CN108554459A - 一种新型聚苯胺/二氧化钛复合材料及其在环境修复中的应用 - Google Patents
一种新型聚苯胺/二氧化钛复合材料及其在环境修复中的应用 Download PDFInfo
- Publication number
- CN108554459A CN108554459A CN201810340567.1A CN201810340567A CN108554459A CN 108554459 A CN108554459 A CN 108554459A CN 201810340567 A CN201810340567 A CN 201810340567A CN 108554459 A CN108554459 A CN 108554459A
- Authority
- CN
- China
- Prior art keywords
- polyaniline
- new
- titania material
- water
- composite titania
- 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.)
- Granted
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000005067 remediation Methods 0.000 title claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002608 ionic liquid Substances 0.000 claims abstract description 14
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000447 pesticide residue Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 26
- 238000001556 precipitation Methods 0.000 claims description 21
- 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 13
- 238000002156 mixing Methods 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 239000000575 pesticide Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- -1 1- ethyl-3-methylimidazole halogens Chemical class 0.000 claims description 4
- 239000003993 organochlorine pesticide Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- WWFKDEYBOOGHKL-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;bromide Chemical class Br.CCN1CN(C)C=C1 WWFKDEYBOOGHKL-UHFFFAOYSA-N 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- VQXSOUPNOZTNAI-UHFFFAOYSA-N Pyrethrin I Natural products CC(=CC1CC1C(=O)OC2CC(=O)C(=C2C)CC=C/C=C)C VQXSOUPNOZTNAI-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- XQUXKZZNEFRCAW-UHFFFAOYSA-N fenpropathrin Chemical compound CC1(C)C(C)(C)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 XQUXKZZNEFRCAW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 3
- HYJYGLGUBUDSLJ-UHFFFAOYSA-N pyrethrin Natural products CCC(=O)OC1CC(=C)C2CC3OC3(C)C2C2OC(=O)C(=C)C12 HYJYGLGUBUDSLJ-UHFFFAOYSA-N 0.000 claims description 3
- VJFUPGQZSXIULQ-XIGJTORUSA-N pyrethrin II Chemical compound CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VJFUPGQZSXIULQ-XIGJTORUSA-N 0.000 claims description 3
- OMFRMAHOUUJSGP-IRHGGOMRSA-N bifenthrin Chemical compound C1=CC=C(C=2C=CC=CC=2)C(C)=C1COC(=O)[C@@H]1[C@H](\C=C(/Cl)C(F)(F)F)C1(C)C OMFRMAHOUUJSGP-IRHGGOMRSA-N 0.000 claims description 2
