CN107970965B - 碳氮烯/碳酸银复合纳米材料、其制备方法及其应用 - Google Patents
碳氮烯/碳酸银复合纳米材料、其制备方法及其应用 Download PDFInfo
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- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910001958 silver carbonate Inorganic materials 0.000 title claims abstract description 28
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title description 7
- 229910052799 carbon Inorganic materials 0.000 title description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- KQTXIZHBFFWWFW-UHFFFAOYSA-L silver(I) carbonate Inorganic materials [Ag]OC(=O)O[Ag] KQTXIZHBFFWWFW-UHFFFAOYSA-L 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
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- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
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- 239000004202 carbamide Substances 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 239000002135 nanosheet Substances 0.000 claims abstract description 6
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 5
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- WIKQEUJFZPCFNJ-UHFFFAOYSA-N carbonic acid;silver Chemical compound [Ag].[Ag].OC(O)=O WIKQEUJFZPCFNJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000011736 potassium bicarbonate Substances 0.000 claims description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 3
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- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
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- 238000003786 synthesis reaction Methods 0.000 claims description 2
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- 229910001316 Ag alloy Inorganic materials 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
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- 230000015556 catabolic process Effects 0.000 abstract description 4
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 7
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- 238000001228 spectrum Methods 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical group [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
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- 230000035945 sensitivity Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
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- 239000003403 water pollutant Substances 0.000 description 1
