CN103071498B - A kind of preparation method of Cu2O composite photocatalyst - Google Patents
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 8
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 27
- 239000010949 copper Substances 0.000 claims abstract description 25
- 239000010439 graphite Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 150000001879 copper Chemical class 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 239000005749 Copper compound Substances 0.000 abstract description 4
- 150000001880 copper compounds Chemical class 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 7
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
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- 238000002835 absorbance Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
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- 238000003889 chemical engineering Methods 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明提供一种Cu2O复合型光催化剂的制备方法，包括如下步骤：将蒸馏水、无水乙醇和铜盐溶液混合，然后加入膨胀石墨搅拌均匀，接着加入NaOH溶液和无水乙醇，最后加入NH2OH?HCl溶液，搅拌后静置；所得溶液进行水浴加热并搅拌，反应完成分层后，倒掉上层清液，冲洗沉淀，最后将沉淀溶解在无水乙醇中，烘干后即得一种Cu2O复合型光催化剂。本发明中以膨胀石墨和铜化合物为原料制备出膨胀石墨负载纳米Cu2O样品，原材料来源容易，价格低，制备工艺简单，对设备要求低，可操作性好；制备的光催化剂中纳米颗粒均匀负载在膨胀石墨表面，能够在可见光条件下高效降解有毒有害物质，回收利用简单，非常适用于有机污染物的处理。The invention provides a preparation method of Cu 2 O composite photocatalyst, comprising the following steps: mixing distilled water, absolute ethanol and copper salt solution, then adding expanded graphite and stirring evenly, then adding NaOH solution and absolute ethanol, and finally adding NH 2 OH?HCl solution, stirred and left standing; the obtained solution was heated and stirred in a water bath, after the reaction was separated, poured off the supernatant, washed the precipitate, and finally dissolved the precipitate in absolute ethanol, and dried it to obtain A Cu 2 O composite photocatalyst. In the present invention, expanded graphite and copper compounds are used as raw materials to prepare expanded graphite-loaded nano- Cu2O samples. The source of raw materials is easy, the price is low, the preparation process is simple, the requirements for equipment are low, and the operability is good; the nanoparticles in the prepared photocatalyst Evenly loaded on the surface of expanded graphite, it can efficiently degrade toxic and harmful substances under visible light conditions, and is easy to recycle, making it very suitable for the treatment of organic pollutants.
Description
技术领域 technical field
本发明涉及化学工程中的光催化剂制备技术领域，具体是一种Cu2O复合型光催化剂的制备方法。 The invention relates to the technical field of photocatalyst preparation in chemical engineering, in particular to a method for preparing a Cu2O composite photocatalyst.
背景技术 Background technique
近年来，纳米Cu2O由于其具有优越的光催化性能，在环境污染治理方面逐步受到了环境研究者的重视，是继TiO2之后的新一代光催化剂，是一种极具开发前景的绿色环保光催化剂。有关研究表明，以纳米Cu2O为光催化剂，利用太阳光作为光源处理印染废水的研究，表明Cu2O多相催化法将可能成为染料废水治理的有效途径。 In recent years, due to its superior photocatalytic performance, nano-Cu 2 O has gradually attracted the attention of environmental researchers in the field of environmental pollution control. It is a new generation of photocatalyst after TiO 2 and a green Environmentally friendly photocatalyst. Relevant studies have shown that using nano-Cu 2 O as a photocatalyst and using sunlight as a light source to treat printing and dyeing wastewater shows that Cu 2 O heterogeneous catalysis may become an effective way to treat dye wastewater.
为了提高Cu2O的光催化性能，可对其进行改性。有关学者对Cu2O内嵌碳纳米管复合球的合成及光催化性能的研究，说明了Cu2O复合球对硝基苯酚溶液的光催化降解率比Cu2O高出10%左右。然而碳纳米管由于价格昂贵不适用于工业生产，所以用价格低廉的载体代替碳纳米管负载Cu2O就成为研究者的研究重点。 In order to improve the photocatalytic performance of Cu 2 O, it can be modified. Relevant scholars have studied the synthesis and photocatalytic performance of Cu 2 O embedded carbon nanotube composite spheres, indicating that the photocatalytic degradation rate of Cu 2 O composite spheres for nitrophenol solution is about 10% higher than that of Cu 2 O. However, carbon nanotubes are not suitable for industrial production due to their high price, so it has become the research focus of researchers to replace carbon nanotubes with Cu 2 O with low-cost supports.