- 231100000572 poisoning Toxicity 0.000 claims description 2
- 230000000607 poisoning effect Effects 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims 1
- 239000002689 soil Substances 0.000 abstract description 14
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 9
- 239000011651 chromium Substances 0.000 abstract description 8
- 239000011133 lead Substances 0.000 abstract description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052804 chromium Inorganic materials 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VEMKTZHHVJILDY-UXHICEINSA-N bioresmethrin Chemical class CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)OCC1=COC(CC=2C=CC=CC=2)=C1 VEMKTZHHVJILDY-UXHICEINSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 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
- 231100000719 pollutant Toxicity 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/306—Pesticides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Hydrology & Water Resources (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Soil Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明涉及一种新型聚苯胺/二氧化钛复合材料及其在环境修复中的应用,本发明通过使用离子液体、巯基乙酸修饰改性获得一种新型聚苯胺/二氧化钛复合材料,其能有效地清除环境中(水、土壤)中重金属铬和铅以及土壤中农药残留。
Description
技术领域
本发明属于材料领域,具体涉及一种新型聚苯胺/二氧化钛复合材料及其在环境修复中的应用。
背景技术
工业废水的排放、农业上农药的使用,导致水体、土壤中存在大量重金属及农药残留,重金属及多数农药具有不可降解性及蓄积性,严重威胁着人类的健康。因此,急需开发一种能有效清除环境中(水、土壤)重金属、农药残留的新型材料。聚苯胺/二氧化钛复合材料多用于光催化反应,也可用于降解有机染料污染物甲基橙、罗丹明B等。本发明通过使用离子液体、巯基乙酸修饰改性获得一种新型聚苯胺/二氧化钛复合材料,其能有效地清除环境中(水、土壤)中重金属铬和铅以及农药残留。
发明内容
本发明提供一种新型聚苯胺/二氧化钛复合材料,即离子液体修饰的聚苯胺/二氧化钛复合材料,所述新型聚苯胺/二氧化钛复合材料的制备方法包括如下步骤:
(1)将离子液体与无水乙醇混合均匀后,加入钛酸正丁酯搅拌0.5-1.0h后得混合液a;
(2)向混合液a中加入聚苯胺和巯基乙酸继续搅拌0.5-1.0h后,加水,升温至50-60℃继续搅拌1-2h后,过滤得沉淀,沉淀经后处理即得所述新型聚苯胺/二氧化钛复合材料。
步骤(1)中离子液体选自1-乙基-3-甲基咪唑卤盐,优选1-乙基-3-甲基咪唑氯盐、1-乙基-3-甲基咪唑溴盐;离子液体、无水乙醇、钛酸正丁酯的质量比为1:5-10:1;步骤(2)中聚苯胺的用量为钛酸正丁酯质量的0.1-0.2倍,巯基乙酸与聚苯胺的质量比为1:1,水的用量与钛酸正丁酯质量用量相同;所述水优选为去离子水或蒸馏水;所述后处理为依次用乙醇、水洗涤后,于60-80℃条件下真空干燥12-24h。
本发明的另一实施方案上述离子液体修饰的聚苯胺/二氧化钛复合材料的制备方法,其特征在于包括如下步骤:
(1)将离子液体与无水乙醇混合均匀后,加入钛酸正丁酯搅拌0.5-1.0h后得混合液a;
(2)向混合液a中加入聚苯胺和巯基乙酸继续搅拌0.5-1.0h后,加水,升温至50-60℃继续搅拌1-2h后,过滤得沉淀,沉淀经后处理即得所述新型聚苯胺/二氧化钛复合材料。
步骤(1)中离子液体选自1-乙基-3-甲基咪唑卤盐,优选1-乙基-3-甲基咪唑氯盐、1-乙基-3-甲基咪唑溴盐;离子液体、无水乙醇、钛酸正丁酯的质量比为1:5-10:1;步骤(2)中聚苯胺的用量为钛酸正丁酯质量的0.1-0.2倍,巯基乙酸与聚苯胺的质量比为1:1,水的用量与钛酸正丁酯质量用量相同;所述水优选为去离子水或蒸馏水;所述后处理为依次用乙醇、水洗涤后,于60-80℃条件下真空干燥12-24h。
本发明的另一实施方案提供上述新型聚苯胺/二氧化钛复合材料在环境修复中的应用。
本发明的另一实施方案提供上述新型聚苯胺/二氧化钛复合材料在清除土壤、水中重金属方面的应用。所述重金属优选铬、铅。