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Abstract
本发明公开了碳氮烯/碳酸银复合纳米材料、其制备方法及其应用，复合纳米材料中，g‑C3N4占1wt％～10wt％，余量为Ag2CO3,且Ag2CO3微米棒附着在片层g‑C3N4的表面。制备方法是：将尿素与三聚氰胺在管式炉内固相烧结制得g‑C3N4纳米片；在搅拌及超声波的条件下，将g‑C3N4纳米片分散到去离子水中，再加入可溶性的银盐和沉淀剂，室温发生溶液沉淀反应，清洗、干燥，得到反应产物，可应用于有机废水处理、空气中有机污染物的降解。g‑C3N4的加入能有效提高光催化降解有机物的能力。
Description
技术领域
本发明涉及纳米材料领域，具体地，是一种碳氮烯/碳酸银复合纳米材料、其制备方法及其用作光催化剂的用途。
背景技术
Ag2CO3半导体光催化剂对RhB、MO和MB等多种染料都具有高效的可见光催化活性，但是其光催化稳定性还不够理想。因此，需要在不影响其光催化活性的同时提高其稳定性。最近，类石墨结构的氮化碳(g-C3N4)半导体光催化剂由于其稳定性、无毒性且带隙能只有2.7eV引起人们的广泛关注。g-C3N4是一种非金属半导体光催化剂，它可以应用于分解水和有机污染物。近期大量的g-C3N4半导体光催化剂与银基的复合材料被报道，如g-C3N4/Ag3VO4，g-C3N4/Ag3PO4，g-C3N4/Ag2O等,同时这些g-C3N4修饰的银基半导体复合材料都表现出较高的光催化活性和稳定性。
发明内容
针对现有技术的不足，本发明的目的在于提供碳氮烯/碳酸银复合纳米材料、其制备方法及其应用，成本低廉、工艺简单、产率高、光催化效率高。
上述发明目的是通过如下技术方案实现的：
一种碳氮烯/碳酸银(g-C3N4/Ag2CO3)复合纳米材料，Ag2CO3微米棒附着在片层g-C3N4的表面，其主要成份g-C3N4的质量百分含量为1％～10％，余量为Ag2CO3。
较佳地，g-C3N4的质量百分含量为2％～6％。，余量为Ag2CO3，因为在该g-C3N4范围的复合纳米材料有更好的催化效果。
一种碳氮烯/碳酸银(g-C3N4/Ag2CO3)复合纳米材料的制备方法，包括如下步骤：
步骤(1)、片层结构的g-C3N4纳米片的合成：将尿素与三聚氰胺的混合物置于石英坩埚内，在管式炉内固相烧结制得g-C3N4片状结构；
尿素与三聚氰胺的混合物，其摩尔比为1：0.5-1:6，优选1:1；
固相烧结的温度400℃～650℃，保温时间为0.5～4h；优选为580℃反应1h，升温速率为5/min。
步骤(2)、碳氮烯/碳酸银复合光催化剂的合成：在搅拌及超声波的条件下，将步骤(1)制备所得g-C3N4纳米片分散到去离子水中，再将可溶性的银盐和碳酸盐或碳酸氢盐加入上述反应液，然后在室温条件下，发生溶液沉淀反应，用去离子水与无水乙醇反复清洗产物，干燥后得到反应产物。
所述银盐为AgNO3；
可溶性碳酸盐为Na2CO3·10H2O或K2CO3；
碳酸氢盐为NaHCO3、KHCO3或(NH4)2CO3；
碳氮烯/碳酸银复合纳米材料，作为光纳米催化剂，应用于有机废水处理、空气中有机污染物的降解。
本发明方法的成本价廉，生产工艺简单易控，产物差率高，适合大规模的工业生产。
本发明合成高光催化性能碳氮烯/碳酸银复合材料，g-C3N4的加入能有效提高光催化降解有机物的能力，其效率提升20％，同时降解速度提升30％-50％，其在光催化、气敏、污水处理等领域中具有重要的应用，有望用于大规模的工业生产。
附图说明
图1为本发明制得的纯Ag2CO3、纯g-C3N4和碳氮烯/碳酸银复合光催化剂的XRD图谱。从图中可以看出，纯Ag2CO3的衍射峰与标准卡片(JCPDS NO.70-2184)单斜Ag2CO3的衍射峰相一致，且具有良好的结晶性能。纯g-C3N4在2θ角度27.4°出现一个强特征峰，对应六方相g-C3N4的(002)晶面(JCPDS NO.87-1526)。在碳氮烯/碳酸银复合光催化剂XRD图谱中，Ag2CO3特征衍射峰的位置没有发生变化。当g-C3N4的质量比为2％时(碳氮烯/碳酸银-1)，我们并没有发现g-C3N4的特征衍射峰，可能是含量太低超出了XRD检测极限，而当继续增加g-C3N4的质量，在碳氮烯/碳酸银-2和碳氮烯/碳酸银-3都观察到g-C3N4的特征峰，证明制备的样品是碳氮烯/碳酸银复合光催化剂。另外，从碳氮烯/碳酸银复合光催化剂的XRD图谱中并没有观察到其他杂峰，说明制备得到的样品有较高的纯度。
图2为本发明制得的g-C3N4、Ag2CO3和不同含量的碳氮烯/碳酸银光催化剂的红外图谱。从纯Ag2CO3的红外谱图可以看出，3440cm-1周围出现了较宽的吸收峰，对应样品表面羟基的特征伸缩振动峰，1449cm-1、1382cm-1、883cm-1和705cm-1吸收峰则为碳酸盐的拉伸振动峰。从g-C3N4的FT-IR谱图可看出，800cm-1处的吸收峰是组成g-C3N4单元的碳氮环的弯曲振动特征峰；1250cm-1、1560cm-1和1630cm-1为g-C3N4碳氮杂环上的C＝N、C-N和环外C-N伸缩振动特征峰；而在3000-3500cm-1的吸收带则是其表面吸附水分子的伸缩振动峰。仔细观察碳氮烯/碳酸银复合光催化剂样品的红外光谱图，从图中可以同时看出g-C3N4和Ag2CO3的特征吸收峰，这一结果说明实验成功制备出碳氮烯/碳酸银复合光催化剂，也进一步验证了XRD的结果。
