CN106423301A - 一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料及其制备和应用 - Google Patents
一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料及其制备和应用 Download PDFInfo
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- CN106423301A CN106423301A CN201611095892.3A CN201611095892A CN106423301A CN 106423301 A CN106423301 A CN 106423301A CN 201611095892 A CN201611095892 A CN 201611095892A CN 106423301 A CN106423301 A CN 106423301A
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- 229910002900 Bi2MoO6 Inorganic materials 0.000 title claims abstract description 43
- 239000000835 fiber Substances 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 38
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 23
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000005406 washing Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000004753 textile Substances 0.000 claims abstract description 10
- 238000005470 impregnation Methods 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 48
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 34
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 239000003381 stabilizer Substances 0.000 claims description 9
- HFBMWMNUJJDEQZ-UHFFFAOYSA-N acryloyl chloride Chemical compound ClC(=O)C=C HFBMWMNUJJDEQZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- ZXQBXHYVVKUTOV-UHFFFAOYSA-N C(CCCCC)I.[F] Chemical compound C(CCCCC)I.[F] ZXQBXHYVVKUTOV-UHFFFAOYSA-N 0.000 claims description 7
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- 229920000428 triblock copolymer Polymers 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 239000008363 phosphate buffer Substances 0.000 claims description 4
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 3
- 229960003511 macrogol Drugs 0.000 claims description 3
- 239000000176 sodium gluconate Substances 0.000 claims description 3
- 235000012207 sodium gluconate Nutrition 0.000 claims description 3
- 229940005574 sodium gluconate Drugs 0.000 claims description 3
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 3
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- NCSHGROOCJHAFK-UHFFFAOYSA-N [Cl].N#CC#N Chemical compound [Cl].N#CC#N NCSHGROOCJHAFK-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims 1