膨胀石墨是天然石墨经强氧化剂氧化得到一种层状化合物，具有比表面积大、层间离子交换能力强等特点，这些特点有利于膨胀石墨与无机材料的复合。以膨胀石墨作为载体所制备的纳米复合材料显示出了诸多优越的性能，而其成本却比碳纳米管复合材料低很多，因而具有潜在的应用前景。目前的研究主要集中在膨胀石墨/有机物纳米复合材料方面，关于膨胀石墨/无机物复合材料的研究相对较少。 Expanded graphite is a layered compound obtained by oxidizing natural graphite with a strong oxidant. It has the characteristics of large specific surface area and strong ion exchange capacity between layers. These characteristics are conducive to the compounding of expanded graphite and inorganic materials. Nanocomposites prepared with expanded graphite as a carrier show many superior properties, but their cost is much lower than that of carbon nanotube composites, so they have potential application prospects. The current research mainly focuses on expanded graphite/organic nanocomposites, and there are relatively few studies on expanded graphite/inorganic composites.
基于以上分析，本发明以膨胀石墨和铜化合物为原料，通过直接沉淀法制备出一种Cu2O复合型光催化剂，这种催化剂制备成本低，制备工艺简单，对设备要求低，可操作性好，在可见光下能够高效降解有毒有害物质，回收利用简单，非常适用于染料废水的深度治理。 Based on the above analysis, the present invention uses expanded graphite and copper compounds as raw materials to prepare a Cu 2 O composite photocatalyst by direct precipitation method. This catalyst has low preparation cost, simple preparation process, low equipment requirements, and high operability Well, it can efficiently degrade toxic and harmful substances under visible light, and is easy to recycle. It is very suitable for the advanced treatment of dye wastewater.
发明内容 Contents of the invention
本发明的目的在于提供一种Cu2O复合型光催化剂的制备方法，以膨胀石墨和铜化合物为原料，通过直接沉淀法制备出膨胀石墨负载纳米Cu2O样品，该制备工艺简单，成本低，对设备要求低，可操作性好。 The purpose of the present invention is to provide a preparation method of Cu2O composite photocatalyst, using expanded graphite and copper compound as raw materials, to prepare expanded graphite supported nano Cu2O sample by direct precipitation method, the preparation process is simple and the cost is low , low requirements on equipment, good operability.
本发明提供的技术方案是：一种Cu2O复合型光催化剂的制备方法，其特征在于包括如下步骤： The technical solution provided by the present invention is: a method for preparing a Cu 2 O composite photocatalyst, which is characterized in that it includes the following steps:
（1）将83.4单位体积的蒸馏水、20单位体积的无水乙醇和5单位体积的0.5 mol/L的铜盐溶液混合，然后加入膨胀石墨搅拌均匀，接着交替加入9单位体积的1.0 mol/L 的NaOH溶液和30单位体积的无水乙醇，最后均加入0.5~15单位体积的0.5 mol/L的NH2OH•HCl溶液，搅拌后静置1~6 小时； (1) Mix 83.4 unit volumes of distilled water, 20 unit volumes of absolute ethanol and 5 unit volumes of 0.5 mol/L copper salt solution, then add expanded graphite and stir evenly, then alternately add 9 unit volumes of 1.0 mol/L NaOH solution and 30 unit volumes of absolute ethanol, and finally add 0.5~15 unit volumes of 0.5 mol/L NH 2 OH·HCl solution, stir and let stand for 1~6 hours;
（2）将步骤一中所得溶液进行水浴加热1~30分钟并搅拌，待溶液反应完成分层后，倒掉上层清液，用无水乙醇和蒸馏水的混合溶液来冲洗沉淀，最后将沉淀溶解在无水乙醇中，在20~80℃下烘干沉淀，即得一种Cu2O复合型光催化剂。 (2) Heat the solution obtained in step 1 in a water bath for 1 to 30 minutes and stir. After the solution has reacted and stratified, pour off the supernatant, wash the precipitate with a mixed solution of absolute ethanol and distilled water, and finally dissolve the precipitate In absolute ethanol, dry the precipitate at 20-80°C to obtain a Cu 2 O composite photocatalyst.
所述步骤一中的铜盐溶液为CuCl2或Cu(NO3)2溶液，铜盐与膨胀石墨的质量比为5:1~1:1。 The copper salt solution in the first step is CuCl 2 or Cu(NO 3 ) 2 solution, and the mass ratio of copper salt to expanded graphite is 5:1-1:1.