图3为纯Ag2CO3和碳氮烯/碳酸银复合光催化剂的SEM图谱。由图3(a)可得，Ag2CO3是由一些短棒构成，其表面光滑且具有较好的分散性。随着g-C3N4的加入，与Ag2CO3形成复合光催化剂，整体的尺寸、形貌发生了明显的改变(图3(b-d)分别对应碳氮烯/碳酸银-1、2、3)，类石墨结构的氮化碳呈现片层结构，Ag2CO3微米棒附着在片层g-C3N4的表面，且随着g-C3N4量的增加，片层g-C3N4包覆着Ag2CO3微米棒开始出现。
图4为本发明制得的纯Ag2CO3和碳氮烯/碳酸银复合光催化剂性能考核曲线：(a)降解RhB曲线和(b)动力学曲线。如图所示，相较于纯Ag2CO3(40min)，碳氮烯/碳酸银-1、碳氮烯/碳酸银-2和碳氮烯/碳酸银-3复合光催化剂的光催化活性都有显著提高，分别能够在25min、15min和20min将RhB染料降解完全。同样地，实验采用准一级反应动力学模型ln(Ct/C)＝-kt求解一级反应速率常数来考察碳氮烯/碳酸银复合光催化剂降解RhB的动力学曲线。由图4(b)可知，纯Ag2CO3、碳氮烯/碳酸银-1、碳氮烯/碳酸银-2和碳氮烯/碳酸银-3复合光催化剂的一级反应速率常数分别为0.072min-1、0.113min-1、0.193min-1以及0.131min-1，其中碳氮烯/碳酸银-2的k值是最大的，是纯Ag2CO3的2.68倍。
具体实施方式
以下通过具体实施方式进一步描述本发明，由技术常识可知，本发明也可通过其它的不脱离本发明技术特征的方案来描述，因此所有在本发明范围内或等同本发明范围内的改变均被本发明包含。本发明所涉及的试剂均为商业产品，不需要再制备。
实施例1：
步骤(1)、称取10g尿素与三聚氰胺混合物(摩尔比1:1)加入坩埚中，接着再马弗炉中以580℃焙烧1h，升温速率为5/min。将合成的黄色粉末用去离子水和无水乙醇反复洗涤数次，最后在真空条件下60℃干燥12h得到g-C3N4片层结构；
步骤(2)、室温条件下，将2mg(1)所制备的g-C3N4溶解在20mL去离子水中超声分散至少1h，然后将2mmol AgNO3分散在20mL去离子水中，充分溶解后将其逐步滴加到上述g-C3N4溶液中搅拌充分，最后将20mL Na2CO3·10H2O(0.05M)溶液逐滴滴加到上述溶液中并充分搅拌1h后用去离子水和乙醇多次洗涤离心，60℃烘干，得2％-碳氮烯/碳酸银样品，定义为碳氮烯/碳酸银-1。
实施例2：
步骤(1)、将称取的10g尿素与三聚氰胺混合物(摩尔比1:0.5)加入坩埚中，接着再马弗炉中以400℃焙烧4h，升温速率为5/min。将合成的黄色粉末用去离子水和无水乙醇反复洗涤数次，最后在真空条件下60℃干燥12h得到g-C3N4片层结构；
步骤(2)、室温条件下，将4mg(1)所制备的g-C3N4溶解在20mL去离子水中超声分散至少1h，然后将2mmol AgNO3分散在20mL去离子水中，充分溶解后将其逐步滴加到上述g-C3N4溶液中搅拌充分，最后将20mL NaHCO3(0.05M)溶液逐滴滴加到上述溶液中并充分搅拌1h后用去离子水和乙醇多次洗涤离心，60℃烘干，得4％-碳氮烯/碳酸银样品，定义为碳氮烯/碳酸银-2。
实施例3：
步骤(1)、将称取的10g尿素与三聚氰胺混合物(摩尔比1:6)加入坩埚中，接着再马弗炉中以650℃焙烧0.5h，升温速率为5/min。将合成的黄色粉末用去离子水和无水乙醇反复洗涤数次，最后在真空条件下60℃干燥12h得到g-C3N4片层结构；
步骤(2)、室温条件下，将6mg(1)所制备的g-C3N4溶解在20mL去离子水中超声分散至少1h，然后将2mmol AgNO3分散在20mL去离子水中，充分溶解后将其逐步滴加到上述g-C3N4溶液中搅拌充分，最后将20mL K2CO3(0.05M)溶液逐滴滴加到上述溶液中并充分搅拌1h后用去离子水和乙醇多次洗涤离心，60℃烘干，得6％-碳氮烯/碳酸银样品，定义为碳氮烯/碳酸银-3。
实施例4：
与实施例1不同之处在于：步骤(2)所用沉淀剂为KHCO3。
实施例5：
与实施例1不同之处在于：步骤(2)所用沉淀剂为(NH4)2CO3。发明人还制备了主要成份g-C3N4的质量百分含量为1％、10％的样品。
Claims (3)
1.碳氮烯/碳酸银复合纳米材料的制备方法，碳氮烯/碳酸银复合纳米材料的Ag2CO3微米棒附着在片层g-C3N4的表面，主要成份g-C3N4的质量百分含量为2%～6%，余量为Ag2CO3；其特征在于，包括如下步骤：
步骤（1）、片层结构的g-C3N4纳米片的合成：将尿素与三聚氰胺的混合物置于石英坩埚内，在管式炉内400℃～650℃固相烧结0.5～4 h制得g-C3N4片状结构；尿素与三聚氰胺的摩尔比为1：0.5-1:6；
步骤（2）、碳氮烯/碳酸银复合光催化剂的合成：在搅拌及超声波的条件下，将步骤（1）制备所得g-C3N4纳米片分散到去离子水中，再将可溶性的银盐和碳酸盐或碳酸氢盐加入反应液，然后在室温条件下，发生溶液沉淀反应，用去离子水与无水乙醇反复清洗产物，干燥后得到反应产物；
所述银盐为AgNO3；可溶性碳酸盐为Na2CO3•10H2O或K2CO3；碳酸氢盐为NaHCO3、KHCO3或(NH4)2CO3。
2.根据权利要求1所述的碳氮烯/碳酸银复合纳米材料的制备方法，其特征在于步骤（1）中，尿素与三聚氰胺的摩尔比为1:1。
3.根据权利要求1所述的碳氮烯/碳酸银复合纳米材料的制备方法，其特征在于步骤（1）中固相烧结的温度580℃，反应时间为1h。
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