CN116673062A - 一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用 - Google Patents

一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用 Download PDF

Info

Publication number
CN116673062A
CN116673062A CN202310873908.2A CN202310873908A CN116673062A CN 116673062 A CN116673062 A CN 116673062A CN 202310873908 A CN202310873908 A CN 202310873908A CN 116673062 A CN116673062 A CN 116673062A
Authority
CN
China
Prior art keywords
nitrogen
doped
porous carbon
tio
flower
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202310873908.2A
Other languages
English (en)
Inventor
帅桂荣
刘甜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi Yichen Xinrui Environmental Technology Co ltd
Original Assignee
Jiangxi Yichen Xinrui Environmental Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangxi Yichen Xinrui Environmental Technology Co ltd filed Critical Jiangxi Yichen Xinrui Environmental Technology Co ltd
Priority to CN202310873908.2A priority Critical patent/CN116673062A/zh
Publication of CN116673062A publication Critical patent/CN116673062A/zh
Withdrawn legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • 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
    • B01J20/0207Compounds of Sc, Y or Lanthanides
    • 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
    • B01J20/0259Compounds of N, P, As, Sb, Bi
    • 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
    • B01J20/0274Solid 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
    • B01J20/0296Nitrates of compounds other than those provided for in B01J20/04
    • 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
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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 form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/082Decomposition and pyrolysis
    • B01J37/084Decomposition of carbon-containing compounds into carbon
    • 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
    • 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
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • 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
    • B01J2220/42Materials 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
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Catalysts (AREA)

Abstract

本发明涉及水污染处理技术领域,且公开了一种氮掺杂多孔碳负载花状Dy掺杂TiO2,氮掺杂在碳层基体中形成丰富的含氮官能团,这些活性含氮官能团的氮原子上含有孤对电子,对Cu2+等重金属具有很强的螯合作用,起到对重金属离子的吸附效果,同时氮原子的电负性比碳大,具有高电负性,可以调节碳层表面的电荷排布,增强碳层的表面亲和性,促进对亚甲基蓝的吸附作用,花状的纳米TiO2具有更高的比表面积,Dy掺杂有利于促进TiO2的光吸收边发生红移,在可见光下也具有良好的光吸收范围和光化学响应性,具有优异的光催化降解活性,当氮掺杂多孔碳将亚甲基蓝吸附后,负载的Dy掺杂TiO2可以将亚甲基蓝充分降解为无毒的小分子。