所述步骤一中膨胀石墨的负载量为10%~50%。 The loading capacity of expanded graphite in the step 1 is 10%-50%.
所述步骤一中加入NH2OH•HCl溶液的时间为1~30秒。 The time for adding the NH 2 OH·HCl solution in the first step is 1-30 seconds.
所述步骤二中用来冲洗沉淀的混合溶液中，无水乙醇和蒸馏水的体积比为1：1。 In the mixed solution used to wash the precipitate in the second step, the volume ratio of absolute ethanol and distilled water is 1:1.
本发明的有益效果是： The beneficial effects of the present invention are:
（1）本发明中以膨胀石墨和铜化合物为原料，通过直接沉淀法制备出膨胀石墨负载纳米Cu2O样品，所采用的原材料来源容易，价格低，制备工艺简单，对设备要求低，可操作性好； (1) In the present invention, expanded graphite and copper compounds are used as raw materials to prepare expanded graphite-loaded nano-Cu 2 O samples by direct precipitation method. The source of raw materials used is easy, the price is low, the preparation process is simple, and the requirements for equipment are low. Good operability;
（2）本发明制备的光催化剂中纳米颗粒均匀负载在膨胀石墨表面，能够在可见光条件下高效降解有毒有害物质，回收利用简单，非常适用于有机污染物的处理； (2) Nanoparticles in the photocatalyst prepared by the present invention are evenly loaded on the surface of expanded graphite, which can efficiently degrade toxic and harmful substances under visible light conditions, and are easy to recycle, and are very suitable for the treatment of organic pollutants;
（3）膨胀石墨具有比表面积大、层间离子交换能力强等特点，这些特点有利于膨胀石墨与无机材料的复合，以膨胀石墨作为载体所制备的纳米光催化复合材料具有很好的协同作用，可以大大提高其光催化降解能力。 (3) Expanded graphite has the characteristics of large specific surface area and strong interlayer ion exchange capacity. These characteristics are conducive to the composite of expanded graphite and inorganic materials. The nano-photocatalytic composite material prepared with expanded graphite as a carrier has a good synergistic effect , can greatly improve its photocatalytic degradation ability.
具体实施方式 Detailed ways
下面结合具体实施例对本发明做进一步说明，本发明不仅仅限于这些实施例。 The present invention will be further described below in conjunction with specific embodiments, and the present invention is not limited to these embodiments.
实施例1： Example 1:
一种Cu2O复合型光催化剂的制备方法，其特征在于包括如下步骤： A method for preparing a Cu2O composite photocatalyst, characterized in that it comprises the following steps:
（1）将83.4ml的蒸馏水、20ml的无水乙醇和5ml的0.5 mol/L的CuCl2溶液混合，然后加入膨胀石墨搅拌均匀，其中铜盐与膨胀石墨的质量比为5:1，接着交替加入9ml的1.0 mol/L 的NaOH溶液和30ml的无水乙醇，最后在5秒内均加入9.8ml的0.5 mol/L的NH2OH•HCl溶液，搅拌后静置6小时； (1) Mix 83.4ml of distilled water, 20ml of absolute ethanol and 5ml of 0.5 mol/L CuCl 2 solution, then add expanded graphite and stir evenly, wherein the mass ratio of copper salt to expanded graphite is 5:1, then alternately Add 9ml of 1.0 mol/L NaOH solution and 30ml of absolute ethanol, and finally add 9.8ml of 0.5 mol/L NH 2 OH·HCl solution within 5 seconds, stir and let stand for 6 hours;
（2）将步骤一中所得溶液进行水浴加热10分钟并搅拌，待溶液反应完成分层后，倒掉上层清液，用体积比为1:1的无水乙醇和蒸馏水的混合溶液来冲洗沉淀，最后将沉淀溶解在无水乙醇中，在75℃下烘干沉淀，即得一种Cu2O复合型光催化剂。 (2) Heat the solution obtained in step 1 in a water bath for 10 minutes and stir. After the solution has reacted and stratified, pour off the supernatant and wash the precipitate with a mixed solution of absolute ethanol and distilled water with a volume ratio of 1:1. , and finally dissolve the precipitate in absolute ethanol, and dry the precipitate at 75°C to obtain a Cu 2 O composite photocatalyst.
