CN106902760A - 一种蛋壳负载氧化锌材料及其制备方法和应用 - Google Patents
一种蛋壳负载氧化锌材料及其制备方法和应用 Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 210000003278 egg shell Anatomy 0.000 title claims abstract description 74
- 102000002322 Egg Proteins Human genes 0.000 title claims abstract description 71
- 108010000912 Egg Proteins Proteins 0.000 title claims abstract description 71
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 50
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000003911 water pollution Methods 0.000 claims abstract description 15
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000007146 photocatalysis Methods 0.000 claims abstract description 8
- 239000007822 coupling agent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- -1 titanate ester Chemical class 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 150000004756 silanes Chemical class 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 2
- 239000002585 base Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 239000005416 organic matter Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 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 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 229940012466 egg shell membrane Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 241000276489 Merlangius merlangus Species 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
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- 230000004083 survival effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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Abstract
本发明涉及一种蛋壳负载氧化锌材料及其制备方法和应用，属于吸附有机物和光催化分解有机物的处理水污染技术领域。所述材料是以包含蛋膜的蛋壳为载体，首先将洗净的蛋壳放入偶联剂中浸泡，取出放入锌离子溶液中，缓慢滴加与所述锌离子溶液摩尔比为1：2的碱溶液，滴加完毕后，搅拌1～2小时，最后用微波加热法制得蛋壳负载氧化锌材料。此发明的优点在于利用氧化锌的光催化效应同时结合蛋膜的吸附性处理水体污染，工艺简单、处理效果好、易回收、成本低。
Description
技术领域
本发明涉及一种蛋壳负载氧化锌材料及其制备方法和应用，属于吸附有机物和光催化分解有机物处理水污染技术领域。
背景技术
