CN111889075A - 一种利用造纸污泥制备的活性炭吸附剂及其制备方法和应用 - Google Patents

一种利用造纸污泥制备的活性炭吸附剂及其制备方法和应用 Download PDF

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CN111889075A
CN111889075A CN202010775071.4A CN202010775071A CN111889075A CN 111889075 A CN111889075 A CN 111889075A CN 202010775071 A CN202010775071 A CN 202010775071A CN 111889075 A CN111889075 A CN 111889075A
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包红旭
徐晓红
宋泽斌
巨承文
李泽
刘洪源
胡家伟
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Liaoning University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/024Compounds of Zn, Cd, Hg
    • B01J20/0244Compounds of Zn
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0288Halides of compounds other than those provided for in B01J20/046
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041Oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents

Abstract

本发明公开一种利用造纸污泥制备活性炭吸附剂的方法,以造纸污泥为原料,以ZnCl2、KOH为活化剂制备活性炭吸附剂,通过对污泥的脱水、干燥、研磨,再用活化剂振荡浸渍、干燥、高温热解炭化、漂洗、干燥,得到活性炭吸附剂成品。活性炭吸附剂在对品红吸附脱色时,最佳投加量为150mg,最佳反应时间为40min。

Description

一种利用造纸污泥制备的活性炭吸附剂及其制备方法和应用
技术领域
本发明涉及固体废弃物资源化利用处置技术领域,具体涉及一种利用造纸污泥制备活性炭吸附剂的方法及应用。
背景技术
污泥是城市污水处理过程中产生的副产物。目前,污泥改性制备活性炭已有了一些基础性的研究。活性炭具有很强的吸附性能力主要是因为其比表面积高和内部发达的空隙结构。由于社会的快速发展,能源的需求量越来越高,继而间接导致活性炭制作成本升高,故在充分利用农作物秸秆、纸浆废液、有机废弃物等含碳物质制造价格低廉的活性炭方面的研究受到重视。近年来,国内外出现了许多用活性污泥作为活性炭原料的报道和研究。目前,国内外污泥碳质吸附剂的制备方法主要分为四种:碳化法、物理活化法、化学活化法、物理化学活化法。碳化法制备工艺虽然简便快捷,但是制成的碳化产品因没有经过活化这一步,孔隙不均匀,吸附效果不理想,品质较差;物理活化法要求的温度高,能耗大,原料中碳量损耗大,制备的活性炭吸附性能较差;物理化学活化法虽然制备的活性炭吸附性能好,但其对生产设备要求严格,不易操作。相比而言化学活化法制备效果就显得比较好了,虽说活化剂本身或在活化过程中会产生有腐蚀性的物质,具有腐蚀设备和污染环境的缺陷,但其最大的优点是活化剂与活化工艺条件较易控制,且制备工艺较为成熟。
发明内容
本发明的目的之一是针对能源的需求量越来越高,继而间接导致活性炭制作成本升高,利用造纸污泥和化学活化发的优点,提出一种利用造纸污泥制备活性炭吸附剂的方法。
本发明的目的之二是提供一种利用造纸污泥制备活性炭吸附剂在染料品红吸附中的方法。
为实现本发明目的所采用的技术方案为:一种利用造纸污泥制备的活性炭吸附剂,以造纸污泥为原料,以ZnCl2、KOH为活化剂,将造纸污泥与活化剂混合,震荡反应后,烘干,用HCl溶液洗涤后,烘干得到活性炭吸附剂。
一种利用造纸污泥制备活性炭吸附剂的制备方法,包括如下步骤:
1)将造纸污泥置于高速沉降离心脱水机中脱水,取离心后的污泥烘干,再经过研钵研磨成粉末、过筛,得到预处理后的造纸污泥;
2)向将步骤1)中得到的造纸污泥粉末中加入ZnCl2、KOH活化剂,在振荡器中进行震荡浸渍活化处置18h,离心分离,去除上层清液,将下层污泥置于烘箱中100℃干燥1h,再置于马弗炉中,隔绝空气,升温至热解温度,进行炭化,得到活性炭吸附剂粗产品;
3)将步骤2)中得到的粗产品用洗涤液反复冲洗,以除去残留的活化剂和其他杂质,干燥得到活性炭吸附剂。
上述的制备方法,步骤1)中,造纸污泥在高速沉降离心脱水机中以3000r/min脱水20min,造纸污泥烘干是在烘箱中以90-100℃干燥1-3h。
上述的制备方法,步骤2)中,按摩尔比,ZnCl2:KOH=1:1-5。
上述的制备方法,步骤2)中,预处理后的造纸污泥粉末与活性剂的质量比为1:0.5-4。
上述的制备方法,步骤2)中,所述热解温度为600-650℃,升温速率为15-25℃/min,碳化时间为1-2h。
上述的制备方法,步骤3)中,所述洗涤液分别为3mol/L的HCl溶液和70-80℃蒸馏水。
上述的制备方法,步骤3)中,所述的干燥为100-110℃干燥5-10h。
上述的一种利用造纸污泥制备的活性炭吸附剂在吸附染料中的应用。
上述的应用,所述的染料是品红。
本发明的有益效果为:
(1)本发明以造纸污泥为原料制备活性炭,为污泥的处理处置和资源化利用提供一条新的出路。
(2)本发明为活性炭生产找到了廉价可得、来源广泛的原料,可以在一定程度上缓解能源短缺的矛盾。
(3)本发明活化剂与活化工艺条件较易控制,活化炭制备成本低。
(4)本发明采用化学活化法制备活性炭效果比较好,虽说活化剂本身或在活化过程中会产生有腐蚀性的物质,具有腐蚀设备和污染环境的缺陷,但其最大的优点是活化剂与活化工艺条件较易控制,且制备工艺较为成熟。
附图说明
图1是活性炭吸附剂投加量对品红脱色率的影响。
图2是反应时间对品红脱色率的影响。
具体实施方式
实施例1一种利用造纸污泥制备的活性炭吸附剂
1、将造纸污泥置于高速沉降离心脱水机中3000r/min脱水20min,取离心后的污泥置于烘箱中100℃干燥2h,再经过研钵研磨成粉末、过筛,得到粉末粒径为1-2mm预处理后的造纸污泥。
2、向100g预处理后的造纸污泥粉末加入100ml 3mol/L ZnCl2和150ml 3mol/LKOH,在振荡器中进行震荡浸渍活化处置18h,离心分离,去除上层清液,将下层污泥置于烘箱中100℃干燥1h,再置于马弗炉中,隔绝空气,以20℃/min的速度进行程序性升至620℃,热解炭化1.5h,得到活性炭吸附剂粗产品。
3、将活性炭吸附剂粗产品3mol/L HCl溶液和75℃蒸馏水交替反复冲洗,以除去残留的活化剂和其他杂质,然后105℃干燥8h,得到活性炭吸附剂。
实施例2活性炭吸附剂在染料品红吸附实验中的应用
1、活性炭吸附剂投加量对品红脱色率的影响
方法:取10支石英管,分别加入50mL初始浓度为50g/L、0.5%中性品红溶液,各加入25mg,50mg,75mg,100mg,125mg,150mg,175mg,200mg,225mg和250mg的实施例1制备的活性炭吸附剂,在微波辐射功率在550W的条件下,辐射40min,使品红溶液达到吸附/解吸平衡,考察品红溶液在活性炭吸附剂投加量改变的情况下的品红脱色率。
结果如图1所示,随着活性炭吸附剂投加量的增加,脱色率逐渐增加。当活性炭吸附剂的投加量为150mg时,对品红的脱色率为86.7%,此后脱色率趋于平缓。因此本发明优选,每mL初始浓度为50g/L的0.5%中性品红溶液中加入3mg活性炭吸附剂。
2、反应时间对品红脱色率的影响
方法:取6支石英管,分别加入50mL初始浓度为50g/L、0.5%中性品红溶液,各加入150mg的实施例1制备的活性炭吸附剂,在微波辐射功率在550W的条件下,分别辐射10min,20min,30min,40min,50min和60min使品红溶液得到到吸附/解吸平衡,考察品红溶液在活性炭吸附剂投加量改变的情况下的品红脱色率。
结果如图2所示,随着反应时间的增加,脱色率逐渐增加。当微波辐射时间为40min时,对品红的脱色率为87.5%,此后脱色率趋于平缓。因此本发明优选,0.5%中性品红溶液脱色时间为40min。

