CN107008331A - NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法及该催化剂的应用 - Google Patents
NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法及该催化剂的应用 Download PDFInfo
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- 229910003264 NiFe2O4 Inorganic materials 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000010949 copper Substances 0.000 claims abstract description 21
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims abstract description 20
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000975 dye Substances 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 10
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- 238000003756 stirring Methods 0.000 claims abstract description 9
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical class [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 6
- 239000008103 glucose Substances 0.000 claims abstract description 6
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 6
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
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- 239000008187 granular material Substances 0.000 claims description 11
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
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- 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 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000011109 contamination Methods 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 7
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- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 abstract 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 abstract 1
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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Abstract
本发明属于催化剂技术领域,具体涉及一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,该制备过程以六水合氯化镍、六水合三氯化铁、六水合醋酸铜、葡萄糖、氢氧化钠和去离子水为原料。首先六水合氯化镍和六水合三氯化铁配制成混合溶液,然后对混合溶液进行加热、分离、洗涤、烘干,得到磁性NiFe2O4纳米催化剂。其次,二水合醋铜溶于乙二醇甲醚并搅拌,再把NiFe2O4固体粉末加入到混合溶液中,搅拌加入葡萄糖,分离、洗涤、烘干获得磁性NiFe2O4/Cu2O复合纳米催化剂材料。该材料不但能效且快速吸附‑光催化去除水体中的有机染料,而且能通过磁铁回收催化剂。同时,具有制备简单和能重复使用的特点。
Description
技术领域
本发明属于催化剂技术领域,具体涉及一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法及该催化剂的应用。
背景技术