本发明的另一实施方案提供上述新型聚苯胺/二氧化钛复合材料在去除农药残留中的应用。所述农药优选有机氯农药或菊酯类农药。有机氯农药优选氯丹、毒杀酚,菊酯类农药优选甲氰菊酯、联苯菊酯。
本发明所述聚苯胺(5612-44-2)可以通过商业购买或由如下方法制备:
将苯胺加入酸液中,冰浴下,滴加过硫酸铵溶液,继续在冰浴下反应6-10h,过滤、沉淀依次用水、无水乙醇洗涤,于50-60℃条件下真空干燥18-24h即得所述聚苯胺;所述酸液优选稀盐酸或稀硫酸,其摩尔浓度为1-2mol/L,每毫升苯胺使用1.5-2.5g过硫酸铵,使用20-25mL酸液。
与现有技术相比,本发明的优点在于:本发明通过使用离子液体、巯基乙酸修饰改性获得一种新型聚苯胺/二氧化钛复合材料,其能有效地清除环境中(水、土壤)中重金属铬和铅以及农药残留;离子液体与巯基乙酸在改性修饰合成新型聚苯胺/二氧化钛复合材料中的作用不可替代;而且本发明中各试剂的加料顺序对合成产品——聚苯胺/二氧化钛复合材料的性能起决定性作用。
附图说明
图1是产品A的SEM图;
图2是产品C的SEM图;
图3是产品D的SEM图;
图4是产品E的SEM图;
图5是产品F的SEM图。
具体实施方式
为了便于对本发明的进一步理解,下面提供的实施例对其做了更详细的说明。但是这些实施例仅供更好的理解发明而并非用来限定本发明的范围或实施原则,本发明的实施方式不限于以下内容。
实施例1聚苯胺的制备
将苯胺(20mL)加入1mol/L稀盐酸(500mL)中,冰浴下,滴加250mL过硫酸铵溶液(含过硫酸铵30g),继续在冰浴下反应6h,过滤、沉淀依次用水、无水乙醇洗涤,于50℃条件下真空干燥24h即得聚苯胺。
实施例2
将苯胺(10mL)加入2mol/L稀硫酸(200mL)中,冰浴下,滴加200mL过硫酸铵溶液(含过硫酸铵25g),继续在冰浴下反应10h,过滤、沉淀依次用水、无水乙醇洗涤,于60℃条件下真空干燥18h即得聚苯胺。
实施例3
(1)将1-乙基-3-甲基咪唑氯盐(1.0g)与无水乙醇(5.0g)混合均匀后,加入钛酸正丁酯(1.0g)搅拌1.0h后得混合液a;
(2)向混合液a中加入聚苯胺(100mg)和巯基乙酸(100mg)继续搅拌0.5h后,加去离子水(1.0g),升温至50℃继续搅拌2h后,过滤得沉淀,沉淀依次用乙醇、水洗涤后,于60℃条件下真空干燥24h后即得所述新型聚苯胺/二氧化钛复合材料312mg(以下简称产品A)。
实施例4
(1)将1-乙基-3-甲基咪唑溴盐(1.0g)与无水乙醇(10.0g)混合均匀后,加入钛酸正丁酯(1.0g)搅拌0.5h后得混合液a;
(2)向混合液a中加入聚苯胺(200mg)和巯基乙酸(200mg)继续搅拌1.0h后,加蒸馏水(1.0g),升温至60℃继续搅拌1h后,过滤得沉淀,沉淀依次用乙醇、水洗涤后,于80℃条件下真空干燥12h后即得所述新型聚苯胺/二氧化钛复合材料428mg(以下简称产品B)。
实施例5
(1)将1-乙基-3-甲基咪唑氯盐(1.0g)与无水乙醇(5.0g)混合均匀后,加入钛酸正丁酯(1.0g)搅拌1.0h后得混合液a;
(2)向混合液a中加入聚苯胺(100mg)和冰乙酸(100mg)继续搅拌0.5h后,加去离子水(1.0g),升温至50℃继续搅拌2h后,过滤得沉淀,沉淀依次用乙醇、水洗涤后,于60℃条件下真空干燥24h后即得聚苯胺/二氧化钛复合材料278mg(以下简称产品C)。
实施例6
将1-乙基-3-甲基咪唑氯盐(1.0g)、无水乙醇(5.0g)、钛酸正丁酯(1.0g)、聚苯胺(100mg)和巯基乙酸(100mg)、去离子水(1.0g)混合均匀升温至50℃继续搅拌2h后,过滤得沉淀,沉淀依次用乙醇、水洗涤后,于60℃条件下真空干燥24h后即得聚苯胺/二氧化钛复合材料330mg(以下简称产品D)。
实施例7
(1)将1-乙基-3-甲基咪唑氯盐(1.0g)与无水乙醇(5.0g)混合均匀后,加入钛酸正丁酯(1.0g)搅拌1.0h后得混合液a;
(2)向混合液a中加入聚苯胺(100mg)继续搅拌0.5h后,加去离子水(1.0g),升温至50℃继续搅拌2h后,过滤得沉淀,沉淀依次用乙醇、水洗涤后,于60℃条件下真空干燥24h后即得聚苯胺/二氧化钛复合材料305mg(以下简称产品E)。
实施例8
(1)将钛酸正丁酯(1.0g)与无水乙醇(5.0g)混合均匀后,继续搅拌1.0h后得混合液a;
(2)向混合液a中加入聚苯胺(100mg)和巯基乙酸(100mg)继续搅拌0.5h后,加去离子水(1.0g),升温至50℃继续搅拌2h后,过滤得沉淀,沉淀依次用乙醇、水洗涤后,于60℃条件下真空干燥24h后即得聚苯胺/二氧化钛复合材料322mg(以下简称产品F)。
实施例3、5-8中使用的聚苯胺由实施例1制备得到的,实施例4使用的聚苯胺为市售聚苯胺(5612-44-2)。按照中国发明专利申请号:CN201610042772.0实施例1记载的方法制备聚苯胺修饰的介孔单晶二氧化钛微球(以下简称产品G)。
实施例9重金属清除实验
(1)水中铬清除实验
各取200mL六价铬标准水溶液(10mg/L),分别加入20mg产品A、B、C、D、E、F、G,搅拌4小时后;加入产品A、B的标准溶液中六价铬的含量小于100μg/L,加入产品C-G的标准溶液中六价铬的含量均大于7.5mg/L。
(2)土壤中铅清除实验
各取500g含铅Pb2+的土壤样本(每克土壤含铅2mg),分别加入20mg产品A、F、G,加水混匀使之成泥浆状,吸附8小时后,再分别补加20mg相应的产品A、F、G,混匀,继续吸附8小时后检测,结果表明产品A对土壤样本中铅的清除率达78.6%,产品F、G对土壤样本中铅的清除率不足20%。