Claims (10)

1.一种利用造纸污泥制备的活性炭吸附剂,其特征在于,以造纸污泥为原料,以ZnCl2、KOH为活化剂,将造纸污泥与活化剂混合,震荡反应后,烘干,用HCl溶液洗涤后,烘干得到活性炭吸附剂。
2.一种利用造纸污泥制备活性炭吸附剂的制备方法,其特征在于,包括如下步骤:
1)将造纸污泥置于高速沉降离心脱水机中脱水,取离心后的污泥烘干,再经过研钵研磨成粉末、过筛,得到预处理后的造纸污泥;
2)向将步骤1)中得到的造纸污泥粉末中加入ZnCl2、KOH活化剂,在振荡器中进行震荡浸渍活化处置18h,离心分离,去除上层清液,将下层污泥置于烘箱中100℃干燥1h,再置于马弗炉中,隔绝空气,升温至热解温度,进行碳化,得到活性炭吸附剂粗产品;
3)将步骤2)中得到的粗产品用洗涤液反复冲洗,以除去残留的活化剂和其他杂质,干燥得到活性炭吸附剂。
3.根据权利要求2所述的制备方法,其特征在于:步骤1)中,造纸污泥在高速沉降离心脱水机中以3000r/min脱水20min,造纸污泥烘干是在烘箱中以90-100℃干燥1-3h。
4.根据权利要求3所述的制备方法,其特征在于:步骤2)中,按摩尔比,ZnCl2:KOH=1:1-5。
5.根据权利要求4所述的制备方法,其特征在于:步骤2)中,预处理后的造纸污泥粉末与活性剂的质量比为1:0.5-4。
6.根据权利要求5所述的制备方法,其特征在于:步骤2)中,所述热解温度为600-650℃,升温速率为15-25℃/min,碳化时间为1-2h。
7.根据权利要求6所述的制备方法,其特征在于:步骤3)中,所述洗涤液分别为3mol/L的HCl溶液和70-80℃蒸馏水。
8.根据权利要求7所述的制备方法,其特征在于:步骤3)中,所述的干燥为100-110℃干燥5-10h。
9.权利要求1所述的一种利用造纸污泥制备的活性炭吸附剂在吸附染料中的应用。
10.根据权利要求9所述的应用,其特征在于,所述的染料是品红。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624559A (zh) * 2020-11-10 2021-04-09 上海交通大学 一种改性污泥基多孔生物炭的制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624559A (zh) * 2020-11-10 2021-04-09 上海交通大学 一种改性污泥基多孔生物炭的制备方法

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