CN103623821B - Method for preparing supported cuprous oxide catalyst - Google Patents

Method for preparing supported cuprous oxide catalyst Download PDF

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Publication number
CN103623821B
CN103623821B CN201310624500.8A CN201310624500A CN103623821B CN 103623821 B CN103623821 B CN 103623821B CN 201310624500 A CN201310624500 A CN 201310624500A CN 103623821 B CN103623821 B CN 103623821B
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cuprous oxide
agent
preparation
support type
oxide catalysis
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CN103623821A (en
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马建锋
李良银
姚超
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Changshu intellectual property operation center Co.,Ltd.
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Changzhou University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention discloses a method for preparing a supported cuprous oxide catalyst. The method comprises the following steps: respectively dissolving a copper salt, a magnesium salt and an aluminum salt in water, preparing the salts to solutions with concentrations of 1-2 mol/L, mixing the three solutions, keeping the molar ratio of the mol sum of Cu and Mg ions to Al ions to 2-4, dripping a certain amount of NaOH into a water bath with a constant temperature of 70-80 DEG C, keeping the pH value to 12-13, reacting for 2-3 hours and aging for 12-24 hours, wherein a precipitate of a layered structure is formed in the process; adding 2-5 mol of reducing agent in each liter of the system after the aging procedure is finished, stirring for 2-3 hours, ethanol washing, filtering and vacuum drying at 65-75 DEG C to obtain the supported cuprous oxide catalyst.