Description

一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的 应用
技术领域
本发明涉及水污染处理技术领域,具体为一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用。
背景技术
水污染主要是未经处理的生活污水、工业废水等随意排放进自然环境中,污染物主要有无机污染物和有机污染物,如Cu2+、Cd2+等重金属离子;亚甲基蓝、甲基橙等有机染料;四环素等抗生素等,目前对于污水处理和水污染治理的方法主要有物理絮凝法、化学吸附法、生物降解法、光催化降解法等。
吸附法是一种简单高效、成本低廉的水污染治理方法,吸附材料主要有活性炭、氧化铝、聚丙烯酰胺等,其中活性多孔碳材料具有孔隙丰富、比表面积高、结构稳定,重金属离子吸附和有机污染物吸附方面具有广泛的应用,纳米TiO2是一种常见的光催化剂,无毒无污染、制备方法简单、形貌可调控、光化学性能优异,在有机污染物降解方面具有重要的应用,因此可以采取提高纳米TiO2的光催化活性,增强活性多孔碳材料的吸附性能,同时将两者进行原位复合,得到具有吸附和光催化降解的双功能材料,应用于重金属离子和有机污染物的污水处理中。
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用,解决了传统的纳米TiO2的光催化降解活性不高,同时解决了多孔碳材料的活性吸附位点不足,吸附性能有效的问题。
(二)技术方案
为实现上述目的,本发明提供如下技术方案:一种氮掺杂多孔碳负载花状Dy掺杂TiO2,所述氮掺杂多孔碳负载花状Dy掺杂TiO2的制法如下所示:
(1)向烧瓶中加入蒸馏水和纤维素,超声分散均匀后,加入高碘酸钠,并滴加浓硫酸,控制H2SO4的物质的量浓度为0.1-0.15mol/L,进行氧化反应,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入低氧化度醛基纤维素,超声分散后加入2,5-二氨基嘧啶,进行席夫碱交联缩合反应,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入嘧啶席夫碱交联纤维素和氢氧化钾,搅拌4-10h,将溶液真空干燥、固体化合物放入气氛炉中高温炭化,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、氮掺杂多孔碳和钛酸四丁酯、超声分散后后加入硝酸镝,搅拌6-12h,将溶液倒入反应釜中水热反应,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在300-350℃下煅烧2-3h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
优选的,所述步骤(1)中纤维素和高碘酸钠的质量比为100:15-30。
优选的,所述步骤(1)中氧化反应在10-25℃下反应1-3h。
优选的,所述步骤(2)中低氧化度醛基纤维素和2,5-二氨基嘧啶的质量比为100:5-25。
优选的,所述步骤(2)中席夫碱交联缩合反应在20-40℃下,反应6-24h。
优选的,所述步骤(3)中嘧啶席夫碱交联纤维素和氢氧化钾的质量比为10:20-35。
优选的,所述步骤(3)中高温炭化在700-850℃下,炭化2-4h。
优选的,所述步骤(4)中氮掺杂多孔碳、钛酸四丁酯和硝酸镝的质量比为180-300:100:5-9。
优选的,所述步骤(4)中水热反应在140-170℃下,反应8-12h。
优选的,所述氮掺杂多孔碳负载花状Dy掺杂TiO2应用于吸附材料和水污染处理领域。
(三)有益的技术效果
与现有技术相比,本发明具备以下有益技术效果:
该一种氮掺杂多孔碳负载花状Dy掺杂TiO2,通过调控氧化剂高碘酸钠的用量和反应条件,控制纤维的氧化度,得到醛基含量较少的低氧化度的纤维素,低氧化度的纤维素的开环度较少,碳骨架更加完整,成炭率高,容易被碳化。
该一种氮掺杂多孔碳负载花状Dy掺杂TiO2,纤维素分子链上的醛基与2,5-二氨基嘧啶的两个氨基发生席夫碱交联反应,得到嘧啶席夫碱交联纤维素,形成三维化学交联网络,三维空间结构使纤维素的比表面积更大,并且空间网络结构有利于碳化形成多孔碳结构,以纤维素三维碳骨架作为碳源,接枝的2,5-二氨基嘧啶作为氮源,通过碳化和氢氧化钾制孔作用,得到得到纤维素基氮掺杂多孔碳,并通过控制氧化度和醛基含量,来调节与和2,5-二氨基嘧啶的接枝率,从而控制多孔碳的含氮量,氮掺杂在碳层基体中形成丰富的含氮官能团,这些活性含氮官能团的氮原子上含有孤对电子,对Cu2+等重金属具有很强的螯合作用,起到对重金属离子的吸附效果,同时氮原子的电负性比碳大,具有高电负性,可以调节碳层表面的电荷排布,从而增强碳层的表面亲和性,促进对亚甲基蓝的吸附作用。
该一种氮掺杂多孔碳负载花状Dy掺杂TiO2,在醋酸的热溶剂体系中,以氮掺杂多孔碳作为生长载体,硝酸镝作为Dy源,通过热溶剂法,在氮掺杂多孔碳基体中原位生成花状Dy掺杂TiO2,原位生长法有利于花状Dy掺杂TiO2的分散性,改善团聚现象,同时花状的纳米TiO2具有更高的比表面积,同时Dy掺杂取代了部分Ti的晶格,产生的杂质能级有利于促进TiO2的光吸收边发生红移,使Dy掺杂TiO2在可见光下也具有良好的光吸收范围和光化学响应性,克服了传统的纳米TiO2只能在紫外光下进行吸收和光催化活性,使Dy掺杂TiO2具有优异的光催化降解活性,当氮掺杂多孔碳将亚甲基蓝吸附后,碳基体负载的Dy掺杂TiO2可以将亚甲基蓝充分降解为无毒的小分子,实现高效的光催化降解过程。
具体实施方式
为实现上述目的,本发明提供如下具体实施方式和实施例:一种氮掺杂多孔碳负载花状Dy掺杂TiO2制法如下所示:
(1)向烧瓶中加入蒸馏水、纤质量比为100:15-30纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.1-0.15mol/L,在10-25℃下进行氧化反应1-3h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:5-25低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在20-40℃下,进行席夫碱交联缩合反应6-24h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:20-35的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌4-10h,将溶液真空干燥、固体化合物放入气氛炉中,在700-850℃下,高温炭化2-4h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为180-300:100:5-9的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌6-12h,将溶液倒入反应釜中,在140-170℃下,水热反应8-12h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在300-350℃下煅烧2-3h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2,应用于吸附材料和水污染处理领域。
实施例1
(1)向烧瓶中加入蒸馏水、纤质量比为100:15纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.1mol/L,在10℃下进行氧化反应1h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:5低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在20℃下,进行席夫碱交联缩合反应6h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:20的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌4h,将溶液真空干燥、固体化合物放入气氛炉中,在700℃下,高温炭化2h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为180:100:5的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌6h,将溶液倒入反应釜中,在140℃下,水热反应8h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在300℃下煅烧2h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
