A CN 116651400 A CN116651400 A CN 116651400A CN 202310785490 A CN202310785490 A CN 202310785490A CN 116651400 A CN116651400 A CN 116651400A
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- activated carbon
- ammonia
- cigarette butt
- butts
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 163
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 77
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 69
- 239000004005 microsphere Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 title abstract description 92
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 22
- 239000011159 matrix material Substances 0.000 claims abstract description 15
- 239000012043 crude product Substances 0.000 claims abstract description 14
- 238000000197 pyrolysis Methods 0.000 claims abstract description 13
- 239000002912 waste gas Substances 0.000 claims abstract description 13
- 230000004913 activation Effects 0.000 claims abstract description 11
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- 239000002351 wastewater Substances 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000002699 waste material Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 230000004048 modification Effects 0.000 claims description 18
- 238000012986 modification Methods 0.000 claims description 18
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 17
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 11
- 229910001510 metal chloride Inorganic materials 0.000 claims description 11
- 238000001994 activation Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- 229960002337 magnesium chloride Drugs 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- 241000208125 Nicotiana Species 0.000 claims description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 229960001939 zinc chloride Drugs 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 21
- 238000005470 impregnation Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 23
- 230000000694 effects Effects 0.000 description 20
- 238000004064 recycling Methods 0.000 description 7
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- 230000001788 irregular Effects 0.000 description 6
- 238000011069 regeneration method Methods 0.000 description 6
- 230000001747 exhibiting effect Effects 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 239000012190 activator Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical class N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 238000009656 pre-carbonization Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 nickel chloride Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开一种改性烟蒂活性炭微球的制备方法及其在吸附氨中的应用。先在磷酸存在的条件下进行水热反应获得固体一次球化炭基质,再通过热解炭化活化得到球状活性炭粗品,然后进行金属盐浸渍获得改性烟蒂活性炭微球,所得产品具有介孔结构和球状形貌,微球的直径为1~30微米,微球上的孔径主要分布在2~30纳米的范围。本发明所得产品用于吸附氨气,吸附容量高达6.0mmol/g~8.0mmol/g,能够为改善排放的含氨氮的废水质量或含氨的废气质量提供一种有效可行的便捷方式,具有良好的应用前景。
Description
技术领域
本发明涉及生物炭的制备及应用,特别涉及一种改性烟蒂活性炭微球的制备方法及其在吸附氨中的应用。
背景技术
NH3和NH4+是对环境影响最为严重的含氮物种。水体中含氮化合物的含量提升会导致富营养化,影响饮用水质量。排入大气的氨与NOX和SO2一起反应产生的硝酸铵或硫酸铵盐,是形成雾霾的重要因素。大气中的NH3具有强烈的刺激性,对人体呼吸道、眼睛等造成损伤。随着人口的增长和人为活动的增加,全球氨排放量急剧增加。与此同时,氨作为一种重要的化肥与工业原料,在制药、农业和化工等领域有着大规模应用,甚至可以部分代替化石燃料作为低碳能源使用。因此,含氨废气和废水的净化、氨的分离和储存具有很强的现实需求,高效的吸附材料和技术受到广泛关注。
据统计,世界上每年香烟消费量巨大,多达4.95万亿个烟蒂被丢弃于环境中。烟蒂在自然环境中很难降解,烟蒂中的微量重金属中会随着雨水浸出而进入土壤和水体,不仅对自然环境造成污染,而且对人类和生态中生物构成了健康威胁。因此,将废弃烟蒂制成活性炭吸附材料用于净化环境中的污染物,能够实现以废治废,受到欢迎。
中国发明CN109173994A提供了一种高温炭化改性废弃烟蒂制备生物炭的方法以及生物炭的应用,其制备方法包括水热炭化、高温热解活化和酸处理等步骤,所得生物炭作为吸附剂在不同pH条件下去除水体中的双酚A即BPA,具有明显的选择性。中国发明专利CN111003709B公开了一种利用废弃烟蒂制备活性炭的方法及制得的活性炭,所述方法包括废弃烟蒂的热解预炭化、活化和热解炭化等步骤,其通过优化预炭化的条件,将烟蒂中纤维丝束和焦油预炭化,从而获得较佳的活性炭的比表面积、中孔率和活性炭的得率。
上述将烟蒂制成活性炭吸附材料的技术方案确实在某些性能上获得了较好的提升,但所得活性炭更适用于吸附净化水体中的有机物和重金属,所得活性炭形貌结构不规则,进一步改性获得均匀活性位点的难度大,性质较单一且不稳定,尚不能在吸附氨中获得好的吸附效果。
发明内容
针对现有烟蒂活性炭形貌结构不规则,性质较单一且不稳定,吸附氨效果较差等技术问题,本发明提供一种改性烟蒂活性炭微球的制备方法及其在吸附氨中的应用。
