CN105964281A - 一种片状碱式氯化铜催化剂的制备方法及用途 - Google Patents
一种片状碱式氯化铜催化剂的制备方法及用途 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 title claims abstract description 10
- 239000003513 alkali Substances 0.000 title abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 16
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 8
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 8
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- SKQUUKNCBWILCD-UHFFFAOYSA-J dicopper;chloride;trihydroxide Chemical compound [OH-].[OH-].[OH-].[Cl-].[Cu+2].[Cu+2] SKQUUKNCBWILCD-UHFFFAOYSA-J 0.000 claims description 35
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000011534 incubation Methods 0.000 claims description 7
- 239000000975 dye Substances 0.000 claims description 6
- 239000000356 contaminant Substances 0.000 claims description 3
- 230000000593 degrading effect Effects 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims 3
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- 239000008187 granular material Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 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 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012028 Fenton's reagent Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000009279 wet oxidation reaction Methods 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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- B01J27/06—Halogens; Compounds thereof
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- B01J27/122—Halides of copper
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Abstract
本发明公开了一种片状碱式氯化铜催化剂的制备方法及用途,该制备方法包括以下步骤:室温下,向水中加入氢氧化钠,搅拌溶解,氢氧化钠浓度为0.2mol/L‑0.28mol/L;向氢氧化钠水溶液中加入氯化铜,室温下搅拌溶解制成混合溶液,其中,铜离子水溶液浓度为0.16mol/L‑0.24mol/L;继续向上述混合溶液中加入氟化钠,室温下搅拌溶解;将得到的混合溶液加入到聚四氟乙烯内衬中,80℃‑120℃恒温水热反应15‑30小时,离心、洗涤、干燥后即得。本发明制备方法简单,制备的碱式氯化铜颗粒为规则的片状形貌,结构新颖,而且对芬顿反应具有较高的催化性能。
Description
技术领域
本发明涉及催化剂制备技术领域,具体涉及一种片状碱式氯化铜催化剂的制备方法及用途。
背景技术
工业废水中染料废水的排放量大而难降解,一直是废水处理的难点,湿法氧化是处理此类难降解染料废水的重要方法之一。1893年,化学家Fenton发现,过氧化氢(H2O2)与二价铁离子的混合溶液具有强氧化性,可以将羧酸、醇、酯类等有机化合物氧化为无机态,氧化效果十分显著,但此后半个多世纪中,这种氧化性试剂却因为氧化性极强没有被太多重视。进入20世纪70年代,芬顿试剂在环境化学中找到了它的位置,具有高效去除难降解有机污染物能力的芬顿试剂,在印染废水、含油废水、含酚废水、焦化废水、含硝基苯废水、二苯胺废水等废水处理中得到了广泛的应用。
与传统的环境净化方法相比,半导体光催化技术拥有反应条件温和、无二次污染、操作简单和降解效果显著等优势。含铜盐化合物中,碱式氯化铜作为一种功能材料,有着广泛的用途。目前,已报道的公开号分别为CN102730743A和CN103214021A的发明专利公开了制备碱式氯化铜的相关工艺,但是由上述方法合成的碱式氯化铜颗粒形貌不规则、尺寸较大。
发明内容
本发明所要解决的技术问题是克服现有技术的不足,提供一种片状碱式氯化铜催化剂的制备方法及用途,制备的碱式氯化铜颗粒为规则的片状形貌,结构新颖,制备方法简单,而且对芬顿反应具有较高的催化性能。
为解决以上技术问题,本发明采取如下技术方案:
一种片状碱式氯化铜催化剂的制备方法,包括以下步骤:
(1)室温下,向水中加入氢氧化钠,搅拌溶解,氢氧化钠浓度为0.2mol/L-0.28mol/L;
(2)向氢氧化钠水溶液中加入氯化铜,室温下搅拌溶解制成混合溶液,其中,铜离子水溶液浓度为0.16mol/L-0.24mol/L;