- 229910001950 potassium oxide Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- 239000002202 Polyethylene glycol Substances 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 229920001223 polyethylene glycol Polymers 0.000 abstract description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 2
- 238000004332 deodorization Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000004043 dyeing Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 4
- 235000019799 monosodium phosphate Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 4
- 235000011008 sodium phosphates Nutrition 0.000 description 4
- 239000012265 solid product Substances 0.000 description 4
- 239000000872 buffer Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- BULLJMKUVKYZDJ-UHFFFAOYSA-N 1,1,1,2,2,3,3,4,4,5,5,6,6-tridecafluoro-6-iodohexane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)I BULLJMKUVKYZDJ-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000282320 Panthera leo Species 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000009990 desizing Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000009992 mercerising Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 238000005070 sampling Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 1
- 229940019931 silver phosphate Drugs 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- 238000009955 starching Methods 0.000 description 1
- 230000036561 sun exposure Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Nanotechnology (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
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Abstract
本发明涉及一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料及其制备和应用,多功能碳纳米管在纺织纤维表面构筑三维连续结构,其中多功能纳米管表面负载有纳米Bi2MoO6;制备:将纤维浸渍到含有碳纳米管复合Bi2MoO6和聚乙二醇2000分散液中,60‑80℃反应2‑4h,烘干,水洗,重复浸渍,烘干和水洗过程3‑5次,即得。本发明的成本低廉,制备方法简单,对设备的要求低,可操作性好;本发明的水处理剂可以去除水中高浓度有机污染物,适用于各种废水的深度处理,环保无二次污染,且具有抗菌、除臭、可以吸附其他重金属离子等优点。
Description
技术领域
本发明属于催化剂材料及其制备和应用领域,特别涉及一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料及其制备和应用。
背景技术