目前我国各种染料产量已达90万吨,染料废水已成为环境重点污染源之一。染料行业品种繁多,工艺复杂,其废水中含有大量的有机物,具有CODCr高、色泽深、酸碱性强等特点,一直是废水处理中的难题。于是开发新型水处理材料和新型工艺,控制有毒有机污染物已成为环境领域亟待解决的关键问题之一。经过几十年的研究发现,利用Cu2O、ZnO、TiO2等半导体可发生光催化使水分解成氢和氧,光催化反应能将有机污染物完全矿化成CO2、H2O等无机小分子物质,且反应条件温和,能耗低,安全无毒,操作简便,被视为一种理想的高效、低耗的绿色环境治理技术而受到环境专家的关注。据文献报道,氧化亚铜属于P型半导体,禁带宽度约为2.2ev,吸收波长为 563nm,能吸收可见光,可以将太阳光转化为电能或化学能,因此氧化亚铜在太阳光照射下即可发生光催化反应,是一种极具潜能的光催化剂。目前,氧化亚铜光催化材料的制备及其处理难降解的有机废水逐渐成为研究的热点。目前,光催化剂(尤其纳米光催化剂)在使用过程中还存在固液分离和回收困难,可能造成二次污染等问题,这严重阻碍了光催化技术的实际应用。氧化亚铜粉末状光催化剂处理废水的研究中,难以回收催化剂再次利用,一直是限制应用的难题之一。因此制备一种便于回收的氧化亚铜复合光催化剂是非常必要的。
为了提高可见光或太阳光对Cu2O的光催化性能,常用的方法是贵金属修饰、量子点敏化、半导体复合、染料敏化、过渡金属离子和非金属掺杂等。近年来出现的将磁性分离技术与固相催化剂/吸附剂相结合的方法,在解决环境污染问题中发挥了很好的作用。由于磁性光催化剂既具备悬浮相光催化剂的高效性,又可利用磁性分离技术高效快速地回收,实现资源的再利用,是一种环境友好型催化剂,也是未来水处理光催化剂的重要发展方向之一。
现有技术中有报道过磁性纳米复合物,但其一般制备的工艺都比较复杂,耗费较长的时间,光催化降解效率低,制备的催化剂颗粒较大,比表面积较小,光催化降解效率低等一些不足,因此优化 NiFe2O4/Cu2O磁性复合纳米材料的制备方法对促进经济发展具有重要的现实意义。
发明内容
本发明主要提供了一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,该方法工艺简单,制备的催化剂能效且快速吸附-光催化去除水体中的有机染料。其技术方案如下:
一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,其包括以下步骤:
Ⅰ)NiFe2O4的制备:
(1)按铁和镍的摩尔比为2:1-1.5分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中;
(2)向混合溶液中滴加碱性溶液调节pH值为10-14,将混合溶液加热至80-100℃保温2.5-3.5h;
(3)将加热后的溶液转移至反应釜中,将反应釜加热到600-800℃并保温2.5-3.5h;
(4)将加热后获得的粉末固体在磁场中进行分离,然后对磁性粉末洗涤并烘干,得到NiFe2O4催化剂颗粒;
Ⅱ)NiFe2O4/Cu2O磁性复合物的制备:
(1)将六水合醋酸铜搅拌溶于去离子水中,并超声处理;
(2)加入制备完成的NiFe2O4催化剂颗粒,NiFe2O4与醋酸铜的质量比为2-2.15:4.05,然后加入碱性溶液,并进行搅拌;
(3)加入葡萄糖溶液进行反应,混合液变成红褐色;
(4)将混合液冷却,使用磁铁磁吸固体物,清洗并干燥,得 NiFe2O4/Cu2O磁性复合纳米催化剂。
优选的,NiFe2O4催化剂颗粒的粒径为20-30nm,NiFe2O4/Cu2O 磁性复合纳米催化剂的粒径为10-30nm。
优选的,NiFe2O4/Cu2O磁性复合纳米催化剂的比表面积为 78.89m2/g。
NiFe2O4/Cu2O磁性复合纳米催化剂在处理染料废水有机污染物中的应用,所述磁性复合纳米催化剂对亚甲基蓝有机溶液的光催化降解效率达到98%以上。
采用上述方法,本发明具有以下优点:
本发明方法工艺简单,耗时较短,制得的复合磁性材料直径范围为10-30nm,材料比表面积为78.89m2/g,可以能效且快速吸附-光催化去除水体中的有机染料,对于亚甲基蓝有机溶液的光催化降解效率达到98%以上,对染料废水有机污染物处理效率高。而且能通过磁铁回收催化剂进行重复利用。
附图说明
图1为NiFe2O4/Cu2O的XRD图谱;
图2为NiFe2O4/Cu2O磁性复合纳米颗粒的SEM图片;
图3为NiFe2O4/Cu2O的Uv-Vis图谱;
图4为NiFe2O4/Cu2O磁性复合纳米催化剂对亚甲基蓝溶液的降解效果曲线。
具体实施方式
实施例1
一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,其包括以下步骤:
Ⅰ)NiFe2O4的制备:
(1)按铁和镍的摩尔比为2:1分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中;
(2)向混合溶液中滴加氢氧化钠溶液调节pH值为13,将混合溶液加热至90℃保温3h;
(3)将加热后的溶液转移至反应釜中,将反应釜加热到700℃并保温3h;
(4)将加热后获得的粉末固体在磁场中进行分离,然后对磁性粉末洗涤并烘干,得到黑色的NiFe2O4催化剂颗粒,NiFe2O4的直径为20-30nm;
Ⅱ)NiFe2O4/Cu2O磁性复合物的制备:
(1)在35℃下,将3.993g六水合醋酸铜搅拌溶于50ml去离子水中,搅拌15min,并超声处理60min;
(2)加入1.972g制备完成的NiFe2O4催化剂颗粒,搅拌15min,然后加入0.04g/mL的氢氧化钠溶液24mL,50℃下搅拌10min;
(3)加入0.05g/mL葡萄糖溶液24mL进行反应,反应1h后混合液变成红褐色;