实施例2
(1)向烧瓶中加入蒸馏水、纤质量比为100:20纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.15mol/L,在10℃下进行氧化反应2h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:12低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在40℃下,进行席夫碱交联缩合反应12h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:25的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌8h,将溶液真空干燥、固体化合物放入气氛炉中,在800℃下,高温炭化3h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为240:100:6.5的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌10h,将溶液倒入反应釜中,在170℃下,水热反应102h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在320℃下煅烧2h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
实施例3
(1)向烧瓶中加入蒸馏水、纤质量比为100:22纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.12mol/L,在20℃下进行氧化反应2h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:18低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在30℃下,进行席夫碱交联缩合反应12h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:30的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌8h,将溶液真空干燥、固体化合物放入气氛炉中,在800℃下,高温炭化3h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为260:100:7.5的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌8h,将溶液倒入反应釜中,在160℃下,水热反应10h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在320℃下煅烧2.5h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
实施例4
(1)向烧瓶中加入蒸馏水、纤质量比为100:30纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.15mol/L,在25℃下进行氧化反应3h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:25低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在40℃下,进行席夫碱交联缩合反应24h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:35的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌10h,将溶液真空干燥、固体化合物放入气氛炉中,在850℃下,高温炭化4h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为300:100:9的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌12h,将溶液倒入反应釜中,在170℃下,水热反应12h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在350℃下煅烧3h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
对比例1
(1)向烧瓶中加入蒸馏水、纤质量比为100:8纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.15mol/L,在25℃下进行氧化反应2h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:2低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在30℃下,进行席夫碱交联缩合反应18h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:15的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌8h,将溶液真空干燥、固体化合物放入气氛炉中,在850℃下,高温炭化3h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为140:100:2的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌12h,将溶液倒入反应釜中,在140℃下,水热反应8h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在350℃下煅烧2h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
对比例1
(1)向烧瓶中加入蒸馏水、纤质量比为100:38纤维素和高碘酸钠,超声分散后并滴加浓硫酸,控制H2SO4的物质的量浓度为0.15mol/L,在20℃下进行氧化反应1h,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素。
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入质量比为的100:32低氧化度醛基纤维素和2,5-二氨基嘧啶,超声分散后,在30℃下,进行席夫碱交联缩合反应24h,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素。
(3)向蒸馏水中加入质量比为10:40的嘧啶席夫碱交联纤维素和氢氧化钾,搅拌4h,将溶液真空干燥、固体化合物放入气氛炉中,在850℃下,高温炭化4h,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳。
(4)向烧瓶中加入醋酸溶剂、质量比为350:100:11的氮掺杂多孔碳、钛酸四丁酯和硝酸镝,超声分散后搅拌6h,将溶液倒入反应釜中,在170℃下,水热反应8h,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在320℃下煅烧3h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
向1000mL的10mg/L的硝酸铜溶液中,加入100mg的氮掺杂多孔碳负载花状Dy掺杂TiO2作为吸附材料,搅拌均匀后进行4h的吸附过程,使用UV752型紫外可见分光光度计测试吸附后Cu2+的浓度,测试吸附性能。
配置500mL的10mg/L的亚甲基蓝溶液,加入200mg的氮掺杂多孔碳负载花状Dy掺杂TiO2作为吸附材料,置于避光处,搅拌均匀后进行6h的吸附过程,使用UV752型紫外可见分光光度计测试吸附后亚甲基蓝的浓度,测试吸附性能。
配置500mL的10mg/L的亚甲基蓝溶液,加入200mg的氮掺杂多孔碳负载花状Dy掺杂TiO2作为吸附材料,在200W氙灯下,搅拌均匀后照射6h的吸附-光催化降解过程,使用UV752型紫外可见分光光度计测试吸附-降解后的亚甲基蓝的浓度,测试吸附-光催化降解性能。