全球仅约10%的水是直接为人类所用。最大的份额,70%用于农业,剩余的20%为工业用。中国的排污约为全球的20%,而它只得到全球的5%的新鲜水。因此,解决污染问题已列入议事日程。在纺织印染、皮革、造纸行业加工过程中,大量使用了污染环境和对人体有害的助剂,这些助剂大多以液体的形态排放而污染环境,生物降解性差,毒性大,游离甲醛含量高,重金属离子的含量超标。其中,印染湿整理更是无可争议地成为水污染大户。从上浆开始到退浆、水洗、练漂、丝光,然后染色印花、可能还需涂层,按此流程每道工序都涉及水洗,而每道工序每千克材料需20L耗水。结果是湿整理过程中每千克原棉的用水量加起来多达200L。当一件标准的男式衬衣定制后在商店橱窗展示时,超过2000L水在生产加工它时被用掉了(布料:纯棉,125g/m)。
目前使用的处理废水的方法主要有:物理分离法、生物降解法、化学分解法,但这些方法都存在一定的局限性,不利于可持续发展。
发明内容
本发明所要解决的技术问题是提供一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料及其制备和应用,本发明方法操作简单,成本低廉,对设备的要求低;水处理剂适用于各种废水的深度处理,环保无二次污染。
本发明的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料,多功能碳纳米管在纺织纤维表面构筑三维连续结构,其中多功能纳米管表面负载有纳米Bi2MoO6,形成纤维/碳纳米管/Bi2MoO6三维可循环催化材料。
多功能纳米管的比表面积为20~150m2/g;所述纳米Bi2MoO6为单斜晶型结构,晶粒大小为15~200nm;纺织纤维为柔性纺织纤维;纳米Bi2MoO6与多功能纳米管的质量比为1:5~20。
本发明的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,包括:
(1)将Bi2MoO6、稳定剂、模板剂、多功能碳纳米管加入到磷酸盐缓冲液中,搅拌30~60min,形成悬浊液,然后碱液调节pH=5~6,180℃反应3~5h,得到多功能碳纳米管复合Bi2MoO6;其中Bi2MoO6与多功能碳纳米管的质量比为1:5~1:20;
(2)将纤维浸渍到0.05~0.75g/L碳纳米管复合Bi2MoO6和0.025~0.375g/L聚乙二醇2000分散液中,60-80℃反应2-4h,烘干,水洗,重复浸渍,烘干和水洗过程3-5次,即得纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料。
所述步骤(1)中悬浊液中Bi2MoO6浓度为0.01~0.2mol/L;稳定剂为乙二胺四乙酸二钠、乙二胺四乙酸四钠、葡萄糖酸钠、丁烷四羧酸中的一种,稳定剂浓度为0.01~0.1mol/L。
所述步骤(1)中模板剂为质量比1:3的三嵌段聚醚P123和三嵌段共聚物F127的混合物;模板剂浓度为0.01~0.1mol/L。
所述步骤(1)中磷酸盐缓冲液由浓度0.025~0.05mol/L磷酸二氢钠和0.05~0.1mol/L磷酸氢钠组成;碱液为:0.5mol/L~1.5mol/L的氢氧化钠或氢氧化钾的水溶液。
所述步骤(1)中多功能碳纳米管的制备方法,包括:
(a)将碳纳米管CNTs加入到FeCl2溶液中,调节pH=3,然后加入H2O2,室温超声0.5-2h,室温磁力搅拌6-8h,抽滤水洗到中性,抽滤,真空干燥,得产物a;其中碳纳米管CNTs、FeCl2溶液、H2O2的比例为150~200mg:30~40mL:30~40mL;优选碳纳米管CNTs、FeCl2溶液、H2O2的比例为200mg:4 0mL:40mL;其中真空干燥为60℃下真空干燥24h;
(b)在通氮气条件下,在干燥三口烧瓶中,将产物a分散于溶剂DMF中,冰水浴冷却,0℃加入NaH,搅拌20-30min,然后逐渐升温到85-90℃,逐滴加入1-全氟氟己基碘,超声反应18-24h,加水猝灭反应,洗涤、在真空烘箱中50℃干燥96h,得到黑色颗粒产物b;其中产物a、溶剂、NaH、1-全氟氟己基碘的比例为1.5~3g:100~200mL:300~522mg:2-3mL;
优选产物a、溶剂、NaH、1-全氟氟己基碘的比例为3g:200mL:522mg:3mL;
(c)将产物b分散在水中,加入NaOH,超声分散0.5~1h,三聚氯氰分散在水中后加入反应体系中,0~5℃搅拌反应24-48h,离心洗涤(依次用水和乙醇离心洗涤),25℃真空烘干96h,得到产物c;其中产物b、NaOH、三聚氯氰的比例为1~2g:300~438mg:1~2g;优选产物b、NaOH、三聚氯氰的比例为2g:438mg:2g;
(d)通氮气条件下,在干燥三口烧瓶中加入产物c,三乙胺,DMF,冰水浴冷却,0℃下逐滴加入丙烯酰氯(按体积比1:10溶于DMF中),超声反应12-24h,离心洗涤(依次用乙醇和水离心洗涤),室温真空烘干,得到黑色固体产物d;其中产物c、三乙胺、DMF、丙烯酰氯的比例为1~1.5g:3~2.4mL:100~150mL:0.5~1mL;优选:产物c、三乙胺、DMF、丙烯酰氯的比例为1.5g:2.4mL:150mL:1mL;
(e)产物d,亚磷酸二甲酯,DMF混合,将DBU溶于溶剂(按体积比为0.3:20溶于溶剂DMF中)中后逐滴加入反应体系中,25℃超声反应24-48h,离心洗涤(依次用乙醇和水离心洗涤(300mL×3次)),室温真空烘干,得到多功能碳纳米管;其中产物d、亚磷酸甲酯、DBU的比例为1g、300~415mg:0.5mol;其中优选产物d、亚磷酸甲酯、DBU的比例为1g:415mg:0.5mol。