(4)将混合液冷却至室温,至于磁铁上,5min后全部固体物质被磁铁吸引到容器底部,上部溶液变澄清,倒去上清液后即可回收磁性固体物,将磁性固体物清洗并80℃真空干燥8h,得NiFe2O4/Cu2O 磁性复合纳米催化剂。
对本实施制备的NiFe2O4/Cu2O的XRD的图谱分析如图1所示。对本实施制备的NiFe2O4/Cu2O的SEM分析检测如图2所示,从图2 可看出复合纳米颗粒的大小约10-30nm。对NiFe2O4/Cu2O的紫外可见光谱分析如图3所示。取0.5g NiFe2O4/Cu2O复合纳米催化剂材料,加入到100mL、20mg/L的亚甲蓝溶液中,置于500W的紫外可见灯下进行光催化反应,光源离反应液面距离为20cm。光催化60分钟后其脱色率可以达到98%,如图4所示。
实施例2
一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,其包括以下步骤:
Ⅰ)NiFe2O4的制备:
(1)按铁和镍的摩尔比为2:1.5分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中;
(2)向混合溶液中滴加氢氧化钠溶液调节pH值为10,将混合溶液加热至80℃保温3.5h;
(3)将加热后的溶液转移至反应釜中,将反应釜加热到800℃并保温2.5h;
(4)将加热后获得的粉末固体在磁场中进行分离,然后对磁性粉末洗涤并烘干,得到黑色的NiFe2O4催化剂颗粒,NiFe2O4的直径为20-30nm;
Ⅱ)NiFe2O4/Cu2O磁性复合物的制备:
(1)在35℃下,将3.993g六水合醋酸铜搅拌溶于50ml去离子水中,搅拌15min,并超声处理60min;
(2)加入2.12g制备完成的NiFe2O4催化剂颗粒,搅拌15min,然后加入0.04g/mL的氢氧化钠溶液24mL,50℃下搅拌10min;
(3)加入0.05g/mL葡萄糖溶液24mL进行反应,反应1h后混合液变成红褐色;
(4)将混合液冷却至室温,至于磁铁上,5min后全部固体物质被磁铁吸引到容器底部,上部溶液变澄清,倒去上清液后即可回收磁性固体物,将磁性固体物清洗并80℃真空干燥8h,得NiFe2O4/Cu2O 磁性复合纳米催化剂。
对本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及形变,而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (5)
1.一种NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,其特征在于:包括以下步骤:
Ⅰ)NiFe2O4的制备:
(1)按铁和镍的摩尔比为2:1-1.5分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中;
(2)向混合溶液中滴加碱性溶液调节pH值为10-14,将混合溶液加热至80-100℃保温2.5-3.5h;
(3)将加热后的溶液转移至反应釜中,将反应釜加热到600-800℃并保温2.5-3.5h;
(4)将加热后获得的粉末固体在磁场中进行分离,然后对磁性粉末洗涤并烘干,得到NiFe2O4催化剂颗粒;
Ⅱ)NiFe2O4/Cu2O磁性复合物的制备:
(1)将六水合醋酸铜搅拌溶于去离子水中,并超声处理;
(2)加入制备完成的NiFe2O4催化剂颗粒,NiFe2O4与醋酸铜的质量比为2-2.15:4.05,然后加入碱性溶液,并进行搅拌;
(3)加入葡萄糖溶液进行反应,混合液变成红褐色;
(4)将混合液冷却,使用磁铁磁吸固体物,清洗并干燥,得NiFe2O4/Cu2O磁性复合纳米催化剂。
2.根据权利要求1所述的NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,其特征在于:NiFe2O4催化剂颗粒的粒径为20-30nm,NiFe2O4/Cu2O磁性复合纳米催化剂的粒径为10-30nm。
3.根据权利要求1所述的NiFe2O4/Cu2O磁性复合纳米催化剂的制备方法,其特征在于:NiFe2O4/Cu2O磁性复合纳米催化剂的比表面积为78.89m2/g。
4.NiFe2O4/Cu2O磁性复合纳米催化剂在处理染料废水有机污染物中的应用。
5.根据权利要求4所述的NiFe2O4/Cu2O磁性复合纳米催化剂在处理染料废水有机污染物中的应用,其特征在于:所述磁性复合纳米催化剂对亚甲基蓝有机溶液的光催化降解效率达到98%以上。
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101789298A (zh) * | 2010-03-17 | 2010-07-28 | 上海大学 | 一种Cu2O/NiFe2O4磁性复合物的制备方法 |
-
2017
- 2017-04-27 CN CN201710285336.0A patent/CN107008331A/zh active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101789298A (zh) * | 2010-03-17 | 2010-07-28 | 上海大学 | 一种Cu2O/NiFe2O4磁性复合物的制备方法 |
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