本发明提供的改性烟蒂活性炭微球的制备方法,包括如下步骤:
(1)水热反应成球:将废弃烟蒂、水或/和磷酸溶液放入反应釜中搅拌混合,通过水热反应制得水热碳悬浮液,水热反应的温度为200℃~300℃,时间为0.5h~3h,固液分离得到固体一次球化炭基质;
(2)热解碳化活化:将步骤(1)所得一次球化炭基质直接干燥或者先和磷酸溶液均匀混合后再进行干燥,然后在保护气氛下500℃~800℃高温热解0.5h~2h,冷却后得到球状活性炭粗品;
(3)金属氯化物改性:将步骤(2)所得球状活性炭粗品进行洗涤后烘干,然后放入金属氯化物溶液中进行改性,干燥后得到改性烟蒂活性炭微球。
进一步地,步骤(1)中,废弃烟蒂为去除残留烟丝的烟蒂头,优选去除外包装纸的烟蒂。
进一步地,步骤(1)中,水热反应优选加入催化剂,催化剂为葡萄糖或/和纤维素,催化剂的用量为烟蒂质量的0.1~5%。
进一步地,步骤(1)中,废弃烟蒂与体系中水的用量为1g:(5~20ml),体系中的水包括直接加入的水或/和磷酸溶液中的水;水热反应的温度为200℃~300℃,优选225~248℃或250~270℃;时间为0.5h~3h。
进一步地,步骤(1)中,固液分离得到液相转入下一批次的水热反应,实现包括催化剂在内的物料的充分利用。
进一步地,步骤(2)中,热解的温度为580~720℃,时间为1~1.5h。
进一步地,步骤(1)和步骤(2)至少一个步骤中加入磷酸溶液,磷酸的总用量为废弃烟蒂质量的0.5~5倍,步骤(1)中加入磷酸溶液,能够一定程度上促进水热反应的进行,同时又能够为后续的活化做准备,因此在步骤(1)中先加入磷酸,是更优的选择,更优选地,步骤(1)中加入磷酸总用量的50%~100%,即步骤(1)中可以直接加入活化所需的全部磷酸或者部分磷酸,当步骤(1)加量不足时,剩余量在步骤(2)中补充加入。
进一步地,步骤(3)中,金属氯化物选自氯化镁、氯化锰、氯化亚铁、氯化锌和氯化镍中的一种或两种以上,金属氯化物溶液的质量分数为5%~30%,金属氯化物的用量为球状活性炭粗品质量的20%~200%。
进一步地,步骤(3)中,改性在搅拌或/和超声条件下进行,搅拌转速为250~500r/min,超声为20~40min。
上述制备方法得到的改性烟蒂活性炭微球具有介孔结构,微球的直径为1~30微米,微球上的孔径主要分布在2~30纳米的范围。
上述制备方法得到的改性烟蒂活性炭微球用于吸附氨,可以去除废水中的氨氮或含氨废气中的氨气,能够取得良好的吸附效果,尤其是含氨废气中氨气的吸附效果更为显著。
本发明的有益效果在于:
本发明以对环境有污染的废弃烟蒂作为原料制备得到介孔的改性烟蒂活性炭微球,制备工艺产率稳定、生产成本较低,所得产物还具有比表面积大、活性成分负载均匀、吸附氨效果好、容易再生循环使用等优点,实现了废弃烟蒂的资源化利用。
本发明先通过水热炭化成球,再进行高温热解活化,然后进行金属盐浸渍获得改性烟蒂活性炭微球,具有介孔结构和球状形貌,微球的直径为1~30微米,微球上的孔径主要分布在2~30纳米的范围。氯化物改性工序本身并非本发明的原创,然而本发明在获得球状活性炭粗品后,通过氯化物改性,明显放大了所得产物在氨吸附中的应用效果,氯化物改性尤其是氯化镍等氯化物的改性,能够显著提升所得产物的氨吸附效果。此外,本发明通过在水热过程中加入催化剂和活化所需的部分磷酸或者全部磷酸,不仅能够促进水热反应的发生,强化水热反应的效果,更好地保障球状形貌的获得,而且能够进一步提升所得产物吸附氨的效果,从而所得产物更加适用于氨吸附,氨吸附容量高达6.0mmol/g~8.0mmol/g,能够为改善排放的含氨氮的废水质量或含氨的废气质量提供一种有效可行的便捷方式,具有良好的应用前景。
附图说明
图1为本发明的工艺流程示意图。
图2为对比例1所得SFC的扫描电镜图,由图可知,水热反应一次成球碳基质具有初步的球状形貌。
图3为实施例1所得SFC-20%的扫描电镜图。
图4为实施例6的氨气吸附的效果图。
图5为实施例7的氨气吸附的效果图。
图6为实施例8的氨气吸附的效果图。
图7为实施例9的氨气吸附的效果图。
图8为实施例10的氨气吸附的效果图。
图9为实施例11的样品再生的效果图。
图10为不规则改性活性炭样品SFC-D2的扫描电镜图,由图可知,SFC-D2具有不规则形貌。
具体实施方式