Claims (10)

1.一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述氮掺杂多孔碳负载花状Dy掺杂TiO2的制法如下所示:
(1)向烧瓶中加入蒸馏水和纤维素,超声分散均匀后,加入高碘酸钠,并滴加浓硫酸,控制H2SO4的物质的量浓度为0.1-0.15mol/L,进行氧化反应,过滤溶剂,蒸馏水洗涤产物至中性,干燥后得到低氧化度醛基纤维素;
(2)向烧瓶中加入蒸馏水和丙酮混合溶剂,加入低氧化度醛基纤维素,超声分散后加入2,5-二氨基嘧啶,进行席夫碱交联缩合反应,过滤溶剂,蒸馏水和乙醇洗涤,得到嘧啶席夫碱交联纤维素;
(3)向蒸馏水中加入嘧啶席夫碱交联纤维素和氢氧化钾,搅拌4-10h,将溶液真空干燥、固体化合物放入气氛炉中高温炭化,蒸馏水洗涤炭化产物至中性,得到纤维素基氮掺杂多孔碳;
(4)向烧瓶中加入醋酸溶剂、氮掺杂多孔碳和钛酸四丁酯、超声分散后后加入硝酸镝,搅拌6-12h,将溶液倒入反应釜中水热反应,过滤溶剂、蒸馏水和乙醇洗涤,混合产物置于马弗炉中,在300-350℃下煅烧2-3h,得到氮掺杂多孔碳负载花状Dy掺杂TiO2
2.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(1)中纤维素和高碘酸钠的质量比为100:15-30。
3.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(1)中氧化反应在10-25℃下反应1-3h。
4.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(2)中低氧化度醛基纤维素和2,5-二氨基嘧啶的质量比为100:5-25。
5.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(2)中席夫碱交联缩合反应在20-40℃下,反应6-24h。
6.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(3)中嘧啶席夫碱交联纤维素和氢氧化钾的质量比为10:20-35。
7.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(3)中高温炭化在700-850℃下,炭化2-4h。
8.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(4)中氮掺杂多孔碳、钛酸四丁酯和硝酸镝的质量比为180-300:100:5-9。
9.根据权利要求1所述的一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述步骤(4)中水热反应在140-170℃下,反应8-12h。
10.一种氮掺杂多孔碳负载花状Dy掺杂TiO2,其特征在于:所述氮掺杂多孔碳负载花状Dy掺杂TiO2应用于吸附材料和水污染处理领域。
CN202310873908.2A 2023-07-17 2023-07-17 一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用 Withdrawn CN116673062A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310873908.2A CN116673062A (zh) 2023-07-17 2023-07-17 一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310873908.2A CN116673062A (zh) 2023-07-17 2023-07-17 一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用