生活污水和工业废水的排放造成了严重的水污染，加剧了水源匮乏。因此，大力开展污水处理工作，构建良好的生态环境，加强水污染的治理，加强生态环境的保护，既是满足人民群众生存发展的当前需要，也是实现未来可持续发展的关键。
水污染处理方法众多，但存在成本高、效果不明显、技术难度大、二次污染等问题。纳米氧化锌作为一种性能优异的光催化剂，其禁带宽度与纳米氧化钛相近，而且制备操作简单、价格低廉，在光催化领域越来越引起重视。在紫外光的照射下，纳米氧化锌吸收高能量光能，价带电子被激发发生跃迁，即从价带跃迁到导带，从而产生光生电子和空穴，此时吸附在氧化锌颗粒表面的溶解氧俘获电子形成超氧负离子，空穴可以使水分子活化成氧化能力极强的氢氧自由基，从而诱使发生光化学反应，产生光催化效应，氧化分解有机物。
但是用于污水处理的氧化锌光催化材料存在沉降性能差、难与水分离和可再生性差等缺点。例如专利CN 101352676A公开了“以贝壳粉为载体的纳米氧化锌的制备方法”，将氧化锌通过浸渍法负载到贝壳粉载体上，该发明不仅降低了纳米氧化锌的生产成本，而且有利于处理水污染问题，但是应用中将粉体直接投放水源中，由于颗粒小，回收困难，易造成二次污染。专利CN 106000380A公开了“活性炭负载纳米氧化锌臭氧氧化催化剂及其制备和使用”，该发明在活化和吸附协同作用下，处理水污染，但是依然存在回收困难，易造成二次污染问题。专利CN 101590401A公开了“一种水玻璃负载羟基氧化锌的制备方法”该发明得到的水玻璃负载羟基氧化锌颗粒致密且粒径分布均匀，水玻璃负载羟基氧化锌具有在水中易于分散，具有良好的沉降性能，可以提高臭氧利用率，但是本发明实验过程中对pH值需要进行严格的调控，并且该发明最终为粉体状材料不利于回收。
中国是禽蛋生产和消费大国，每年会产生大量废弃蛋壳。蛋壳往往被当作废弃物处理，不能得到回收和利用，蛋壳中残留的蛋液会很快腐败变质，污染环境。 蛋壳外表为碳酸钙，易于氧化锌复合，能提高氧化锌的稳定性；蛋壳中蛋膜具有较好的透水透气性、较高的稳定性及生物相容性，是一种优异的污染物吸附材料。因此，本发明可获得一种蛋壳负载氧化锌材料，既可利用蛋壳中蛋膜吸附水污染，又可利用蛋壳上负载的氧化锌光催化处理水污染，具有工艺简单、处理效果好、易回收、成本低、避免二次污染等优势。
发明内容
本发明的目的之一在于针对废弃蛋壳利用率低，污染环境问题，将蛋壳作为氧化锌的载体，蛋壳被有效利用，可实现以废治废；
本发明的目的之二在于解决氧化锌应用的难题，将氧化锌负载于蛋壳，可有效发挥氧化锌光催化性能和蛋壳中蛋膜的吸附性。氧化锌利用太阳光处理水污染，不需额外能源，节能环保；蛋壳中蛋膜可以吸附水体中污染，是一条处理水污染的新途径。
为了解决上述技术问题，本发明提出的技术方案是：一种蛋壳负载氧化锌材料，其特征在于：所述的氧化锌为纤锌矿结构，负载基体为蛋壳，所述蛋壳为去除蛋液以外的部分。
优选的，所述氧化锌均匀的负载在蛋壳基体上。
优选的，具体步骤如下：
(1)用去离子水超声清洗蛋壳，浸泡1～2小时；
(2)将步骤(1)得到的蛋壳放入浓度为0.5％～2％的偶联剂中浸泡4～6小时；
(3)将步骤(2)得到的蛋壳放入0.05～0.2mol/L锌离子溶液；
(4)按锌离子溶液和碱溶液摩尔比为1:2，在步骤(2)中缓慢滴加0.5～1.0mol/L的碱溶液，滴加完毕后，搅拌1～2小时；
(5)将步骤(4)得到的反应体系微波加热20～60分钟，自然冷却至室温，清洗，干燥即得蛋壳负载氧化锌材料。
优选的，所述偶联剂为硅烷类或钛酸酯类中的一种或多种。
优选的，所述锌离子溶液为乙酸锌、硝酸锌、氯化锌中的一种或多种。
为了解决上述技术问题，本发明提出的另一技术方案是：所述的蛋壳负载氧化锌材料的应用，用蛋壳中蛋膜吸附性和蛋壳上负载氧化锌的光催化性能处理水污染。
本发明的有益效果：
本发明采用的微波加热法加热均匀，较水热法温度低，不破坏蛋壳结构，利于氧化锌的制备以及在蛋壳表面负载。
本发明实现了同步进行氧化锌的制备和氧化锌的负载。
本发明将氧化锌负载于废弃的蛋壳，制备工艺简单、易回收、节能环保，不仅可以利用氧化锌的光催化性能处理水体污染，还能利用蛋壳中蛋膜的吸附性吸附污染水体中有机物和重金属离子。
本发明将蛋壳作氧化锌的载体，能稳定氧化锌，避免氧化锌流失，便于回收再利用，避免二次污染。
附图说明
下面结合附图对本发明的作进一步说明。
