CN110075869A - 一种重金属污染废水处理的油茶果壳制备光催化剂的方法 - Google Patents
一种重金属污染废水处理的油茶果壳制备光催化剂的方法 Download PDFInfo
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 58
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- 239000002351 wastewater Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 19
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- 240000001548 Camellia japonica Species 0.000 title claims description 36
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- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 16
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
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- IHYNKGRWCDKNEG-UHFFFAOYSA-N n-(4-bromophenyl)-2,6-dihydroxybenzamide Chemical compound OC1=CC=CC(O)=C1C(=O)NC1=CC=C(Br)C=C1 IHYNKGRWCDKNEG-UHFFFAOYSA-N 0.000 claims description 8
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
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- 239000008367 deionised water Substances 0.000 claims description 2
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- VPQBLCVGUWPDHV-UHFFFAOYSA-N sodium selenide Chemical compound [Na+].[Na+].[Se-2] VPQBLCVGUWPDHV-UHFFFAOYSA-N 0.000 claims description 2
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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 description 40
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- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 4
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 4
- -1 and electrolysis Substances 0.000 description 3
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- PLZFHNWCKKPCMI-UHFFFAOYSA-N cadmium copper Chemical compound [Cu].[Cd] PLZFHNWCKKPCMI-UHFFFAOYSA-N 0.000 description 1
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- LKDOLJJHAKAFGK-UHFFFAOYSA-N copper cadmium(2+) disulfide Chemical compound [S-2].[Cd+2].[Cu+2].[S-2] LKDOLJJHAKAFGK-UHFFFAOYSA-N 0.000 description 1
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- UQMZPFKLYHOJDL-UHFFFAOYSA-N zinc;cadmium(2+);disulfide Chemical compound [S-2].[S-2].[Zn+2].[Cd+2] UQMZPFKLYHOJDL-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种重金属污染废水处理的油茶果壳制备光催化剂的方法。该方法包括以下步骤:将油茶果壳活化、碳化、粉碎、过筛制得茶壳吸附材料;将茶壳吸附材料置于废水中净化重金属污染废水;将吸附重金属离子的茶壳吸附材料与含硫、含硒试剂反应得到具有光催化性能的金属硫化物和金属硒化物,再进行水热合成,制得碳基光催化剂。该光催化剂能够在光照下加速有机化合物的降解。本发明提供了一种净化重金属污染废水并回收利用重金属吸附材料制备碳基光催化剂的新方法,充分实现废弃资源的再利用,经济环保。
Description
技术领域
本发明属于环保领域,涉及污染废水处理,尤其涉及一种重金属污染废水处理的油茶果壳制备光催化剂的方法。
背景技术
随着工业化的快速发展,水污染问题日益加剧,其中,水体重金属污染成为水体污染的突出问题。重金属废水主要来自矿山坑内排水、选矿厂尾矿排水、废石场淋浸水、有色金属冶炼厂除尘排水、有色金属加工厂酸洗水、电镀厂镀件洗涤水,以及电解、农药、医药、油漆、颜料等工业废水,其中包含大量镉、铅、铬、铜、锌等重金属。废水重金属污染对环境的危害非常之大,同时危及人体健康。