Publications (1)

Publication Number Publication Date
CN116673062A true CN116673062A (zh) 2023-09-01

Family

ID=87789308

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310873908.2A Withdrawn CN116673062A (zh) 2023-07-17 2023-07-17 一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用

Country Status (1)

Country Link
CN (1) CN116673062A (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117567426A (zh) * 2024-01-19 2024-02-20 寿光金远东变性淀粉有限公司 一种丙交酯生产方法及装置

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117567426A (zh) * 2024-01-19 2024-02-20 寿光金远东变性淀粉有限公司 一种丙交酯生产方法及装置
CN117567426B (zh) * 2024-01-19 2024-04-23 寿光金远东变性淀粉有限公司 一种丙交酯生产方法及装置

Similar Documents

Publication Publication Date Title
CN111346609B (zh) 一种用于含重金属染料废水的吸附材料及其制备方法
CN116673062A (zh) 一种氮掺杂多孔碳负载花状Dy掺杂TiO2及在水污染处理中的应用
CN111450871A (zh) 一种Mn掺杂g-C3N4负载多孔ZnCo2O4的光催化材料及其制法
CN110756223A (zh) 一种吸附催化复合材料及其在污染物处理中的应用
CN108339544B (zh) 富勒烯羧基衍生物修饰的光催化剂/超疏水膜复合材料
CN109999909A (zh) 壳聚糖/硅藻土/氧化石墨烯复合材料及其制备方法和应用
CN112619684A (zh) 一种功能化凹凸棒石负载NiO-g-C3N4的光催化-吸附剂和制法
CN111454400A (zh) 一种纳米TiO2修饰壳聚糖-丙烯酸水凝胶吸附材料及其制法
CN112844351A (zh) 一种花状Fe掺杂TiO2负载多孔碳的复合材料的制法及应用
CN113880088A (zh) 一种造纸污泥基生物炭的制备方法
CN116532084A (zh) 一种Nd掺杂Bi2WO6纳米花-生物质多孔碳材料的制备和应用
CN107983323B (zh) 一种纳米铜修饰的聚苯胺基纳米复合吸附剂及其制备方法与应用
CN115779889B (zh) 一种木质素炭/钼酸铋复合光催化剂及其制备方法和应用
CN113171758B (zh) 二氧化碳吸附剂及其制备方法、使用方法
CN112452310B (zh) 一种氮掺杂碳吸附剂及其制备方法和对有机染料的吸附应用
CN114160129A (zh) 二氧化钛/多孔碳负载型复合光催化剂的制备方法
CN111530489A (zh) 一种g-C3N4-Bi2O3异质结光催化降解吸附复合材料及其制法
CN111921494A (zh) 一种文冠果活性炭吸附剂及其制备方法和应用
CN111298759A (zh) 一种pn型半导体-磁性多孔碳光催化复合吸附材料及其制法
CN116116374B (zh) 一种La2O3/BNNFs复合吸附剂的制备方法及其应用
CN113663664B (zh) RuTe2/B-TiO2材料的制备方法及其光催化降解抗生素的应用
CN116673003B (zh) 一种污水处理用吸附剂及其制备方法和应用
CN112058245B (zh) 一种用于污水处理的有机高分子吸附剂及其制备方法
CN118002103A (zh) 一种氮掺杂改性生物炭及其制备方法和应用
CN115155636A (zh) 一种钠硼共掺杂的氮化碳光催化剂、还原氧化石墨烯复合膜及制备方法和应用

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20230901