图1为蛋壳负载氧化锌材料的表面XRD图谱。
图2为蛋壳负载氧化锌材料中蛋壳膜外表面SEM照片。
图3为紫外光下不同样品降解罗丹明B的降解曲线图。
具体实施方式
实施例1
取3g蛋壳，用去离子水超声清洗并浸泡1小时，然后将洗净的蛋壳放入50mL浓度为0.5％的硅烷偶联剂(KH550)中浸泡4小时，再放入50mL、0.1mol/L的乙酸锌溶液，并缓慢滴加10mL、1mol/L的氢氧化钠溶液，滴加完毕后，搅拌2小时，微波加热30分钟，自然冷却至室温，清洗，干燥即得目标产物。用X射线衍射仪(XRD)表征样品，如图1所示，在2θ为31.65°、34.44°和36.24°处出现3个强峰，分别对应氧化锌的(100)、(002)、(101)晶面，分析可知氧化锌成功负载于蛋壳。
实施例2
取3g蛋壳，用去离子水超声清洗并浸泡1小时，然后将洗净的蛋壳放入50mL浓度为1.0％的钛酸酯偶联剂中浸泡5小时，再放入50mL、0.1mol/L的硝酸锌溶液，并缓慢滴加10mL、1mol/L的氨水，滴加完毕后，搅拌1小时，微波加热50分钟，自然冷却至室温，清洗，干燥即得目标产物。用扫描电子显微镜(SEM)表征样品，如图2所示，蛋壳膜呈纤维网络交织状，氧化锌颗粒均匀、紧密负载在蛋壳膜上，氧化锌颗粒呈椭球状。
实施例3
取3g蛋壳，用去离子水超声清洗并浸泡1小时，然后将洗净的蛋壳放入50mL浓度为1％的硅烷偶联剂(KH560)中浸泡6小时，再放入50mL、0.1mol/L的氯化锌溶液，并缓慢滴加10mL、1mol/L的氢氧化钠溶液，滴加完毕后，搅拌2小时，微波加热1小时，自然冷却至室温，清洗，干燥即得目标产物。用50mL的罗丹明B(12mg/L)做污染液，与空白样品进行对比，测试蛋壳(ES)吸附污染物的能力，测试蛋壳负载氧化锌材料(ES-ZnO)在紫外光照射下对污染物的降解能力，结果如图3所示，从图中可以看出溶液中罗丹明B的浓度随着时间的延长逐渐降低；加入蛋壳后，蛋壳中蛋膜具有强烈的吸附作用，罗丹明B的浓度明显降低；蛋壳负载氧化锌材料在紫外的照射下，污染物降低的速度最快，这主要由于蛋壳中蛋膜的吸附作用，还有氧化锌的催化作用，两者协同作用，能有效处理水中污染物。
本发明的不局限于上述实施例所述的具体技术方案，凡采用等同替换形成的技术方案均为本发明要求的保护范围。
Claims (7)
1.一种蛋壳负载氧化锌材料，其特征在于：所述的氧化锌为纤锌矿结构，负载基体为蛋壳，所述蛋壳为去除蛋液以外的部分。
2.根据权利要求1所述蛋壳负载氧化锌材料，其特征在于：所述氧化锌均匀的负载在蛋壳基体上。
3.根据权利要求1所述蛋壳负载氧化锌材料，其特征在于：所述蛋壳负载氧化锌材料按如下制备方法制备而得：
(1)用去离子水超声清洗蛋壳，浸泡1～2小时；
(2)将步骤(1)得到的蛋壳放入浓度为0.5％～2％的偶联剂中浸泡4～6小时；
(3)将步骤(2)得到的蛋壳放入0.05～0.2mol/L锌离子溶液；
(4)按锌离子溶液和碱溶液摩尔比为1:2，在步骤(2)中缓慢滴加0.5～1.0mol/L的碱溶液，滴加完毕后，搅拌1～2小时；
(5)将步骤(4)得到的反应体系微波加热20～60分钟，自然冷却至室温，清洗，干燥即得蛋壳负载氧化锌材料。
4.根据权利要求1所述蛋壳负载氧化锌材料的制备方法，其特征在于：具体步骤如下：
(1)用去离子水超声清洗蛋壳，浸泡1～2小时；
(2)将步骤(1)得到的蛋壳放入浓度为0.5％～2％的偶联剂中浸泡4～6小时；
(3)将步骤(2)得到的蛋壳放入0.05～0.2mol/L锌离子溶液；
(4)按锌离子溶液和碱溶液摩尔比为1:2，在步骤(2)中缓慢滴加0.5～1.0mol/L的碱溶液，滴加完毕后，搅拌1～2小时；
(5)将步骤(4)得到的反应体系微波加热20～60分钟，自然冷却至室温，清洗，干燥即得蛋壳负载氧化锌材料。
5.根据权利要求4所述的蛋壳负载氧化锌材料的制备方法，其特征在于：所述偶联剂为硅烷类或钛酸酯类中的一种或多种。
6.根据权利要求4所述的蛋壳负载氧化锌材料的制备方法，其特征在于：所述锌离子溶液为乙酸锌、硝酸锌、氯化锌中的一种或多种。
7.根据权利要求1～3任一所述的蛋壳负载氧化锌材料的应用，其特征在于：用蛋壳中蛋膜吸附性和蛋壳上负载氧化锌的光催化性能处理水污染。
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