在重金属污染水处理方法中,采用吸附材料将离子态重金属吸附固定来去除废水重金属的方法较为经济环保,但是重金属吸附材料吸附污染废水中的重金属离子后,若随意弃置,又会成为新的污染源。目前的处理方法多为焚烧,资源浪费严重,因此开发重金属吸附材料的再利用对于提升资源的价值具有重要意义。
油茶果壳是油茶果加工茶油的副产物,资源十分丰富,油茶果壳中含有大量木质素和纤维素,且具有独特的物理结构,是制备吸附材料的良好原料。将油茶果壳改性,制备成重金属吸附材料,成本较低,但是在吸附重金属后难以解吸和回收再利用。
发明内容
本发明的目的在于克服上述现有技术的缺点和不足,提供一种重金属污染废水处理的油茶果壳制备光催化剂的方法;本发明充分实现废弃资源的再利用,经济环保,不会造成二次污染。
本发明通过下述技术方案实现:
一种重金属污染废水处理的油茶果壳制备光催化剂的方法,包括如下步骤:
步骤一:将油茶果壳与活化剂混合浸渍12~15h后,置于马弗炉中碳化6~8h,待冷却后用水漂洗至pH=7~9,在经过干燥、粉碎、过筛得到茶壳吸附材料;
步骤二:将茶壳吸附材料置于重金属污染废水中,吸附5~7h后,取出用含有茶壳吸附材料(等质量)的水洗3~6次,经过40~80℃烘干,研磨过筛后得到负载重金属离子的茶壳粉末;
步骤三:将负载重金属离子的茶壳粉末与硫磺、硫脲、硒粉、硒脲、硫化钠溶液、硒化钠溶液、硫化氢钠溶液、硒化氢钠溶液中的一种或两种以上混合,加入去离子水搅拌2~5h得到均匀分散液,将分散液倒入反应釜中,170~230℃水热反应12~15h,冷却至室温后用含有茶壳吸附材料(等质量)的水和乙醇依次洗涤2~3次,50~70℃真空干燥8~12h,研磨过筛,得到光催化剂,即碳基光催化剂。
上述步骤一中油茶果壳粉碎过筛是采用目数为100~200目的筛网;
上述步骤二和步骤三中所述研磨过筛是采用目数为200~500目的筛网。
步骤一中活化剂为磷酸、硝酸或过氧化氢中的一种;活化剂与油茶果壳的浸渍比为体积质量比3:1~5:1(mL/g)。
上述步骤一中活化剂与油茶果壳的浸渍比为3:1~5:1。
上述步骤三中负载重金属离子的茶壳粉末与硫磺、硫脲、硒粉、硒脲固体混合,各原料重量份为:负载重金属茶壳粉末45~60份,硫磺、硫脲、硒粉、硒脲固体分别为20~35份;水15~25份。
上述步骤三中负载重金属离子的茶壳粉末与硫化钠溶液、硒化钠溶液、硫化氢钠溶液、硒化氢钠溶液浓度为0.5~5M,各原料重量份为:负载重金属茶壳粉末20~35份,硫化钠溶液、硒化钠溶液、硫化氢钠溶液、硒化氢钠溶液30~45份。
上述步骤二中重金属污染废水中的重金属为镉、铬、铜、锌、镍中的一种或几种。
上述所述光催化剂能够在光照下加速有机化合物的降解。
本发明相对于现有技术,具有如下的优点及效果:
油茶果壳是一种环境友好的天然物质,且资源丰富。
本发明将油茶果壳碳化制成吸附材料吸附废水中的重金属离子后,与含硫、含硒试剂反应得到具有光催化性能的金属硫化物和金属硒化物,再进行水热反应,制得碳基光催化剂。
本发明充分利用了油茶果壳的结构和组成优势,形成了具有稳定优异光催化性能的碳基金属硫化物和金属硒化物,同时达到了废水净化、油茶果壳和重金属回收利用的目的。
具体实施方式
下面结合具体实施例对本发明作进一步具体详细描述。
实施例1
(1)将油茶果壳与磷酸按体积质量比3:1~5:1(mL/g)混合浸渍12h后,置于马弗炉中碳化8h,冷却后用水漂洗至pH=8,干燥、粉碎,过100目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉污染废水中,处理6h后,取出用茶壳吸附材料等质量的水洗4次,在70℃下烘干,研磨过200目筛;
(3)取负载重金属茶壳粉末45重量份,硫磺25重量份,水17重量份,混合搅拌3h得到均匀分散液,将分散液倒入反应釜中,200℃水热反应12h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤2次,60℃真空干燥10h,研磨过200目筛,得到硫化镉/碳(CdS/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硫化镉/碳(CdS/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照3.5h后,亚甲基蓝的降解率达到91%,而不加催化剂的降解率为11%,说明该催化剂催化降解效果明显。
实施例2
(1)将油茶果壳与硝酸按体积质量比3:1~5:1(mL/g)混合浸渍13h后,置于马弗炉中碳化7h,冷却后用水漂洗至pH=7,干燥、粉碎,过150目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉污染废水中,处理7h后,取出,用茶壳吸附材料等质量的水洗5次,在60℃下烘干,研磨过300目筛;
(3)取负载重金属茶壳粉末50重量份,硒粉20重量份,水20重量份,混合搅拌4h得到均匀分散液,将分散液倒入反应釜中,在210℃烘箱中水热反应14h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤3次,50℃真空干燥12h,研磨过300目筛,得到硒化镉/碳(CdSe/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硒化镉/碳(CdSe/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照5h后,亚甲基蓝的降解率达到90%,而不加催化剂的降解率为9%,说明该催化剂催化降解效果明显。
实施例3
(1)将油茶果壳与过氧化氢按体积质量比3:1~5:1(mL/g)混合浸渍14h后,置于马弗炉中碳化8h,冷却后用水漂洗至pH=8,干燥、粉碎,过200目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉、锌污染废水中,处理6h后,取出用茶壳吸附材料等质量的水洗4次,在70℃下烘干,研磨过250目筛;