实施例10土壤中农药残留的降解试验
土壤样品选择:样品1:氯丹、毒杀酚的含量均为400mg/kg;样品2:甲氰菊酯、联苯菊酯的含量均为400mg/kg。
实验方法:各取7份2kg样品1和2,分别加入产品A-G(各1.0g),混合均匀,保证含水量在20%-30%,48小时后,再分别各自补加相应的产品A-G(各1.0g),混合均匀后,48小时后,检测土壤中农药的含量,结果见下表。
Claims (8)
1.一种新型聚苯胺/二氧化钛复合材料,其特征在于所述新型聚苯胺/二氧化钛复合材料的制备方法包括如下步骤:
(1)将离子液体与无水乙醇混合均匀后,加入钛酸正丁酯搅拌0.5-1.0h后得混合液a;
(2)向混合液a中加入聚苯胺和巯基乙酸继续搅拌0.5-1.0h后,加水,升温至50-60℃继续搅拌1-2h后,过滤得沉淀,沉淀经后处理即得所述新型聚苯胺/二氧化钛复合材料;
步骤(1)中所述离子液体选自1-乙基-3-甲基咪唑卤盐,离子液体、无水乙醇、钛酸正丁酯的质量比为1:5-10:1;
步骤(2)中聚苯胺的用量为钛酸正丁酯质量的0.1-0.2倍,巯基乙酸与聚苯胺的质量比为1:1,水的用量与钛酸正丁酯质量用量相同。
2.权利要求1所述的新型聚苯胺/二氧化钛复合材料,其特征在于所述离子液体选自1-乙基-3-甲基咪唑氯盐、1-乙基-3-甲基咪唑溴盐。
3.权利要求1-2任一项所述的新型聚苯胺/二氧化钛复合材料,其特征在于所述水优选为去离子水或蒸馏水。
4.权利要求1-3任一项所述的新型聚苯胺/二氧化钛复合材料,其特征在于所述后处理为依次用乙醇、水洗涤后,于60-80℃条件下真空干燥12-24h。
5.权利要求1-4任一项所述的新型聚苯胺/二氧化钛复合材料在环境修复中的应用。
6.权利要求1-5任一项所述的新型聚苯胺/二氧化钛复合材料在去除农药残留中的应用。
7.权利要求6所述的应用,其特征在于所述农药优选有机氯农药或菊酯类农药。
8.权利要求7所述的应用,其特征在于有机氯农药优选氯丹、毒杀酚,菊酯类农药优选甲氰菊酯、联苯菊酯。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810340567.1A CN108554459B (zh) | 2018-04-14 | 2018-04-14 | 一种聚苯胺/二氧化钛复合材料及其在环境修复中的应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810340567.1A CN108554459B (zh) | 2018-04-14 | 2018-04-14 | 一种聚苯胺/二氧化钛复合材料及其在环境修复中的应用 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108554459A true CN108554459A (zh) | 2018-09-21 |
CN108554459B CN108554459B (zh) | 2020-07-28 |
Family
ID=63535334
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810340567.1A Active CN108554459B (zh) | 2018-04-14 | 2018-04-14 | 一种聚苯胺/二氧化钛复合材料及其在环境修复中的应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108554459B (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110120307A (zh) * | 2019-04-03 | 2019-08-13 | 江汉大学 | 一种复合材料的制备方法、复合材料及超级电容器 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007146680A1 (en) * | 2006-06-06 | 2007-12-21 | Florida State University Research Foundation , Inc. | Stabilized silica colloid |
WO2011006667A2 (en) * | 2009-07-17 | 2011-01-20 | Technische Universität Graz | Non-leaching heterogeneous catalyst systems for coupling reactions |
CN103144388A (zh) * | 2013-03-21 | 2013-06-12 | 四川农业大学 | 一种聚苯胺/二氧化钛/石墨烯导电复合膜的制备方法及其应用 |
CN104624244A (zh) * | 2014-12-10 | 2015-05-20 | 程如铁 | 一种聚苯胺/TiO2纳米复合膜的制备方法 |
CN105618154A (zh) * | 2016-02-26 | 2016-06-01 | 北京科技大学 | 一种Au-PANI-TiO2三元光催化剂的制备方法 |
-
2018
- 2018-04-14 CN CN201810340567.1A patent/CN108554459B/zh active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007146680A1 (en) * | 2006-06-06 | 2007-12-21 | Florida State University Research Foundation , Inc. | Stabilized silica colloid |