(3)继续向上述混合溶液中加入氟化钠,室温下搅拌溶解;
(4)将步骤(3)得到的混合溶液加入到聚四氟乙烯内衬中,80℃-120℃恒温水热反应15-30小时,离心、洗涤、干燥后即得片状碱式氯化铜催化剂。
优选地,步骤(3)中氟化钠浓度为0.48mol/L-0.64mol/L。
优选地,步骤(4)中恒温水热温度为100℃。
优选地,步骤(4)中干燥温度为60℃。
采用上述制备方法制备的片状碱式氯化铜催化剂应用于降解环境染料污染物。
由于以上技术方案的实施,本发明与现有技术相比具有如下优点:
1、本发明制备的碱式氯化铜颗粒为规则的片状形貌,为六边形,结构新颖;
2、本发明制备的碱式氯化铜颗粒比表面积达到5.3m2/g,对芬顿反应具有较高的催化性能,应用于催化芬顿反应高效降解环境染料污染物方面;
3、本发明制备方法简单,可以广泛推广应用。
附图说明
图1为实施例1制备的片状碱式氯化铜催化剂的扫描电子显微镜(SEM)图;
图2为实施例1制备的片状碱式氯化铜催化剂的X射线衍射(XRD)图;
图3为实施例1制备的片状碱式氯化铜催化剂在降解含有罗丹明B染料水溶液的活性对比图;
其中,C0为罗丹明B的初始浓度,Ct为经过紫外光照射一段时间后测量的罗丹明B浓度,t为时间,曲线a为没有催化剂时的罗丹明B降解情况,曲线b是有催化剂时罗丹明B的光降解情况。
具体实施方式
下面结合附图和具体的实施例对本发明做进一步详细的说明。
实施例1
片状碱式氯化铜催化剂的制备
(1)室温下,取25mL的纯水倒入烧杯中,向水中加入5mmol氢氧化钠,搅拌溶解;
(2)向氢氧化钠水溶液中加入4mmol氯化铜,室温下搅拌溶解制成混合溶液;
(3)继续向上述混合溶液中加入12mmol氟化钠,室温下搅拌10分钟至溶解;
(4)将步骤(3)得到的混合溶液加入到聚四氟乙烯内衬中,在100℃恒温水热反应20小时,蒸馏水离心洗涤3次,在60℃下干燥,即得片状碱式氯化铜催化剂。
由附图1所示,实施例1所制备的碱式氯化铜为均一、规则的六边形,结构新颖。
有附图2所示,与XRD标准卡(JCPDS:86-0899)比较,实施例1制备的产品为纯相的碱式氯化铜。
实施例2
片状碱式氯化铜催化剂的制备
(1)室温下,取25mL的纯水倒入烧杯中,向水中加入6mmol氢氧化钠,搅拌溶解;
(2)向氢氧化钠水溶液中加入5mmol氯化铜,室温下搅拌溶解制成混合溶液;
(3)继续向上述混合溶液中加入14mmol氟化钠,室温下搅拌10分钟至溶解;
(4)将步骤(3)得到的混合溶液加入到聚四氟乙烯内衬中,在80℃恒温水热反应28小时,蒸馏水离心洗涤3次,在60℃下干燥,即得片状碱式氯化铜催化剂。
所制得催化剂组成与实施例1一致,物理性质和催化活性相似。
实施例3
片状碱式氯化铜催化剂的制备
(1)室温下,取25mL的纯水倒入烧杯中,向水中加入7mmol氢氧化钠,搅拌溶解;
(2)向氢氧化钠水溶液中加入6mmol氯化铜,室温下搅拌溶解制成混合溶液;
(3)继续向上述混合溶液中加入16mmol氟化钠,室温下搅拌10分钟至溶解;
(4)将步骤(3)得到的混合溶液加入到聚四氟乙烯内衬中,在120℃恒温 水热反应16小时,蒸馏水离心洗涤3次,在60℃下干燥,即得片状碱式氯化铜催化剂。
所制得催化剂组成与实施例1一致,物理性质和催化活性相似。
将实施例1制备的片状碱式氯化铜催化剂对降解含有罗丹明B染料(RhB)水溶液的活性进行测试。
测试过程:称取实施例1制备的样品0.1g,加入200ml RhB水溶液和2μl过氧化氢(30wt.%),其中RhB浓度为10mg/L,作为测试例,对比例中加入200ml RhB水溶液和2μl过氧化氢(30wt.%),其中RhB浓度为10mg/L。先避光搅拌10min,使染料在催化剂表面达到吸附/脱附平衡,然后开启氙灯光源,在紫外光照射下进行光催化反应,上清液用分光光度计检测。根据Lambert–Beer定律,有机物特征吸收峰强度的变化,可以定量计算其浓度变化,当吸光物质相同、厚度相同时,可以用吸光度的变化直接表示溶液浓度的变化。因为罗丹明B在553nm处有一个特征吸收峰,所以可以利用吸光度的变化来衡量溶液中罗丹明B的浓度变化。
测试结果如附图3所示,横坐标为紫外光照射时间,纵坐标为经过紫外光照射一段时间后测量的RhB浓度值与RhB的初始浓度的比值。从附图3可以看出,光照40min后,片状碱式氯化铜降解RhB高达95%,而未加入片状碱式氯化铜只有57%。由此可见,片状碱式氯化铜催化剂对RhB具有较高的催化活性。
本发明制备方法简单,制备的碱式氯化铜颗粒为规则的片状形貌,结构新颖,而且对芬顿反应具有较高的催化性能。
以上对本发明做了详尽的描述,但本发明不限于上述的实施例。凡根据本发明的精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围内。
Claims (5)
1.一种片状碱式氯化铜催化剂的制备方法,其特征在于:包括以下步骤:
(1)室温下,向水中加入氢氧化钠,搅拌溶解,氢氧化钠浓度为0.2mol/L-0.28mol/L;
(2)向氢氧化钠水溶液中加入氯化铜,室温下搅拌溶解制成混合溶液,其中,铜离子水溶液浓度为0.16mol/L-0.24mol/L;
(3)继续向上述混合溶液中加入氟化钠,室温下搅拌溶解;
(4)将步骤(3)得到的混合溶液加入到聚四氟乙烯内衬中,80℃-120℃恒温水热反应15-30小时,离心、洗涤、干燥后即得片状碱式氯化铜催化剂。
2.根据权要求1所述的片状碱式氯化铜催化剂的制备方法,其特征在于:所述步骤(3)中氟化钠浓度为0.48mol/L-0.64mol/L。
3.根据权要求1所述的片状碱式氯化铜催化剂的制备方法,其特征在于:所述步骤(4)中恒温水热温度为100℃。
4.根据权要求1所述的片状碱式氯化铜催化剂的制备方法,其特征在于:所述步骤(4)中干燥温度为60℃。
5.根据权利要求1-4中任一项权利要求所述的片状碱式氯化铜催化剂的制备方法制备的片状碱式氯化铜催化剂应用于降解环境染料污染物。
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