(3)取负载重金属茶壳粉末28重量份,1M的硫化钠溶液35重量份,混合搅拌4h得到均匀分散液,将分散液倒入反应釜中,在220℃烘箱中水热反应13h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤2次,60℃真空干燥10h,研磨过250目筛,得到硫化镉锌/碳(CdZnS/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硫化镉锌/碳(CdZnS/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照3.5h后,亚甲基蓝的降解率达到93%,而不加催化剂的降解率为12%,说明该催化剂催化降解效果明显。
实施例4
(1)将油茶果壳与磷酸按体积质量比3:1~5:1(mL/g)混合浸渍12h后,置于马弗炉中碳化7h,冷却后用水漂洗至pH=7,干燥、粉碎,过180目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉、锌污染废水中,处理7h后,取出用茶壳吸附材料等质量的水洗5次,在60℃下烘干,研磨过400目筛;
(3)取负载重金属茶壳粉末35重量份,0.5M的硫化钠溶液30重量份,0.5M的硒化钠溶液30重量份,混合搅拌5h得到均匀分散液,将分散液倒入反应釜中,在210℃烘箱中水热反应13h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤3次,70℃真空干燥9h,研磨过400目筛,得到硒硫化镉锌/碳(CdZnSSe/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硒硫化镉锌/碳(CdZnSSe/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照4h后,亚甲基蓝的降解率达到91%,而不加催化剂的降解率为11%,说明该催化剂催化降解效果明显。
实施例5
(1)将油茶果壳与硝酸按体积质量比3:1~5:1(mL/g)混合浸渍12h后,置于马弗炉中碳化8h,冷却后用水漂洗至pH=8,干燥、粉碎,过130目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉、锌、镍污染废水中,处理5h后,取出用茶壳吸附材料等质量的水洗6次,在70℃下烘干,研磨过350目筛;
(3)取负载重金属茶壳粉末25重量份,1.5M硫化氢钠溶液35重量份,混合搅拌4h得到均匀分散液,将分散液倒入反应釜中,在190℃烘箱中水热反应14h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤2次,60℃真空干8h,研磨过350目筛,得到硫化镉镍锌/碳(CdNiZnS/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硫化镉镍锌/碳(CdNiZnS/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照4.5h后,亚甲基蓝的降解率达到92%,而不加催化剂的降解率为10%,说明该催化剂催化降解效果明显。
实施例6
(1)将油茶果壳与过氧化氢按体积质量比3:1~5:1(mL/g)混合浸渍15h后,置于马弗炉中碳化6h,冷却后用水漂洗至pH=7,干燥、粉碎,过100目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉、锌、镍污染废水中,处理5h后,取出用茶壳吸附材料等质量的水洗5次,在80℃下烘干,研磨过450目筛;
(3)取负载重金属茶壳粉末30重量份,2M硫化氢钠溶液35重量份,混合搅拌5h得到均匀分散液,将分散液倒入反应釜中,在220℃烘箱中水热反应13h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤3次,70℃真空干9h,研磨过450目筛,得到硒化镉镍锌/碳(CdNiZnSe/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硒化镉镍锌/碳(CdNiZnSe/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照5.5h后,亚甲基蓝的降解率达到91%,而不加催化剂的降解率为9%,说明该催化剂催化降解效果明显。
实施例7
(1)将油茶果壳与磷酸按体积质量比3:1~5:1(mL/g)混合浸渍14h后,置于马弗炉中碳化7h,冷却后用水漂洗至pH=8,干燥、粉碎,过250目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉、铜污染废水中,处理7h后,取出用茶壳吸附材料等质量的水洗6次,在70℃下烘干,研磨过500目筛;
(3)取负载重金属茶壳粉末50重量份,硫脲30重量份,水18重量份,混合搅拌4h得到均匀分散液,将分散液倒入反应釜中,在210℃烘箱中水热反应14h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤2次,65℃真空干燥10h,研磨过500目筛,得到硫化镉铜/碳(CdCuS/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硫化镉铜/碳(CdCuS/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照3.5h后,亚甲基蓝的降解率达到90%,而不加催化剂的降解率为8%,说明该催化剂催化降解效果明显。
实施例8
(1)将油茶果壳与过氧化氢按体积质量比3:1~5:1(mL/g)混合浸渍15h后,置于马弗炉中碳化8h,冷却后用水漂洗至pH=6,干燥、粉碎,过160目筛得到茶壳吸附材料;
(2)将茶壳吸附材料置于镉、铜污染废水中,处理6h后,取出用茶壳吸附材料等质量的水洗6次,在80℃下烘干,研磨过300目筛;
(3)取负载重金属茶壳粉末45重量份,硫脲20重量份,硒脲20重量份,水25重量份,混合搅拌5h得到均匀分散液,将分散液倒入反应釜中,在220℃烘箱中水热反应15h,冷却至室温后用茶壳吸附材料等质量的水和乙醇依次洗涤3次,60℃真空干燥12h,研磨过300目筛,得到硒硫化镉铜/碳(CdCuSSe/C)复合光催化剂。
光催化效果验证:取浓度500mg/L的亚甲基蓝溶液1L于烧杯中,加1g制得的硒硫化镉铜/碳(CdCuSSe/C)复合光催化剂,置于暗处,并搅拌12h,使得体系达到吸附饱和状态,取样5mL备用。在高压汞灯照射下进行光催化降解亚甲基蓝实验,每隔30min用亚甲基蓝浓度测试仪测定亚甲基蓝浓度,测得光照3h后,亚甲基蓝的降解率达到92%,而不加催化剂的降解率为10%,说明该催化剂催化降解效果明显。
如上所述,便可较好地实现本发明。
本发明的实施方式并不受上述实施例的限制,其他任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (8)
1.一种重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于包括如下步骤:
步骤一:将油茶果壳与活化剂混合浸渍12~15h后,置于马弗炉中碳化6~8h,待冷却后用水漂洗至pH=7~9,在经过干燥、粉碎、过筛得到茶壳吸附材料;
步骤二:将茶壳吸附材料置于重金属污染废水中,吸附5~7h后,取出用含有茶壳吸附材料的水洗3~6次,经过40~80℃烘干,研磨过筛后得到负载重金属离子的茶壳粉末;
步骤三:将负载重金属离子的茶壳粉末与硫磺、硫脲、硒粉、硒脲、硫化钠溶液、硒化钠溶液、硫化氢钠溶液、硒化氢钠溶液中的一种或两种以上混合,加入去离子水搅拌2~5h得到均匀分散液,将分散液倒入反应釜中,170~230℃水热反应12~15h,冷却至室温后用含有茶壳吸附材料的水和乙醇依次洗涤2~3次,50~70℃真空干燥8~12h,研磨过筛,得到碳基光催化剂。
2.根据权利要求1所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:步骤一中油茶果壳粉碎过筛是采用目数为100~200目的筛网;
步骤二和步骤三中所述研磨过筛是采用目数为200~500目的筛网。
3.根据权利要求2所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:步骤一中活化剂为磷酸、硝酸或过氧化氢中的一种;
活化剂与油茶果壳的浸渍比为体积质量比3:1~5:1(mL/g)。
4.根据权利要求1所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:步骤一中活化剂与油茶果壳的浸渍比为3:1~5:1。
5.根据权利要求3所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:步骤三中负载重金属离子的茶壳粉末与硫磺、硫脲、硒粉、硒脲固体混合,各原料重量份为:负载重金属茶壳粉末45~60份,硫磺、硫脲、硒粉、硒脲固体分别为20~35份;水15~25份。
6.根据权利要求3所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:步骤三中负载重金属离子的茶壳粉末与硫化钠溶液、硒化钠溶液、硫化氢钠溶液、硒化氢钠溶液浓度为0.5~5 M,各原料重量份为:负载重金属茶壳粉末20~35份,硫化钠溶液、硒化钠溶液、硫化氢钠溶液、硒化氢钠溶液30~45份。
7.根据权利要求1所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:步骤二中重金属污染废水中的重金属为镉、铬、铜、锌、镍中的一种或几种。
8.根据权利要求1所述重金属污染废水处理的油茶果壳制备光催化剂的方法,其特征在于:所述光催化剂能够在光照下加速有机化合物的降解。
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CN110918053A (zh) * | 2019-11-05 | 2020-03-27 | 广东石油化工学院 | 一种用于吸附金属铬离子的油茶果壳活性炭及其吸附方法 |
CN113413870A (zh) * | 2021-05-17 | 2021-09-21 | 中国科学院青海盐湖研究所 | 氧化镁-金属硫化物-生物质炭复合材料及其制备方法和应用 |
CN113413870B (zh) * | 2021-05-17 | 2022-11-25 | 中国科学院青海盐湖研究所 | 氧化镁-金属硫化物-生物质炭复合材料及其制备方法和应用 |
CN114849639A (zh) * | 2022-06-21 | 2022-08-05 | 内蒙古农业大学 | 一种ZnO/ZnS@氨基化木材气凝胶及其制备方法和应用 |
CN114849639B (zh) * | 2022-06-21 | 2023-09-05 | 内蒙古农业大学 | 一种ZnO/ZnS@氨基化木材气凝胶及其制备方法和应用 |
CN116273179A (zh) * | 2023-03-21 | 2023-06-23 | 中南大学 | 一种Cd配位硫间质的CdxZn1-xS纳米晶体材料的制备方法与应用 |
CN116273179B (zh) * | 2023-03-21 | 2024-04-16 | 中南大学 | 一种Cd配位硫间质的CdxZn1-xS纳米晶体材料的制备方法与应用 |
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