将该复合型光催化剂按照光催化降解有机污染物的评价方法进行光催化降解实验，结果发现甲基橙的降解率可达98%。 The photocatalytic degradation experiment of the composite photocatalyst was carried out according to the evaluation method of photocatalytic degradation of organic pollutants, and it was found that the degradation rate of methyl orange could reach 98%.
实施例2： Example 2:
一种Cu2O复合型光催化剂的制备方法，其特征在于包括如下步骤： A method for preparing a Cu2O composite photocatalyst, characterized in that it comprises the following steps:
（1）将83.4ml的蒸馏水、20ml的无水乙醇和5ml的0.5 mol/L的Cu(NO3)2溶液混合，然后加入膨胀石墨搅拌均匀，其中铜盐与膨胀石墨的质量比为1:1，接着交替加入9ml的1.0 mol/L 的NaOH溶液和30ml的无水乙醇，最后在25秒内均加入15ml的0.5 mol/L的NH2OH•HCl溶液，搅拌后静置1.5小时； (1) Mix 83.4ml of distilled water, 20ml of absolute ethanol and 5ml of 0.5 mol/L Cu(NO 3 ) 2 solution, then add expanded graphite and stir evenly, where the mass ratio of copper salt to expanded graphite is 1: 1. Then alternately add 9ml of 1.0 mol/L NaOH solution and 30ml of absolute ethanol, and finally add 15ml of 0.5 mol/L NH 2 OH·HCl solution within 25 seconds, stir and let stand for 1.5 hours;
（2）将步骤一中所得溶液进行水浴加热20分钟并搅拌，待溶液反应完成分层后，倒掉上层清液，用体积比为1:1的无水乙醇和蒸馏水的混合溶液来冲洗沉淀，最后将沉淀溶解在无水乙醇中，在50℃下烘干沉淀，即得一种Cu2O复合型光催化剂。 (2) Heat the solution obtained in step 1 in a water bath for 20 minutes and stir. After the solution has reacted and stratified, pour off the supernatant and wash the precipitate with a mixed solution of absolute ethanol and distilled water with a volume ratio of 1:1. , and finally dissolve the precipitate in absolute ethanol, and dry the precipitate at 50°C to obtain a Cu 2 O composite photocatalyst.
将该复合型光催化剂按照光催化降解有机污染物的评价方法进行光催化降解实验，结果发现甲基橙的降解率可达93%。 The photocatalytic degradation experiment of the composite photocatalyst was carried out according to the evaluation method of photocatalytic degradation of organic pollutants, and it was found that the degradation rate of methyl orange could reach 93%.
光催化降解有机污染物的评价方法：以甲基橙为目标污染物，配置30mg/L 的甲基橙溶液，将100mg的催化剂样品加到90mL甲基橙溶液中，在上述条件下进行甲基橙溶液的催化脱色降解，在此过程中持续搅拌。首先暗反应30分钟, 随后取6mL试样，立即离心除去光催化剂。用722型分光光度计测定清液在λmax=464nm处的吸光度值。之后，进行光催化反应，每隔10分钟取一次样，测所取试样的吸光度值，光催化实验总时长为2小时。90分钟后得到样品的紫外可见吸收光谱。 Evaluation method for photocatalytic degradation of organic pollutants: take methyl orange as the target pollutant, configure 30mg/L methyl orange solution, add 100mg catalyst sample to 90mL methyl orange solution, and perform methyl orange under the above conditions Catalytic decolorization degradation of the orange solution with constant stirring. First react in dark for 30 minutes, then take a 6mL sample and immediately centrifuge to remove the photocatalyst. Use a 722-type spectrophotometer to measure the absorbance value of the serum at λmax=464nm. Afterwards, the photocatalytic reaction was carried out, and a sample was taken every 10 minutes to measure the absorbance value of the sample taken. The total duration of the photocatalytic experiment was 2 hours. After 90 minutes, the ultraviolet-visible absorption spectrum of the sample was obtained.
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| CN110496624A (en) * | 2019-08-22 | 2019-11-26 | 四川建筑职业技术学院 | Composite material for sewage treatment and preparation method thereof |
| CN113117676A (en) * | 2021-03-08 | 2021-07-16 | 新乡学院 | Cu2Preparation method of O-CuO/bentonite photocatalytic composite material |
| CN113441156A (en) * | 2021-06-24 | 2021-09-28 | 青岛科技大学 | Hollowed-out spherical structure Cu2O/Cu9S5Photocatalytic material and preparation method and application thereof |
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