CN116409778A - 一种聚氯乙烯无害化高附加值处理方法及应用 - Google Patents
一种聚氯乙烯无害化高附加值处理方法及应用 Download PDFInfo
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- CN116409778A CN116409778A CN202310397060.0A CN202310397060A CN116409778A CN 116409778 A CN116409778 A CN 116409778A CN 202310397060 A CN202310397060 A CN 202310397060A CN 116409778 A CN116409778 A CN 116409778A
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- polyvinyl chloride
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- asphalt
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 49
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 28
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- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000010426 asphalt Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
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- 230000000382 dechlorinating effect Effects 0.000 claims abstract description 9
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 4
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 3
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- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
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- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
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- 235000006408 oxalic acid Nutrition 0.000 claims description 2
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- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000006298 dechlorination reaction Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
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- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 2
- 229910039444 MoC Inorganic materials 0.000 description 2
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- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
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- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
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Abstract
本发明公开了一种聚氯乙烯无害化高附加值处理方法及应用。所述的聚氯乙烯无害化高附加值处理方法,包括如下步骤:将聚氯乙烯和脱氯剂加入到分散剂中,超声分散后,加入沥青,充分搅拌混合,在一定温度下反应一定时间后,经过滤,洗涤,干燥后得到前体。前体在惰性气体存在条件下经热处理后得到无序碳材料;或者前体在活化剂存在条件下经活化处理后得到多孔炭材料。本发明优点在于聚氯乙烯和沥青通过简单处理后,实现了聚氯乙烯的脱氯减毒,经过炭化或者炭化‑活化分别制成无序碳和多孔炭,成功实现聚氯乙烯和沥青的高附加值利用,并且制得的无序炭和多孔炭性能优异。
Description
技术领域
本发明属于化工和环境保护领域,具体涉及一种聚氯乙烯无害化高附加值处理方法及应用。
背景技术
聚氯乙烯是一种性能优异的聚合材料,广泛应用于包装、建筑以及家具等行业。然而,由于聚氯乙烯广泛应用导致全球每年产生大量的废聚氯乙烯,目前对废塑料的处理方法主要有焚烧、填埋以及微生物分解,其中焚烧过程中氯化氢的释放和四氯二苯并对二恶英的形成可能造成二次环境污染,填埋处理会造成对土壤的破坏和地下水资源的污染,而微生物分解过程条件苛刻以及效率低下,以至于废聚氯乙烯无法得到合理有效的回收与资源化利用。聚氯乙烯是一种氯代烃,因此其是一种优良的反应前体。与此同时,全球每年也会产生大量沥青(例如煤沥青、石油沥青以及煤液化沥青),这些重质有机物具有芳香度高,碳含量高以及反应活性高等特点。但是目前主要用于建筑行业(例如铺路、防水涂料等),这无法发挥废聚氯乙烯的优异特性以实现其高附加值利用。中国专利CN109368646A公开了一种基于废聚氯乙烯制备碳化钼纳米材料的方法,将含钼化合物、废聚氯乙烯、金属钠和/或镁按照一定比例置于反应器中,后在电炉中加热,反应结束后将产物进行处理后成功制得碳化钼纳米材料。中国专利CN111359581B公开了一种利用废聚氯乙烯塑料制备重金属吸附剂的方法,将废旧聚氯乙烯塑料进行粉碎后,加入催化剂反应后得到水热碳化产物,经过硫酸磺化后得到磺化碳化产物,最后对磺化碳化产物活化得到具有重金属吸附性能的吸附剂。上述方法制备过程相对复杂以及收率较低,这也导致成本较高。
因此,针对于现有技术不足,本发明利用聚氯乙烯以及沥青的诸多优异性质,提出一种操作简单、绿色环保且高效的聚氯乙烯无害化高附加值处理方法及应用。
发明内容
本发明的目的是提供了一种聚氯乙烯无害化高附加值处理方法及应用。
本发明目的是通过以下方式实现:
一种聚氯乙烯无害化高附加值处理方法,其主要包括以下步骤:
将聚氯乙烯和脱氯剂加入到分散剂中,超声分散后,加入沥青,充分搅拌混合,在一定温度下反应一定时间后,经过滤,洗涤,干燥后得到前体。前体在惰性气体存在条件下经热处理后得到无序碳材料;或者前体在活化剂存在条件下经活化处理后得到多孔炭材料。
进一步的,所述的沥青选自煤系沥青或石油沥青中的一种或两种,较优的为煤沥青。
进一步的,所述分散剂为二硫化碳、1,2-二氯乙烷、氯仿或四氯化碳中的一种或两种以上,较优的为1,2-二氯乙烷。
进一步的,所述脱氯剂为无水三氯化铁、无水三氯化铝、无水四氯化锡、浓硫酸、三氟甲磺酸、对甲基苯磺酸、草酸中的一种或两种以上,较优的为无水三氯化铁。
进一步的,所述聚氯乙烯与沥青的质量比为5:1~45。
进一步的,所述聚氯乙烯与脱氯剂的质量比为5:1~45。
进一步的,所述聚氯乙烯与分散剂的质量比为5:1~5000。
进一步的,所述反应温度为20~200℃,反应时间为1~60h。
进一步的,所述干燥条件为:真空50~140℃下干燥1~60h。
进一步的,所述惰性气体为氮气、氩气或氦气中的一种或两种以上;所述活化剂为水蒸气、二氧化碳、氧气、空气、氢氧化钾或氢氧化钠中的一种或两种以上混合,较优的为二氧化碳。
进一步的,所述惰性气体流量为10~100000mL/min。
进一步的,所述热处理温度为300~1600℃,升温速率为2~30℃/min。
进一步的,所述热处理时间为0.1~50h。
进一步的,所述前体与活化剂质量比为10:1~10000。
进一步的,所述活化条件为:活化温度为600~1500℃,升温速率为1~20℃/min,活化时间为0.1~30h。
本发明另一方面在于提供由上述方法制备得到无序炭和多孔炭材料,所述的无序炭材料的d002值大于0.36nm,多孔炭材料比表面积大于500m2/g。
本发明另一方面的在于提供上述无序炭和多孔炭材料的应用。
进一步的,上述无序炭材料可应用于钠离子电池、锂离子电池以及钾离子电池电极材料。
进一步的,上述多孔炭材料可应用于吸附材料、超级电容器电极材料和催化剂载体等领域。
本发明的有益效果:本发明提供了一种聚氯乙烯无害化高附加值处理方法及应用,通过简单处理制得优质前体,后经过热处理或活化制得无序碳和多孔炭。该制备方法能实现了聚氯乙烯的脱氯减毒,以及聚氯乙烯和沥青的高附加值利用,并且耗时短,环境友好,操作简单,生产成本低,收率高,制备得到的无序炭材料钠离子电池性能优异,制备得到的多孔炭材料具有良好的超电性能。