下面结合附图和具体实施例对本发明做进一步详细说明,但本发明并不限于此。
实施例1
一种改性烟蒂活性炭微球的制备方法,按照以下步骤进行:
(1)将废弃烟蒂的外包装纸去掉,洗净干燥后放入水热釜中,按照废弃烟蒂与水的体积比为1g:10ml,向水热釜中加入水、催化剂葡萄糖和磷酸溶液,催化剂葡萄糖和磷酸的质量分别为废弃烟蒂质量的1%和50%,使用水热法240℃碳化2h,固液分离得到固体,即一次球化炭基质;
(2)将步骤(1)制备的一次球化炭基质和废气烟蒂质量50%的磷酸溶液均匀混合后进行干燥,然后在氮气保护下进行600℃高温热解1h,然后在保护气保护下随炉冷却至室温,得到球状活性炭粗品;
(3)将步骤(2)得到的球状活性炭粗品洗涤后用质量分数为20%(又称质量浓度)的氯化镍溶液进行浸渍改性,超声震荡30min使氯化镍沉淀分布均匀于球状活性炭粗品,随后干燥,得到改性烟蒂活性炭微球,所得样品记为SFC-20%。
实施例2
其余与实施例1相同,与实施例1不同的是:步骤(3)中的氯化镍溶液的质量分数为5%,所得改性烟蒂活性炭微球记为SFC-5%。
实施例3
其余与实施例1相同,与实施例1不同的是:步骤(3)中的氯化镍溶液的质量分数为10%,所得改性烟蒂活性炭微球记为SFC-10%。
实施例4
其余与实施例1相同,与实施例1不同的是:步骤(3)中的氯化镍溶液的质量分数为15%,所得改性烟蒂活性炭微球记为SFC-15%。
实施例5
其余与实施例1相同,与实施例1不同的是:步骤(3)中的氯化镍溶液的质量分数为30%,所得改性烟蒂活性炭微球记为SFC-30%。
对实施例1至5制备的改性烟蒂活性炭微球分别进行表征,表1是五种改性烟蒂活性炭微球的表征数据和平衡吸附容量。如数据所示,随着氯化镍溶液的质量浓度由5%升高至30%,样品比表面积随之减小。五种改性烟蒂活性炭微球的孔径都分布在2~20nm,峰值在3.7左右,而氨的分子尺寸为0.3nm,可以很顺利地通过吸附作用在孔道内进行吸附。
表1为各样品测试数据
实施例6
改性烟蒂活性炭微球应用于去除含氨废气中的氨气:将实施例1至5制备的改性烟蒂活性炭微球分别进行氨吸附试验。吸附条件为氨气浓度400ppm、吸附温度30℃、总气速为0.8L/min。使用氨检测仪记录突破时间,突破之后每30s记一次数据,平行测试两次,取平均值。如图4所示,曲线1为SFC-20%、曲线2为SFC-5%、、曲线3为SFC-10%、曲线4为SFC-15%、曲线5为SFC-30%。随着浸渍改性浓度由5%提升到20%,突破时间也延长至87min,最高平衡吸附容量(氨吸附饱和容量)达到6.15mmol/g,吸附氨的性能明显提高。
实施例7
改性烟蒂活性炭微球应用于去除含氨废气中的氨气:将实施例6中表现最高平衡吸附容量的样品SFC-20%放置在不同氨气浓度的条件下进行氨吸附试验。其它吸附条件与实施例6相同,调整氨气浓度为200ppm、300ppm、400ppm、500ppm。如图5所示,曲线6为200ppm、曲线7为300ppm、、曲线8为400ppm、曲线9为500ppm。NH3浓度由200ppm增加到500ppm,试验值的吸附速率(即斜率)是逐渐增加的,同时根据曲线计算得到的NH3吸附容量由3.87mmol/g增加到6.78mmol/g,说明该材料对氨浓度负荷变化的适应性很强。
实施例8
改性烟蒂活性炭微球应用于去除含氨废气中的氨气:将实施例6中表现最高平衡吸附容量的样品SFC-20%放置在不同吸附温度的条件下进行氨吸附试验。其它吸附条件与实施例6相同,调整吸附温度为30℃、50℃、70℃、90℃。如图6所示,曲线10为30℃、曲线11为50℃、曲线12为70℃、曲线13为90℃。吸附温度50℃下,平衡吸附容量最高为7.83mmol/g。吸附温度由30℃上升到50℃,平衡容量增加了25%,突破时间和饱和时间右移。温度升高到90℃,突破时间和饱和时间迅速减少40%,可以看到,温度由70℃升高到90℃,突破时间和饱和时间出现小幅的下降,仅3%。
实施例9
改性烟蒂活性炭微球应用于去除含氨废气中的氨气:将实施例6中表现最高平衡吸附容量的样品SFC-20%放置在不同吸附温度的条件下进行氨吸附试验。其它吸附条件与实施例6相同,调整总气速为0.4L/min、0.6L/min、0.8L/min、1.0L/min。如图7所示,曲线14为0.4L/min、曲线15为0.6L/min、曲线16为0.8L/min、曲线17为1.0L/min。总气速由0.4L/min增加到1.0L/min,试验值吸附速率逐渐增加,对应平衡吸附容量从3.44mmol/g升高至6.12mmol/g,说明该材料对气量负荷变化的适应性也很强。