所述步骤(a)中FeCl2溶液的质量百分浓度为30%。
所述步骤(a)中碳酸钠溶液调节pH值。
本发明的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的应用,作为水处理剂的应用,用于废水的处理,具体为将纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料加入废水中,日光光照3-8h。
碳纳米管作为一种多孔物质,具有特殊的层间特性,可在其表面负载Bi2MoO6微粒,制备成负载型催化剂。这种负载型光催化剂可以提高光催化剂的分散性,利于回收重复利用。本发明在高比表面积碳管表面构筑纳米半导体材料,然后将负载半导体材料的高比表面积碳管在织物表面构筑三维连续结构,然后形成新型的纺织纤维/碳纳米管/半导体异质连续网格结构,利用柔性纤维材料的多孔性和毛细管效应,使纤维既能吸附污染物,同时又能通过吸附污染物在纤维表面富集而为纳米光催化材料提供高浓度反应物坏境,这在很大程度上加快了光催化降解反应速率。此外,纤维的吸附作用还可能使光催化降解反应产生的中间副产物在生成时即被吸附并被进一步氧化降解为简单的无机物,如二氧化碳和水。这样纤维不仅能够浓缩污染物,加速光催化降解反应,而且可以减少中间副产物,及时释放产物,不断推进降解反应。同时也充分发挥碳纳米管的高比表面积有效分散半导体材料,增加催化剂与污染物的接触界面,为光催化反应提供更多的反应活性点,并确保能够实现光生电子的定向传输、有效提高其与空穴分离效率,提高其光催化活性。
本发明利用碳纳米管的多孔、吸附能力强、与水易分离等特点和Bi2MoO6的光催化活性结合起来,将纳米Bi2MoO6成功地负载到碳纳米管上,制备成可以悬浮于废水中而又可以顺利与水分离的高催化活性的可见光光催化材料,并且将其应用于废水的深度处理,可以实现对水中高浓度有机污染物氧化去除,而不是转移到其他地方,是一个环保型的工艺技术。
有益效果
(1)本发明成本低廉,制备方法简单,对设备的要求低,可操作性好;
(2)本发明的水处理剂可以去除水中高浓度有机污染物,适用于各种废水的深度处理,环保无二次污染,且具有抗菌、除臭、可以吸附其他重金属离子等优点;
(3)本发明的水处理剂可以克服现有磷酸银复合水处理剂的不足,水处理效果好,可以循环使用。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
(1)将150mg CNTs加入到30mL的质量百分浓度30%FeCl2溶液中,调节pH=3,然后加入30mL H2O2,室温超声0.5h,室温磁力搅拌6h,加水500mL,抽滤水洗到中性,抽滤。在60℃下真空干燥24h得产物a;
在通氮气条件下,在干燥三口烧瓶中将1.5g产物a分散于100mL DMF中,冰水浴冷却,0℃加入NaH 300mg,继续搅拌20min。然后逐渐升温到85℃,逐滴加入2mL 1-全氟氟己基碘,超声反应18h,加少量水猝灭反应,依次DMF、乙醇和水离心洗涤。得到的黑色颗粒产物b在真空烘箱中50℃干燥96h;
将1g黑色产物b分散在50mL水中,加入300mg NaOH,超声分散0.5h,1g三聚氯氰分散在50mL水中,加入三口烧瓶中,0℃搅拌反应24h。依次用水和乙醇离心洗涤。25℃真空烘干96h,得到产物c;通氮气条件下,在干燥三口烧瓶中加入1g产物c,三乙胺2.4mL,DMF100mL。冰水浴冷却,0℃下逐滴加入丙烯酰氯0.5mL(溶于10mL DMF),超声反应12h。依次用乙醇和水离心洗涤。得到的黑色固体产物d,室温真空烘干;
三口烧瓶中加入1g产物d,亚磷酸二甲酯300mg,DMF 150mL,将0.3mL DBU(0.5mol)溶于20mL DMF中,逐滴加入上述三口烧瓶中,25℃超声反应24h。依次用乙醇和水离心洗涤(300mL×3次)室温真空烘干,得到多功能碳纳米管e。
(2)将Bi2MoO6、乙二胺四乙酸二钠、质量比为1:3的三嵌段聚醚P123和三嵌段共聚物F127的混合物和上述步骤(1)中多功能碳纳米管e加入到浓度为0.025mol/L磷酸二氢钠和0.05mol/L磷酸氢钠组成的缓冲液中,搅拌30min,形成悬浊液;其中Bi2MoO6的浓度为0.01mol/L、稳定剂的浓度为0.01mol/L、模板剂的浓度为0.05mol/L。
(3)用浓度0.5mol/L的氢氧化钠水溶液调节上述悬浊液的pH值为5,加热80℃下,回流6h,过滤,得碳纳米管复合Bi2MoO6;其中Bi2MoO6与碳纳米管的质量比为1:5
(4)将麻纤维浸渍到含有0.05g/L碳纳米管复合Bi2MoO6和0.025g/L聚乙二醇2000分散液中,60℃反应2h,烘干,水洗,重复浸渍,烘干和水洗过程3次,即得纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料。
实施例2
(1)将175mg CNTs加入到35mL的30%FeCl2溶液中,调节pH=3,然后加入35mLH2O2,室温超声1.5h,室温磁力搅拌87h,加水500mL,抽滤水洗到中性,抽滤。在60℃下真空干燥24h得产物a;