附图说明
为了更清楚地说明本发明实施例,下面将对实施例涉及的附图进行简单地介绍。
图1为实施例6制得样品CP-1300和PC-6h-1300的XRD谱图。
图2为实施例7制得样品CP-900-4h和CP-6h-900-4h的氮气吸-脱附曲线和DFT孔分布曲线,(a)为氮气吸-脱附曲线,(b)为DFT孔分布曲线。
图3为应用例1制得样品PC-6h-1300钠电倍率性能图。
图4为应用例2制得样品CP-6h-900-4h在不同电流密度下,(a)恒流充放电曲线和(b)比电容图。
具体实施方式
下面结合实施例对本发明进行详细的说明,但本发明的实施方式不限于此,显而易见地,下面描述中的实施例仅是本发明的部分实施例,对于本领域技术人员来讲,在不付出创造性劳动性的前提下,获得其他的类似的实施例均落入本发明的保护范围。
实施例1
在室温下,将1.5g聚氯乙烯和13g无水三氯化铁加入150mL的1,2-二氯乙烷中,超声处理2h,然后加入1.5g煤沥青(CP),将混合物置于250mL三口烧瓶中,氮气气氛下,先常温搅拌1h,后升温至80℃搅拌反应6h,反应结束后,将过滤得到固体产物分别经过甲醇和四氢呋喃洗涤,最后在120℃真空烘箱中干燥12h,得到产物A,标记为CP-6h。
实施例2
在室温下,将1.5g聚氯乙烯和13g无水三氯化铁加入150mL的1,2-二氯乙烷中,超声处理2h,然后加入1.5g煤液化沥青(CLA),将混合物置于250mL三口烧瓶中,氮气气氛下,先常温搅拌1h,后升温至80℃搅拌反应6h,反应结束后,将过滤得到固体产物分别经过甲醇和四氢呋喃洗涤,最后在120℃真空烘箱中干燥12h,得到产物B,标记为CLP-6h。
实施例3
在室温下,将1.5g聚氯乙烯和13g无水三氯化铁加入150mL的1,2-二氯乙烷中,超声处理2h,然后加入1.5g石油沥青(PA),将混合物置于250mL三口烧瓶中,氮气气氛下,先常温搅拌1h,后升温至80℃搅拌反应6h,反应结束后,将过滤得到固体产物分别经过甲醇和四氢呋喃洗涤,最后在120℃真空烘箱中干燥12h,得到产物C,标记为PP-6h。
实施例4
在室温下,按照表1中质量比例和反应时间,将聚氯乙烯和13g无水三氯化铁加入150mL的1,2-二氯乙烷中,超声处理2h,加入煤沥青后,将混合物置于250mL三口烧瓶中,氮气气氛下,先常温搅拌1h,后升温至80℃搅拌反应,反应结束后,将过滤得到固体产物分别经过甲醇和四氢呋喃洗涤,最后在120℃真空烘箱中干燥12h,得到产物,分别标记为CP-0.5-6h、CP-2-6h、CP-3-6h、CP-0.5-24h、CP-2-24h、CP-3-24h和CP-24h。
表1质量比及反应时间
实施例5
在室温下,按照表2中脱氯剂种类及质量,将1.5g聚氯乙烯和脱氯剂加入150mL的1,2-二氯乙烷中,超声处理2h,加入1.5g煤沥青后,将混合物置于250mL三口烧瓶中,氮气气氛下,先常温搅拌1h,后升温至80℃搅拌反应6h,反应结束后,将过滤得到固体产物分别经过甲醇和四氢呋喃洗涤,最后在120℃真空烘箱中干燥12h,得到产物D,分别标记为CP-Al-6h、CP-Sn-6h、CP-H-6h、CP-S-6h、CP-D-6h、CP-C-6h。
表2脱氯剂种类及质量
实施例6
取产物CP-6h 1.0g,将其置于管式炉中,在60mL/min的Ar气氛下,以5℃/min的升温速率升温至1300℃,保持2h后自然降温。即得到无序碳材料,标记为CP-6h-1300。作为对比将煤沥青(CP)按照上述方法直接炭化得到的样品记为CP-1300。材料的XRD谱图如附图1所示,结构参数如表3所示。
表3样品CP-1300和PC-6h-1300的结构参数
实施例7
取产物CP-6h 1.0g,将其置于管式炉中,在60mL min-1的Ar气氛下,以10℃/min的升温速率升温至900℃,切换流速为80mL min-1的CO2,活化4h,完成后,切换为60mL/min的Ar气氛,冷却至室温,即得到多孔炭材料,标记为CP-6h-900-4h。作为对比将煤沥青(CP)按照上述方法活化得到的样品记为CP-900-4h。样品的氮气吸脱附图如附图2所示,孔结构参数如表4所示。
表4、样品CP-900-4h和CP-6h-900-4h材料孔结构参数
实施例8
取实施例2~5产物1.0g,将其置于管式炉中,在60mL/min的Ar气氛下,以10℃/min的升温速率升温至1300℃,保持2h后自然降温。即得到无序碳材料。
实施例9
取实施例2~5产物1.0g,将其置于管式炉中,在60mL/min的Ar气氛下,以10℃/min的升温速率升温至900℃,切换流速为80mL/min的CO2,依次活化4h,完成后,切换为60mL/min的Ar气氛,冷却至室温,即得到多孔炭材料。
