CN106881071A - 一种改性活性炭/硅藻土吸附剂的制备方法 - Google Patents

一种改性活性炭/硅藻土吸附剂的制备方法 Download PDF

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CN106881071A
CN106881071A CN201510946085.7A CN201510946085A CN106881071A CN 106881071 A CN106881071 A CN 106881071A CN 201510946085 A CN201510946085 A CN 201510946085A CN 106881071 A CN106881071 A CN 106881071A
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diatomite
activated carbon
modified activated
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王福明
曾凡东
林宇
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YINGKOU BOHAI TECHNOLOGY Co Ltd
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    • 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
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
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    • 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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • 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
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42Materials comprising a mixture of inorganic materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
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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
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

Abstract

本发明公开了一种改性活性炭/硅藻土吸附剂的制备方法,包括以下步骤:a)硅藻土矿经酸性水洗提纯后,在N2保护气氛下500~800℃高温煅烧,将有机质碳化,形成无定形活性炭/硅藻土的复合材料。b)配制一定浓度的聚丙烯酰胺(PAM)溶液,与碳化硅藻土混合均匀后,60℃振荡分散均匀过夜。经水洗、抽滤、干燥,得到改性活性炭/硅藻土吸附剂。本发明制备的改性活性炭/硅藻土吸附剂较之常规硅藻土材料吸附性能大大增强,产品性能优异,且工艺过程简单可行,具有极好的工业前景和经济价值。

Description

一种改性活性炭/硅藻土吸附剂的制备方法
技术领域
本发明属于复合材料领域,特别涉及一种改性活性炭/硅藻土吸附剂的制备方法。
背景技术
自然界存在的硅藻土矿主要成分是无定形二氧化硅,为蛋白石及其变种,是由古代单细胞低等水生植物硅藻的硅质遗骸经过沉积作用,在一定的地质条件下形成的天然多孔性生物质矿物材料。硅藻土因具有独特的有序排列的微孔结构、孔隙率高、孔体积大、连通性好、质量轻、密度小、比表面积大、吸附性强、活性好等优点,被广泛用作吸附材料应用于助滤剂、催化剂载体、重金属废水吸附剂等,在国民经济发展中起着重要的作用。
随着经济社会的发展,矿产冶炼、机械制造、化工生产、电子产品以及仪表等的生产过程中产生大量重金属废水,造成了严重的生态环境危害。硅藻土含有活性硅羟基,在水溶液中硅羟基上的H+会解离处理,使得硅藻土的表面带一定的负电荷,因此对于带正电荷的重金属废水中的重金属离子具有较好的吸附效果,但在pH值较低的重金属废水中,水样中H+会抑制硅羟基上H+的解离,导致硅藻土的吸附重金属离子效果降低。另外,所采用的硅藻土颗粒较小,且带负电,在水中的沉降性能较差,对构筑物的容积要求比较大。因此,直接用硅藻土原土处理重金属废水,会降低处理效率.
发明内容
为了克服现有硅藻原土在处理重金属废水过程中存在的效率降低的问题,同时合理有效的实现资源配置和利用,本发明提供一种过程易于控制、产品吸附效率高,经济效益大的一种改性活性炭/硅藻土吸附剂的制备方法。
本发明的目的是通过以下措施来达到:提供一种改性活性炭/硅藻土吸附剂的制备方法,包括以下步骤:a)一定目数的硅藻土矿经酸性水洗提纯后,在N2保护气氛下高温煅烧,将有机质碳化,形成无定形活性炭/硅藻土的复合材料。b)配制一定浓度的改性剂溶液,与碳化硅藻土混合均匀后,一定温度下振荡分散均匀,过夜,经水洗、抽滤、干燥,得到改性活性炭/硅藻土吸附剂。
进一步地,所述硅藻土有机质碳化过程,煅烧温度为500~800℃,碳化时间为2~6h,优选方案为煅烧温度600℃,碳化时间为4h。
进一步地,所用改性剂为聚丙烯酰胺(PAM),其溶液浓度为0.1%~0.3%,优选方案为聚丙烯酰胺的溶液浓度为0.3%。
进一步地,所述改性过程中改性过程中,反应温度为60~80℃,改性时间为24~48h,优选方案为反应温度为60℃,反应时间为24h
有益效果:本发明充分利用了硅藻土自身组成中的有机物质,通过碳化处理,使其变为无定形活性炭,极大地提升了硅藻土的比表面积,形成了无定形活性炭/硅藻土高效吸附剂,不仅合理的利用了天然资源,同时极大地提升了产品性能,而通过使用聚丙烯酰胺对无定形活性炭/硅藻土高效吸附剂进行改性处理,更进一步提高了产品的各项性能,使其经济价值得到了有效的提升,而且该工艺过程实现中工艺简单可行,原料低廉易得,具有极强的工业价值和经济价值。
具体实施方式
下面结合实施例对本发明进行详细说明。
本发明主要包括以下步骤:a)一定目数的硅藻土矿经酸性水洗提纯后,在N2保护气氛下高温煅烧,将有机质碳化,形成无定形活性炭/硅藻土的复合材料。b)配制一定浓度的改性剂溶液,与碳化硅藻土混合均匀后,一定温度下振荡分散均匀,过夜。经水洗、抽滤、干燥,得到改性活性炭/硅藻土吸附剂。
实施例
1、高有机质硅藻土的提纯与碳化
采集高有机质硅藻土矿块状样品经破碎研磨,200目筛筛分。将矿粉混合配成矿浆机械搅拌后,利用盐酸将pH值调节为1以除去无机碳酸盐,浸泡过夜后吸出上层矿浆。经抽滤得到滤饼,用蒸馏水洗涤3次后干燥、研磨过筛,得到提纯高有机质硅藻土。将提纯后的硅藻土粉置于管式炉中,在N2保护下,以10℃/min的升温速率升高到600℃,然后恒温4h,对其进行碳化处理,得到碳化硅藻土。
2、活性炭/硅藻土的改性处理
配制质量分数为0.3%聚丙烯酰胺(PAM)溶液,与碳化硅藻土混合均匀后,60℃振荡分散均匀过夜。经水洗、抽滤、干燥,得到活性炭/硅藻土高效吸附剂。
通过重金属静态饱和吸附实验、亚甲基蓝饱和吸附量测定及样品比表面积测定,得到的活性炭/硅藻土高效吸附剂比表面积是常规商品化硅藻土的3倍,亚甲基蓝饱和吸附量为41187mg/g,对Pb2+、Co2+和Sr2+具有显著的吸附能力,饱和吸附量分别为54147、37134和2511mg/g,改性效果显著。
以上内容是结合优选技术方案对本发明所做的进一步详细说明,不能认定发明的具体实施仅限于这些说明。对本发明所属技术领域的普通技术人员来说,在不脱离本发明的构思的前提下,还可以做出简单的推演及替换,都应当视为本发明的保护范围。