实施例10
改性烟蒂活性炭微球应用于去除含氨废气中的氨气:将实施例6中表现最高平衡吸附容量的样品SFC-20%放置在不同吸附温度的条件下进行氨吸附试验。其它吸附条件与实施例6相同,调整水汽含量为5%、15%、30%、60%。如图8所示,曲线18为5%、曲线19为15%、曲线20为30%、曲线21为60%。可以发现,水汽含量对样品吸附氨具有较大的影响,其突破曲线的变化可以看出,在高水汽含量的条件下如60%,突破时间和饱和时间相对于5%的水汽含量提高了30%。该实验说明水份是有利于氨在该材料上的吸附或吸收的,故将这一材料用于处理废水中的氨氮也会有不错的效果。
实施例11
改性烟蒂活性炭微球应用于去除含氨废气中的氨气:将实施例6中表现最高平衡吸附容量的样品SFC-20%进行再生试验。调整再生温度为90℃、110℃、130℃、150℃。如图9所示,曲线22为90℃、曲线23为110℃、曲线24为130℃、曲线25为150℃。比较可知,在130℃条件下进行样品再生,脱附量最高。经过5次吸附-再生循环测试后,样品吸附容量仅下降19%,说明回用性能较稳定,可显著降低运行成本。
实施例12
其余与实施例3相同,与实施例3不同的是:步骤(3)中的氯化镍溶液换为氯化镁溶液。
按照实施例6的方法对实施例3和实施例12所得产品分别进行氨吸附试验,实验结果表明,实施例3所得产品的氨吸附饱和容量为3.97mmol/g,实施例12所得产品的氨吸附饱和容量为2.38mmol/g。
实施例13
其余与实施例3相同,与实施例3不同的是:步骤(3)中的氯化镍溶液换为氯化锰溶液。
按照实施例6的方法进行氨吸附试验,实验结果表明,实施例13所得产品的氨吸附饱和容量为2.36mmol/g。
实施例14
其余与实施例3相同,与实施例3不同的是:步骤(3)中的氯化镍溶液换为氯化亚铁溶液。
按照实施例6的方法进行氨吸附试验,实验结果表明,实施例14所得产品的氨吸附饱和容量为3.33mmol/g。
实施例15
其余与实施例3相同,与实施例3不同的是:步骤(3)中的氯化镍溶液换为氯化锌溶液。
按照实施例6的方法进行氨吸附试验,实验结果表明,实施例15所得产品的氨吸附饱和容量为2.35mmol/g。
不浸渍改性所得产品的氨吸附饱和容量小于2.11mmol/g,由此可以得知,上述金属氯化物改性后均能提升吸附性能。
实施例16
其余与实施例1相同,与实施例1不同的是:磷酸溶液全部在步骤(1)中加入。
按照实施例6的方法进行氨吸附试验,实验结果表明,实施例16所得产品的氨吸附饱和容量为8.04mmol/g。
实施例17
其余与实施例1相同,与实施例1不同的是:磷酸溶液全部在步骤(2)中加入。
按照实施例6的方法进行氨吸附试验,实验结果表明,实施例17所得产品的氨吸附饱和容量为6.02mmol/g。
通过实施例16和实施例17的实验数据对比,可以看出,活化剂磷酸在水热反应的步骤(1)完全加入,能够体现出明显更好的氨吸附效果。磷酸作为活化剂,在需要进行活化时加入是更为常规的操作。本发明通过在水热反应时先行加入活化剂磷酸,能够使得最终产物获得更好的氨吸附效果。
实施例18
改性烟蒂活性炭微球应用于去除废水中的氨氮:将实施例1至3制备的改性烟蒂活性炭微球分别进行批式吸附试验。称量0.2g改性烟蒂活性炭微球放入50mL硫酸铵配置的100mg/L~1000mg/L模拟氨氮废水中,在20℃下控制搅拌速率200转/min反应24h(至浓度基本无变化)。取水样过滤后用纳氏试剂分光光度法测定滤液中的氨氮浓度,得到对应条件下的吸附平衡浓度,分别获得3种活性炭样品的等温吸附曲线。然后根据朗格缪尔模型拟合,计算得到活性炭SFC-5%、SFC-10%、SFC-20%对氨氮的最大吸附容量分别为4.87mmol/L、6.08mmol/g和8.32mmol/g,表明吸附水中氨氮的性能良好。
对比例1
其余与实施例1相同,不同的是:不进行步骤(3)的浸渍改性,所得产品记为SFC。
按照实施例6的方法进行氨吸附试验,实验结果表明,氨吸附饱和容量为2.11mmol/g。