应用例1
将实施例6的样品作为钠离子电池电极材料进行电化学测试,组装和测试方法按照参考文献[Energy&Fuels[J].2021,35(10):9029-9037]进行。电化学测试结果如附图3所示,0.03A/g的电流密度下,比容量可达270mA h/g,首次库伦效率为60%。
应用例2
将实施例7的样品作为超级电容器电极材料进行电化学测试,组装和测试方法按照参考文献[炭素技术[J].2022,41(1):6-11]进行。测试结果如附图4所示,在0.05A/g电流密度下,比电容为159F/g。
Claims (10)
1.一种聚氯乙烯无害化高附加值处理方法,其特征在于,包括以下步骤:将聚氯乙烯和脱氯剂加入到分散剂中,超声分散后,加入沥青,充分搅拌混合,在一定温度下反应一定时间后,经过滤,洗涤,干燥后得到前体;前体在惰性气体存在条件下经热处理后得到无序碳材料;或者前体在活化剂存在条件下经活化处理后得到多孔炭材料。
2.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述的沥青选自煤系沥青或石油沥青中的一种或两种;所述分散剂为二硫化碳、1,2-二氯乙烷、氯仿或四氯化碳中的一种或两种以上;所述脱氯剂为无水三氯化铁、无水三氯化铝、无水四氯化锡、浓硫酸、三氟甲磺酸、对甲基苯磺酸、草酸中的一种或两种以上。
3.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述聚氯乙烯与沥青的质量比为5:1~45;所述聚氯乙烯与脱氯剂的质量比为5:1~45;所述聚氯乙烯与分散剂的质量比为5:1~5000。
4.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述反应温度为20~200℃,反应时间为1~60h;所述干燥条件为:真空50~140℃下干燥1~60h。
5.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述惰性气体为氮气、氩气或氦气中的一种或两种以上。
6.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述惰性气体流量为10~100000mL/min;所述热处理温度为300~1600℃,升温速率为2~30℃/min;所述热处理时间为0.1~50h。
7.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述活化剂为水蒸气、二氧化碳、氧气、空气、氢氧化钾或氢氧化钠中的一种或两种以上混合。
8.根据权利要求1所述的一种聚氯乙烯无害化高附加值处理方法,其特征在于,所述前体与活化剂质量比为10:1~10000;所述活化条件为:活化温度为600~1500℃,升温速率为1~20℃/min,活化时间为0.1~30h。
9.权利要求1-8任一所述的一种聚氯乙烯无害化高附加值处理方法制得的无序炭和多孔炭材料,其特征在于,所述的无序炭材料的d002值大于0.36nm,多孔炭材料比表面积大于500m2/g。
10.权利要求1-8任一所述的一种聚氯乙烯无害化高附加值处理方法制得的无序炭和多孔炭材料的应用,其特征在于,无序炭材料应用于钠离子电池、锂离子电池以及钾离子电池电极材料;多孔炭材料应用于吸附材料、超级电容器电极材料和催化剂载体。
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KR102037463B1 (ko) * | 2018-10-29 | 2019-11-26 | 한국화학연구원 | 폐플라스틱과 석유계 잔사유를 활용한 고수율 활성탄 제조 방법 및 이에 의해 제조된 고효율 흡착 활성탄 |
CN110903836A (zh) * | 2019-11-29 | 2020-03-24 | 同济大学 | 一种有机废物的资源化处理方法 |
CN113003574A (zh) * | 2021-04-07 | 2021-06-22 | 大连理工大学 | 一种高比表面积多孔材料的制备方法及其应用 |
CN114572982A (zh) * | 2022-04-02 | 2022-06-03 | 中国科学院山西煤炭化学研究所 | 一种利用固废物制备的活性炭、微孔活性炭及其制备方法 |
CN115863566A (zh) * | 2022-11-23 | 2023-03-28 | 广东工业大学 | 一种硬炭/软炭/石墨三元复合碳材料及其制备方法与应用 |
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