Claims (4)

1.一种改性活性炭/硅藻土吸附剂的制备方法,其特征在于,包括以下步骤:a)一定目数的硅藻土矿经酸性水洗提纯后,在N2保护气氛下高温煅烧,将有机质碳化,形成无定形活性炭/硅藻土的复合材料。b)配制一定浓度的改性剂溶液,与碳化硅藻土混合均匀后,一定温度下振荡分散均匀,过夜,经水洗、抽滤、干燥,得到改性活性炭/硅藻土吸附剂。
2.根据权利要求1所述的一种改性活性炭/硅藻土吸附剂的制备方法,其特征在于,所述硅藻土有机质碳化过程,煅烧温度为500~800℃,碳化时间为2~6h。
3.根据权利要求1所述的一种改性活性炭/硅藻土吸附剂的制备方法,其特征在于,所用改性剂为聚丙烯酰胺(PAM),其溶液浓度为0.1%~0.2%。
4.根据权利要求1所述的一种改性活性炭/硅藻土吸附剂的制备方法,其特征在于,改性过程中,反应温度为60~80℃,改性时间为24~48h。
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107347975A (zh) * 2017-07-07 2017-11-17 广西驰胜农业科技有限公司 一种百合的加工保鲜方法
CN107892373A (zh) * 2017-11-16 2018-04-10 唐山国丰钢铁有限公司 一种物理‑化学复合絮凝剂及其制备方法
CN107970887A (zh) * 2017-11-22 2018-05-01 大连智讯科技有限公司 一种粉状硅藻土的制备方法
CN109553110A (zh) * 2018-10-29 2019-04-02 山东大学 一种原位碳化制备介孔硅碳复合材料的方法
CN109593751A (zh) * 2018-09-12 2019-04-09 浙江省农业科学院 一种菌藻改性活性炭微胶囊制备方法
CN110270309A (zh) * 2019-07-25 2019-09-24 西南石油大学 一种页岩气压裂返排液水处理吸附剂制备方法及应用
CN110465263A (zh) * 2019-07-25 2019-11-19 西南石油大学 一种碳纳米管嵌套硅藻土高效吸附材料及制备方法及应用
CN110479209A (zh) * 2019-09-03 2019-11-22 邓晖 一种天然矿物/活性炭复合材料及其制备方法
CN112604646A (zh) * 2020-12-03 2021-04-06 新沂市锡沂高新材料产业技术研究院有限公司 一种改性硅藻土吸附剂的制备方法
CN113731364A (zh) * 2021-09-17 2021-12-03 苏州中材非金属矿工业设计研究院有限公司 一种黑滑石吸附剂及其制备方法和应用

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107347975A (zh) * 2017-07-07 2017-11-17 广西驰胜农业科技有限公司 一种百合的加工保鲜方法
CN107892373A (zh) * 2017-11-16 2018-04-10 唐山国丰钢铁有限公司 一种物理‑化学复合絮凝剂及其制备方法
CN107970887A (zh) * 2017-11-22 2018-05-01 大连智讯科技有限公司 一种粉状硅藻土的制备方法
CN109593751A (zh) * 2018-09-12 2019-04-09 浙江省农业科学院 一种菌藻改性活性炭微胶囊制备方法
CN109553110A (zh) * 2018-10-29 2019-04-02 山东大学 一种原位碳化制备介孔硅碳复合材料的方法
CN110270309A (zh) * 2019-07-25 2019-09-24 西南石油大学 一种页岩气压裂返排液水处理吸附剂制备方法及应用
CN110465263A (zh) * 2019-07-25 2019-11-19 西南石油大学 一种碳纳米管嵌套硅藻土高效吸附材料及制备方法及应用
CN110465263B (zh) * 2019-07-25 2022-04-26 西南石油大学 一种碳纳米管嵌套硅藻土高效吸附材料及制备方法及应用
CN110479209A (zh) * 2019-09-03 2019-11-22 邓晖 一种天然矿物/活性炭复合材料及其制备方法
CN112604646A (zh) * 2020-12-03 2021-04-06 新沂市锡沂高新材料产业技术研究院有限公司 一种改性硅藻土吸附剂的制备方法
CN113731364A (zh) * 2021-09-17 2021-12-03 苏州中材非金属矿工业设计研究院有限公司 一种黑滑石吸附剂及其制备方法和应用

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