由实施例6可知,同等条件下,采用氯化镍进行浸渍改进所得产品的氨吸附饱和容量为6.15mmol/g,因此在改性烟蒂活性炭微球去除含氨废气中氨气的应用中,氯化镍改性提升吸附性能特别显著,提升幅度高达191%。该数据表明,氯化物尤其是氯化镍的改性特别适用于去除氨的应用,提升效果极为显著。
对比例2
将废弃烟蒂的外包装纸去掉,放入水热釜中,按照废弃烟蒂与水的体积比为1g:6ml,向水热釜中加入水,升温到200℃水热反应50min左右,固液分离得到无定型的固体炭基质;将其按照与实施例1第(2)步骤一样的条件进行磷酸活化与碳化处理,得到不规则的生物炭粗品SFC-D1。将该粗品按照实施例1第(3)步骤一样的条件进行浸渍改性,得到不规则改性活性炭样品SFC-D2,SFC-D2的电镜扫描图如图10所示,由图10可知,SFC-D2具有不规则形貌。
按照实施例6的方法进行氨吸附试验,实验结果表明,样品SFC-D1和SFC-D2的氨吸附饱和容量为0.80mmol/g和3.20mmol/g。经过130℃脱附再生然后回用吸附,经过5次吸附-再生循环后测试,样品SFD2的吸附容量下降达34%左右,说明不规则活性炭样品回用性能不太稳定,而本发明所得形貌规则的改性烟蒂活性炭微球体现了良好的回用性能或稳定性能(如实施例11的结果所示)。由实施例1和对比例1可知,同等条件下,未改性的活性炭微球样品SFC的饱和容量为2.11mmol/g,比不规则形貌产品SFC-D1的氨吸附饱和容量有明显提高,进一步改性提升吸附性能及回用稳定性的潜力更大。
Claims (10)
1.一种改性烟蒂活性炭微球的制备方法,其特征在于,包括如下步骤:
(1)水热反应成球:将废弃烟蒂、水或/和磷酸溶液放入反应釜中搅拌混合,通过水热反应制得水热碳悬浮液,水热反应的温度为200℃~300℃,时间为0.5h~3h,固液分离得到固体一次球化炭基质;
(2)热解炭化活化:将步骤(1)所得一次球化炭基质直接干燥或者先和磷酸溶液均匀混合后再进行干燥,然后在保护气氛下500℃~800℃高温热解0.5h~2h,冷却后得到球状活性炭粗品;
(3)金属氯化物改性:将步骤(2)所得球状活性炭粗品进行洗涤后放入金属氯化物溶液中进行改性,干燥后得到改性烟蒂活性炭微球。
2.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(1)中,所述的废弃烟蒂为去除残留烟丝的烟蒂头。
3.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(1)中,所述水热反应加入催化剂,所述催化剂为葡萄糖或/和纤维素,所述催化剂的用量为烟蒂质量的0.1~5%。
4.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(1)中,废弃烟蒂与体系中水的用量为1g:(5~20ml);所述水热反应的温度为225℃~248℃或250℃~270℃。
5.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(1)中,固液分离得到液相转入下一批次的水热反应,实现包括催化剂在内的物料的充分利用。
6.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(2)中,所述热解的温度为580~720℃,时间为1~1.5h;步骤(3)中,所述改性在搅拌或/和超声条件下进行,搅拌转速为250~500r/min,超声时间10~60min。
7.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(1)和步骤(2)至少一个步骤中加入磷酸溶液,磷酸的总用量为废弃烟蒂质量的0.5~5倍。
8.如权利要求1所述的改性烟蒂活性炭微球的制备方法,其特征在于,步骤(3)中,所述金属氯化物为氯化镁、氯化锰、氯化亚铁、氯化锌和氯化镍中的一种或两种以上,所述金属氯化物溶液的质量分数为5%~30%,金属氯化物的用量为球状活性炭粗品质量的20%~200%。
9.如权利要求1至8任一项所述的制备方法得到的改性烟蒂活性炭微球,其特征在于,所述改性烟蒂活性炭微球具有介孔结构,直径为1~30微米,孔径分布在2~30纳米。
10.如权利要求9所述的改性烟蒂活性炭微球在吸附氨中的应用,所述氨为废水中的氨氮或含氨废气中的氨气。
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