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 PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 65
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 34
- 238000003911 water pollution Methods 0.000 title claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 229920002678 cellulose Polymers 0.000 claims description 68
- 239000001913 cellulose Substances 0.000 claims description 68
- 239000012153 distilled water Substances 0.000 claims description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 63
- 239000002904 solvent Substances 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 36
- 239000002262 Schiff base Substances 0.000 claims description 33
- 238000007254 oxidation reaction Methods 0.000 claims description 32
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 27
- 238000005406 washing Methods 0.000 claims description 27
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 24
- -1 pyrimidine Schiff base Chemical class 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 230000007935 neutral effect Effects 0.000 claims description 18
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- 230000003647 oxidation Effects 0.000 claims description 14
- DNACGYGXUFTEHO-UHFFFAOYSA-N pyrimidine-2,5-diamine Chemical compound NC1=CN=C(N)N=C1 DNACGYGXUFTEHO-UHFFFAOYSA-N 0.000 claims description 14
- QXPQVUQBEBHHQP-UHFFFAOYSA-N 5,6,7,8-tetrahydro-[1]benzothiolo[2,3-d]pyrimidin-4-amine Chemical compound C1CCCC2=C1SC1=C2C(N)=NC=N1 QXPQVUQBEBHHQP-UHFFFAOYSA-N 0.000 claims description 12
- 150000004753 Schiff bases Chemical class 0.000 claims description 12
- 238000004132 cross linking Methods 0.000 claims description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000006482 condensation reaction Methods 0.000 claims description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 238000010000 carbonizing Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000012046 mixed solvent Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000003763 carbonization Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 18
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 11
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 230000009920 chelation Effects 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 150000003384 small molecules Chemical class 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- 239000003575 carbonaceous material Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 125000003172 aldehyde group Chemical group 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004098 Tetracycline Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 231100001240 inorganic pollutant Toxicity 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
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。
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