在通氮气条件下,在干燥三口烧瓶中将2.5g产物a分散于150mL DMF中,冰水浴冷却,0℃加入NaH 411mg,继续搅拌30min。然后逐渐升温到88℃,逐滴加入2.5mL 1-全氟氟己基碘,超声反应全氟己基碘,超声反应20h。加少量水猝灭反应,依次DMF、乙醇和水离心洗涤。得到的黑色颗粒产物b在真空烘箱中50℃干燥96h;
将1.5g产物b分散在50mL水中,加入438mg NaOH,超声分散1h,1.5g三聚氯氰分散在50mL水中,加入三口烧瓶中,2.5℃搅拌反应36h。依次用水和乙醇离心洗涤。25℃真空烘干96h,得到产物c;
通氮气条件下,在干燥三口烧瓶中加入1.5g产物c,三乙胺2.8mL,DMF 125mL。冰水浴冷却,0℃下逐滴加入丙烯酰氯0.75mL(溶于10mL DMF),超声反应18h。依次用乙醇和水离心洗涤。得到的黑色固体产物d,室温真空烘干;三口烧瓶中加入产物1g d,亚磷酸二甲酯350mg,DMF 150mL,将0.18mL DBU(0.3mol)溶于20mL DMF中,逐滴加入上述三口烧瓶中,25℃超声反应36h。依次用乙醇和水离心洗涤(300mL×3次)室温真空烘干,得到多功能碳纳米管e;
(2)将Bi2MoO6、葡萄糖酸钠、质量比为1:3的三嵌段聚醚P123和三嵌段共聚物F127的混合物和上述步骤(1)中多功能碳纳米管e加入到浓度为0.03mol/L磷酸二氢钠和0.05mol/L磷酸氢钠组成的缓冲液中,搅拌45min,形成悬浊液;其中Bi2MoO6的浓度为0.01mol/L、稳定剂的浓度为0.03mol/L、模板剂的浓度为0.07mol/L。
(3)用浓度0.5mol/L的氢氧化钠水溶液调节上述悬浊液的pH值为7,加热90℃下,回流16h,过滤,得碳纳米管复合Bi2MoO6;其中Bi2MoO6与碳纳米管的质量比为1:15。
(4)将涤纶纤维浸渍到含有0.375g/L碳纳米管复合Bi2MoO6和0.15g/L聚乙二醇2000分散液中,70℃反应3h,烘干,水洗,重复浸渍,烘干和水洗过程4次,即得纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料。
实施例3
(1)将200mg CNTs加入到40mL的30%FeCl2溶液中,调节pH=3,然后加入40mLH2O2,室温超声2h,室温磁力搅拌8h,加水500mL,抽滤水洗到中性,抽滤。在60℃下真空干燥24h得产物a;
在通氮气条件下,在干燥三口烧瓶中将3g产物a分散于200mL DMF中,冰水浴冷却,0℃加入NaH 522mg,继续搅拌30min。然后逐渐升温到90℃,逐滴加入3mL 1-全氟氟己基碘,超声反应全氟己基碘,超声反应24h。加少量水猝灭反应,依次DMF、乙醇和水离心洗涤。得到的黑色颗粒产物b在真空烘箱中50℃干燥96h;
将2g产物b分散在50mL水中,加入438mg NaOH,超声分散1h,2g三聚氯氰分散在50mL水中,加入三口烧瓶中,0~5℃搅拌反应48h。依次用水和乙醇离心洗涤。25℃真空烘干96h,得到产物c;
通氮气条件下,在干燥三口烧瓶中加入1.5g产物c,三乙胺2.4mL,DMF 150mL。冰水浴冷却,0℃下逐滴加入丙烯酰氯1mL(溶于10mL DMF),超声反应24h。依次用乙醇和水离心洗涤。得到的黑色固体产物d,室温真空烘干;
三口烧瓶中加入产物d1g,亚磷酸二甲酯415mg,DMF 150mL,将0.3mL DBU(0.5mol)溶于20mL DMF中,逐滴加入上述三口烧瓶中,25℃超声反应48h。依次用乙醇和水离心洗涤(300mL×3次)室温真空烘干,得到多功能碳纳米管e;
(2)将Bi2MoO6、丁烷四羧酸、质量比为1:3的三嵌段聚醚P123和三嵌段共聚物F127的混合物和上述步骤(1)中多功能碳纳米管e加入到浓度为0.05mol/L磷酸二氢钠和0.1mol/L磷酸氢钠组成的缓冲液中,搅拌60min,形成悬浊液;其中Bi2MoO6的浓度0.15mol/L、稳定剂的浓度为0.05mol/L、模板剂的浓度为0.1mol/L。
(3)用浓度1.5mol/L的氢氧化钾水溶液调节上述悬浊液的pH值为9,加热100℃下,回流24h,过滤,得碳纳米管复合Bi2MoO6;其中Bi2MoO6与碳纳米管的质量比为1:20。
(4)将芳纶纤维浸渍到含有0.75g/L碳纳米管复合Bi2MoO6和0.375g/L聚乙二醇2000分散液中,80℃反应4h,烘干,水洗,重复浸渍,烘干和水洗过程5次,即得纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料。
以同一时间取样的印染厂的印染废水为处理对象,在含有0.2g/l染料废水中分别加入浓度5g/l催化纤维材料的实施例1~3所得的水处理剂,经过6小时日光照射后,水处理剂对印染废水的脱色率如下表所示:
Claims (10)
1.一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料,其特征在于:多功能碳纳米管在纺织纤维表面构筑三维连续结构,其中多功能纳米管表面负载有纳米Bi2MoO6,形成纤维/碳纳米管/Bi2MoO6三维可循环催化材料。