WO2011006667A2 (en) * | 2009-07-17 | 2011-01-20 | Technische Universität Graz | Non-leaching heterogeneous catalyst systems for coupling reactions |
CN103144388A (zh) * | 2013-03-21 | 2013-06-12 | 四川农业大学 | 一种聚苯胺/二氧化钛/石墨烯导电复合膜的制备方法及其应用 |
CN104624244A (zh) * | 2014-12-10 | 2015-05-20 | 程如铁 | 一种聚苯胺/TiO2纳米复合膜的制备方法 |
CN105618154A (zh) * | 2016-02-26 | 2016-06-01 | 北京科技大学 | 一种Au-PANI-TiO2三元光催化剂的制备方法 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110120307A (zh) * | 2019-04-03 | 2019-08-13 | 江汉大学 | 一种复合材料的制备方法、复合材料及超级电容器 |
Also Published As
Publication number | Publication date |
---|---|
CN108554459B (zh) | 2020-07-28 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Wong et al. | The removal of basic and reactive dyes using quartenised sugar cane bagasse | |
CN102161781B (zh) | 一种吸附重金属离子的改性壳聚糖材料及其制备方法 | |
CN102527347B (zh) | 一种磁性壳聚糖/阳离子表面活性剂改性沸石吸附剂及其制备方法和应用 | |
CN106512950A (zh) | 一种表面活性剂改性沸石吸附剂的制备方法 | |
CN108940237B (zh) | 一种磁性吸附材料的制备方法与应用 | |
CN108479857A (zh) | 一种离子液体修饰的聚苯胺/二氧化钛复合材料的制备方法 | |
CN106824113B (zh) | 一种咪唑类离子液体改性壳聚糖吸附剂的制备及其应用 | |
CN1171805C (zh) | 菌丝体表面包覆生物吸附剂及其制备方法 | |
Su et al. | Preparation of a surface molecular‐imprinted adsorbent for Ni2+ based on Penicillium chrysogenum | |
Zuo et al. | Biosorption of copper, zinc and cadmium using sodium hydroxide immersed Cymbopogon schoenanthus L. Spreng (lemon grass) | |
Kalkan et al. | Experimental Study to Remediate Acid Fuchsin Dye Using Laccase-Modified Zeolite from Aqueous Solutions. | |
Husin et al. | Sorption equilibrium and kinetics of oil from aqueous solution using banana pseudostem fibers | |
CN106135275A (zh) | 一种有机改性并负载银离子的海泡石抗菌粉体的制备方法 | |
CN104841287B (zh) | 一种多功能分等级油水分离复合膜材料的制备方法 | |
CN109589951A (zh) | 一种用于回收溶液中金硫代硫酸根络离子的活性炭的制备方法 | |
CN108160025A (zh) | 一种牡蛎壳粉氧化铁纳米复合材料的制备方法及应用 | |
CN108311118A (zh) | 一种改性合成沸石重金属离子吸附材料的制备方法 | |
CN108554459A (zh) | 一种新型聚苯胺/二氧化钛复合材料及其在环境修复中的应用 | |
CN107413305A (zh) | 聚苯胺‑硅藻土/Fe3 O4‑壳聚糖复合材料的制备方法 | |
CN105149003B (zh) | 一种壳聚糖双金属配合物催化剂的制备方法及应用 | |
CN106622191A (zh) | 超支化聚酰胺胺交联改性沸石、其制备方法及其在重金属废水处理中的应用 | |
CN112058219A (zh) | 一种高炉镍铁渣基沸石分子筛的制备方法及应用 | |
CN108525640A (zh) | 一种提高凹凸棒土吸附性能的改性工艺 | |
CN106861685B (zh) | 一种Ag/Ag2O/TiO2/硅藻土复合光催化材料的制备方法 | |
CN107266606A (zh) | 一种从海带加工废液中提取岩藻聚糖硫酸酯的新工艺 |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant |