CN107899594A - 一种碳点修饰羟基磷酸铜光催化材料及其制备方法 - Google Patents
一种碳点修饰羟基磷酸铜光催化材料及其制备方法 Download PDFInfo
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- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 7
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开了一种碳点修饰羟基磷酸铜光催化材料及其制备方法。制备过程是将硝酸铜、磷酸氢二铵、聚乙烯吡咯烷酮及L‑异亮氨酸依次加入到蒸馏水中搅拌溶解;调节pH值,搅拌均匀后水热反应,水热所得产物经洗涤、干燥后得到碳点修饰羟基磷酸铜材料。该制备方法工艺简单,可通过一步水热法制成;可行性强。所制备的碳点修饰羟基磷酸铜作为光催化材料应用时,表现出电子‑空穴对复合率低、光催化活性高及太阳能利用率高的特点。
Description
技术领域
本发明涉及光催化材料技术领域,具体涉及一种碳点修饰羟基磷酸铜光催化材料及其制备方法。
背景技术
以TiO2为代表的光催化技术基于反应条件温和,工艺简单以及环境友好等特点,被认为是一种理想的环境污染治理技术。而TiO2带隙能高,只能在紫外光区(<387nm,占太阳光3%-5%)响应,太阳能利用率低,使其应用受到限制。因此,开发合成可见光响应型光催化材料,提高太阳能利用率是目前光催化领域研究的热点问题。
羟基磷酸铜(Cu2(OH)PO4)基于易于产物分离、催化活性优异及稳定性等优势,被广泛应用于催化领域。近年来,相关研究(Cho I-S. Advanced Functional Materials,2008; 18(15): 2154-2162; G. Wang,et al. Angewandte Communication, 2013, 52:4810-4813)证明:羟基磷酸铜在可见光区域(约占太阳光46%)到近红外区域下都具有光催化活性,提高了太阳能的利用率。但仍存在电子-空穴对复合率高,光催化活性低等缺点。针对此,CN201410447867.1公开了一种石墨烯/羟基磷酸铜复合催化剂及其制备方法,利用石墨烯与羟基磷酸铜复合,降低催化剂粒径、增大其比表面积,从而加快电子-空穴复合,提高光催化性能。
碳点是一种新型的碳纳米材料,基于优异的光电性能被应用于光催化领域。如碳点用来修饰ZnO、CuWO4(冯昌. 物理化学学报, 2015, 31(12):2349-2357; Puthalapattu,Journal of Molecular Structure, 2015, 1098:146-152),上述研究表明碳点作为光生电子转移体,可有效降低电子-空穴对分离,从而提高光催化活性。但碳点用来修饰羟基磷酸铜的研究尚未见诸报道。
发明内容
本发明旨在解决羟基磷酸铜电子-空穴对复合率高的缺点,在羟基磷酸铜表面生成的碳点,可作为光生电子转移体,加快羟基磷酸铜电子-空穴的分离,提高其光催化活性,从而提供了一种碳点修饰羟基磷酸铜光催化材料及其制备方法。
为了解决上述技术问题,本发明提供了如下的技术方案:
一种碳点修饰羟基磷酸铜光催化材料,所述碳点修饰羟基磷酸铜光催化材料是以硝酸铜、磷酸氢二铵、聚乙烯吡咯烷酮及L-异亮氨酸为原料,采用水热合成法制备而成。
一种碳点修饰羟基磷酸铜光催化材料的制备方法,包括如下步骤:
1)按摩尔比依次将硝酸铜、磷酸氢二铵、聚乙烯吡咯烷酮、L-异亮氨酸混合于去离子水中,搅拌30min得悬浮液;
2)调节体系pH值为4-8,并继续搅拌10-20min;
3)将所得的悬浮液转移到聚四氟乙烯反应釜中,在170-210℃水热反应15-24小时;
4)冷却,过滤,洗涤后干燥得到碳点修饰羟基磷酸铜粉末。
所述步骤1)中,磷酸根离子浓度为0.3mol/L,铜离子、磷酸根离子、聚乙烯吡咯烷酮以及L-异亮氨酸化学剂量摩尔比为2:1:0.5:0.2-0.6,其中聚乙烯吡咯烷酮的化学剂量按照其结构单元分子量111g/mol计算。
所述步骤2)中,采用磷酸和氨水调节混合液的pH值。
所述步骤4)中,冷却至室温。
所述步骤4)中,采用去离子水和乙醇洗涤直至中性。
与现有技术相比,本发明的优点如下:
1. 本发明采用一步水热法制备了碳点修饰羟基磷酸铜光催化材料,与CN201410447867.1及上述碳点修饰复合材料制备方法相比,无需先行制备复合剂,工艺简单,易操作,是一种有效的复合材料制备方法。
2. 本发明所制备的碳点修饰羟基磷酸铜材料,碳点作为光生电子转移体修饰在羟基磷酸铜表面,该结构能有效加快电子-空穴对分离,增强材料的光催化活性,能在较短时间内将超过90%的有机废水降解。
附图说明
图1为实施例1中产物中X射线衍射图;
图2为实施例1中产物的XPS全谱图;
图3为实施例1中产物的C元素的XPS谱图;
图4为实施例2中产物的扫描电镜图;
图5为实例2与对比样的光致发光光谱图;
图6为实例1对罗丹明B的光催化降解效果图。
具体实施方式
以下结合实施例和附图对本发明做具体说明,而不是对本发明的进一步限定。
实施例1:将5.64g硝酸铜、1.98g磷酸氢二铵、0.83g聚乙烯吡咯烷酮及0.79g L-异亮氨酸,依次加入到50mL水中,搅拌30min;用磷酸和氨水将溶液调节pH值至6,搅拌15min;将混合溶液装入聚四氟乙烯反应釜中,移入鼓风干燥箱中,在温度为190℃条件下反应19h;冷却至室温后,用去离子水和乙醇洗涤直至中性,并经干燥,制得目标产物。其X射线衍射图如图1所示,通过与羟基磷酸铜XRD标准卡片(JCPDS:83-2264)对比,基体相为羟基磷酸铜;其X光电子能谱图(XPS)如图2所示,XPS全谱图中显示有C元素,图3为C元素的XPS谱图,其中,287.2和289.2分别对应表面氧化基团C=O和O-C=O,表明有碳点的存在;结合图1、图2及图3可得,所制得的材料为碳点修饰羟基磷酸铜。
实施例2:将5.64g硝酸铜、1.98g磷酸氢二铵、0.83g聚乙烯吡咯烷酮及0.98g L-异亮氨酸,依次加入到50mL水中,搅拌30min;用磷酸和氨水将溶液调节pH值至8,搅拌15min;将混合溶液装入聚四氟乙烯反应釜中,移入鼓风干燥箱中,在温度为200℃条件下反应18h;冷却至室温后,用去离子水和乙醇洗涤直至中性,经干燥制得碳点修饰羟基磷酸铜粉体。其形貌如图4所示。
为考察其电子-空穴对复合率,做了例2的对比样,其制备工艺中未添加L-异亮氨酸,其它步骤与例2一致。其光致发光光谱图如图5所示,碳点修饰羟基磷酸铜比纯相羟基磷酸铜的电子-空穴复合率低。
实施例3:采用的光催化性能试验方法如下:
称取20mg实施例1所制备的碳点修饰的羟基磷酸铜,将其加入20mL的罗丹明B溶液(浓度为20mg/L)。将上述溶液置于光催化系统中,暗反应搅拌15min,随后在500W氙灯(采用滤波片过滤,波长λ≥410nm)下进行光催化反应,每隔10min取上层液,经10000rpm,10min的离心分离后,取上层清液,用紫外可见分光光度计测量剩余罗丹明B的吸光度,并与原罗丹明B溶液的吸光度比较,计算得出罗丹明B的降解率为91.4%(如图6所示)。
Claims (8)
1.一种碳点修饰羟基磷酸铜光催化材料,其特征在于,以硝酸铜、磷酸氢二铵、聚乙烯吡咯烷酮及L-异亮氨酸为原料,采用水热合成法制备碳点修饰羟基磷酸铜光催化材料。
2.一种碳点修饰羟基磷酸铜光催化材料的制备方法,其特征在于包括如下步骤:
1)按摩尔比依次将硝酸铜、磷酸氢二铵、聚乙烯吡咯烷酮、L-异亮氨酸混合于去离子水中,搅拌30min得悬浮液;
2)调节体系pH值为4-8,并继续搅拌10-20min;
3)将所得的悬浮液转移到聚四氟乙烯反应釜中,在170-210℃水热反应15-24小时;
4)冷却,过滤,洗涤后干燥得到碳点修饰羟基磷酸铜粉末。
3.根据权利要求2所述的一种碳点修饰羟基磷酸铜光催化材料的制备方法,其特征在于,磷酸根离子浓度为0.3mol/L,铜离子、磷酸根离子、聚乙烯吡咯烷酮以及L-异亮氨酸化学剂量摩尔比为2:1:0.5:0.2-0.6,其中聚乙烯吡咯烷酮的化学剂量按照其结构单元分子量111g/mol计算。
4.根据权利要求2所述的一种碳点修饰羟基磷酸铜光催化材料的制备方法,其特征在于,采用磷酸和氨水调节混合液的pH值。
5.根据权利要求2所述的一种碳点修饰羟基磷酸铜光催化材料的制备方法,其特征在于,采用去离子水和乙醇洗涤直至中性。
6.根据2—5任一权利要求所述的一种碳点修饰羟基磷酸铜光催化材料的制备方法制备的碳点修饰羟基磷酸铜。
7.根据2—5任一权利要求所述的一种碳点修饰羟基磷酸铜光催化材料的制备方法制备的碳点修饰羟基磷酸铜在光催化系统中的应用。
8.根据2—5任一权利要求所述的一种碳点修饰羟基磷酸铜光催化材料的制备方法制备的碳点修饰羟基磷酸铜,在可见光的照射下还原工业废水中有机污染物的应用。
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CN114990578A (zh) * | 2022-06-23 | 2022-09-02 | 陕西科技大学 | 一种铜/羟基磷酸铜电催化材料及其制备方法 |
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CN112371173A (zh) * | 2020-11-27 | 2021-02-19 | 沈阳化工研究院有限公司 | 一种应用于间硝基苯磺酸加氢的铂炭催化剂及其制备方法 |
CN112371173B (zh) * | 2020-11-27 | 2023-09-08 | 沈阳化工研究院有限公司 | 一种应用于间硝基苯磺酸加氢的铂炭催化剂及其制备方法 |
CN113578301A (zh) * | 2021-07-28 | 2021-11-02 | 中北大学 | 磷化亚铜-碳点-铜三元复合光催化剂的制备方法 |
CN113578301B (zh) * | 2021-07-28 | 2023-04-25 | 中北大学 | 磷化亚铜-碳点-铜三元复合光催化剂的制备方法 |
CN114990578A (zh) * | 2022-06-23 | 2022-09-02 | 陕西科技大学 | 一种铜/羟基磷酸铜电催化材料及其制备方法 |
CN114990578B (zh) * | 2022-06-23 | 2024-01-19 | 陕西科技大学 | 一种铜/羟基磷酸铜电催化材料及其制备方法 |
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