2.根据权利要求1所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料,其特征在于:多功能纳米管的比表面积为20~150m2/g;所述纳米Bi2MoO6为单斜晶型结构,晶粒大小为15~200nm;纺织纤维为柔性纺织纤维;纳米Bi2MoO6与多功能纳米管的质量比为1:5~20。
3.一种如权利要求1-2任一所述的纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,包括:
(1)将Bi2MoO6、稳定剂、模板剂、多功能碳纳米管加入到磷酸盐缓冲液中,搅拌30~60min,形成悬浊液,然后碱液调节pH=5~6,180℃反应3~5h,得到碳纳米管复合Bi2MoO6;其中Bi2MoO6与多功能碳纳米管的质量比为1:5~1:20;
(2)将纤维浸渍到含有碳纳米管复合Bi2MoO6和聚乙二醇2000分散液中,60-80℃反应2-4h,烘干,水洗,重复浸渍,烘干和水洗过程3-5次,即得纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料。
4.根据权利要求3所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,其特征在于:所述步骤(1)中悬浊液中Bi2MoO6浓度为0.01~0.2mol/L;稳定剂为乙二胺四乙酸二钠、乙二胺四乙酸四钠、葡萄糖酸钠、丁烷四羧酸中的一种,稳定剂浓度为0.01~0.1mol/L。
5.根据权利要求3所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,其特征在于:所述步骤(1)中模板剂为质量比1:3的三嵌段聚醚P123和三嵌段共聚物F127的混合物;模板剂浓度为0.01~0.1mol/L;磷酸盐缓冲液由浓度0.025~0.05mol/L磷酸二氢钠和0.05~0.1mol/L磷酸氢钠组成;碱液为:0.5mol/L~1.5mol/L的氢氧化钠或氢氧化钾的水溶液。
6.根据权利要求3所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,其特征在于:所述步骤(2)分散液中含有0.05~0.75g/L碳纳米管复合Bi2MoO6和0.025~0.375g/L聚乙二醇2000。
7.根据权利要求3所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,其特征在于:所述步骤(1)中多功能碳纳米管的制备方法,包括:
(a)将碳纳米管CNTs加入到FeCl2溶液中,调节pH=3,然后加入H2O2,室温超声0.5-2h,室温磁力搅拌6-8h,抽滤水洗到中性,抽滤,真空干燥,得产物a;其中碳纳米管CNTs、FeCl2溶液、H2O2的比例为150~200mg:30~40mL:30~40mL;
(b)在通氮气条件下,将产物a分散于溶剂中,冰水浴冷却,0℃加入NaH,搅拌20-30min,然后逐渐升温到85~90℃,逐滴加入1-全氟氟己基碘,超声反应18-24h,加水猝灭反应,洗涤、干燥,得到产物b;其中产物a、溶剂、NaH、1-全氟氟己基碘的比例为1.5~3g:100~200mL:300~522mg:2-3mL;
(c)将产物b分散在水中,加入NaOH,超声分散0.5~1h,三聚氯氰分散在水中后加入反应体系中,0~5℃搅拌反应24-48h,离心洗涤,真空烘干,得到产物c;其中产物b、NaOH、三聚氯氰的比例为1~2g:300~438mg:1~2g;
(d)通氮气条件下,产物c,三乙胺,DMF,冰水浴冷却,0℃下逐滴加入丙烯酰氯,超声反应12-24h,离心洗涤,室温真空烘干,得到产物d;其中产物c、三乙胺、DMF、丙烯酰氯的比例为1~1.5g:3~2.4mL:100~150mL:0.5~1mL;
(e)产物d,亚磷酸二甲酯,DMF混合,将DBU溶于溶剂中后逐滴加入反应体系中,25℃超声反应24-48h,离心洗涤,室温真空烘干,得到多功能碳纳米管;其中产物d、亚磷酸甲酯、DBU的比例为1g、300~415mg:0.5mol。
8.根据权利要求7所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,其特征在于:所述步骤(a)中FeCl2溶液的质量百分浓度为30%。
9.根据权利要求7所述的一种纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的制备方法,其特征在于:所述步骤(a)中碳酸钠溶液调节pH值。
10.一种如权利要求1-2任一所述的纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料的应用,其特征在于:作为水处理剂的应用,用于废水的处理,具体为将纤维/碳纳米管/Bi2MoO6三维可循环高效催化材料加入废水中,日光光照3-8h。
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