Description

The preparation method of a kind of support type cuprous oxide catalysis agent
Technical field
The present invention relates to the preparation method of a kind of support type cuprous oxide catalysis agent, belong to catalysis material preparation field.
Background technology
Traditional method for treating water efficiency is low, cost is high, there is secondary pollution problems, the solution that waste water control can not get always.Dyeing waste water because of discharge capacity large, pollution concentration is high, becomes in industrial wastewater compared with one of waste water of refractory reason.How efficiency utilization solar energy dyeing waste water of degrading has caused the extensive concern of countries in the world.Hydrotalcite because have special structure and larger specific area, standing carrier or the catalyst being used for doing supported catalyst.Due to Cu 2o has good photocatalysis performance, is therefore often loaded (ZnO, TiO on a lot of carrier 2, Graphene and hydrotalcite).Cu after load 2o has excellent photocatalysis effect to dyeing waste water.Tradition hydrotalcite loaded Cu 2the method of O can not make Cu 2o loads to hydrotalcite surface uniformly, reduces catalyst service efficiency.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, disclose the preparation method of a kind of support type cuprous oxide catalysis agent.
The technical solution used in the present invention adopts following steps:
1) mantoquita, magnesium salts and aluminium salt are dissolved in water respectively, be configured to the solution that concentration is 1 ~ 2mol/L, by three kinds of solution mixing, mole sum of Cu and Mg two kinds of ions and the mol ratio of Al ion is kept to be 2 ~ 4, in constant temperature 70 ~ 80 DEG C of water-baths, instill a certain amount of NaOH, keep pH value to be 12 ~ 13, reaction 2 ~ 3h, aging 12 ~ 24h, forms the precipitation with layer structure in this process;
2) after aging end, wherein adding 2 ~ 5mol reducing agent to often going up in the system of stating, stirring 2 ~ 3h, ethanol washing, filtration, vacuum 65 ~ 75 DEG C of dryings, namely obtain the agent of support type cuprous oxide catalysis.
Described mantoquita is CuCl 2, Cu (NO 3) 2, CuSO 4deng in one.
Described magnesium salts is MgCl 2, Mg (NO 3) 2deng in one.
Described aluminium salt is AlCl 3, Al 2(SO 4) 3deng in one.
Described reducing agent is the one in ascorbic acid, hydrazine hydrate etc.
The invention has the beneficial effects as follows:
(1) traditional supported copper is infusion method to the method for hydrotalcite surface, and because copper ion is cation, the method can not by Cu 2o loads to hydrotalcite layers.This method breaches the limitation of traditional ion-exchange process, and the Rotating fields of hydrotalcite can not be destroyed.
(2) Cu of hydrotalcite load 2the size of O is less, Cu 2o can load to hydrotalcite surface uniformly.
(3) this catalyst there is catalysis simultaneously, adsorb difunctional.
(4) Cu 2the load capacity of O realizes by the content controlling the copper in hydrotalcite.
Accompanying drawing explanation
Fig. 1 is the XRD figure of support type cuprous oxide in embodiment 1
Fig. 2 is the uv drs figure of support type cuprous oxide in embodiment 1
Detailed description of the invention
Embodiment 1
By CuCl 2, MgCl 2and AlCl 3be dissolved into respectively in water, be configured to the solution that concentration is 1mol/L, by three kinds of solution mixing, mole sum of Cu and Mg two kinds of ions and the mol ratio of Al ion is kept to be 2, in constant temperature 70 DEG C of water-baths, instill a certain amount of NaOH, keep pH value to be 12, reaction 2h, aging 12h, forms the precipitation with layer structure in this process; After aging end, wherein adding 2mol reducing agent to often going up in the system of stating, stirring 2 ~ 3h, ethanol washing, filtration, vacuum 65 DEG C of dryings, namely obtain the agent of loaded nano cuprous oxide catalysis.
The sample 0.5g obtained being joined 300mL concentration is in the gold orange II waste water of 30mg/L, and under 300w Metal halogen lamp irradiates, reaction 120min, percent of decolourization is 98.5%, and after catalyst separation reuses 3 times, under similarity condition, reaction 120min, percent of decolourization is 92.5%.It is 62.5% that the cuprous oxide of equal quality reuses 3 rear decoloring rates under the same conditions.
Embodiment 2
By Cu (NO 3) 2, Mg (NO 3) 2and Al 2(SO 4) 3be dissolved into respectively in water, be configured to the solution that concentration is 2mol/L, by three kinds of solution mixing, mole sum of Cu and Mg two kinds of ions and the mol ratio of Al ion is kept to be 4, in constant temperature 80 DEG C of water-baths, instill a certain amount of NaOH, keep pH value to be 13, reaction 3h, aging 24h, forms the precipitation with layer structure in this process; After aging end, wherein adding 5mol reducing agent to often going up in the system of stating, stirring 3h, ethanol washing, filtration, vacuum 65 DEG C of dryings, namely obtain the agent of loaded nano cuprous oxide catalysis.
The sample 0.5g obtained being joined 300mL concentration is in the acid scarlet waste water of 30mg/L, under 300w Metal halogen lamp irradiates, and reaction 120min, percent of decolourization is 97.1%, after catalyst separation reuses 3 times, under similarity condition, reaction 120min, percent of decolourization is 93.2%.It is 58.5% that the cuprous oxide of equal quality reuses 3 rear decoloring rates under the same conditions.
Embodiment 3
By CuSO 4, Mg (NO 3) 2and Al 2(SO 4) 3be dissolved into respectively in water, be configured to the solution that concentration is 2mol/L, by three kinds of solution mixing, mole sum of Cu and Mg two kinds of ions and the mol ratio of Al ion is kept to be 3, in constant temperature 75 DEG C of water-baths, instill a certain amount of NaOH, keep pH value to be 13, reaction 3h, aging 24h, forms the precipitation with layer structure in this process; After aging end, wherein adding 4mol reducing agent to often going up in the system of stating, stirring 3h, ethanol washing, filtration, vacuum 75 DEG C of dryings, namely obtain the agent of loaded nano cuprous oxide catalysis.
It is in the rhodamine B of 30mg/L that the sample 0.5g obtained is joined 300mL concentration, under 300w Metal halogen lamp irradiates, and reaction 120min, percent of decolourization is 96.7%, after catalyst separation reuses 3 times, under similarity condition, reaction 120min, percent of decolourization is 89.3%.It is 58.5% that the silver orthophosphate of equal quality reuses 3 rear decoloring rates under the same conditions.

Claims (5)

1. a preparation method for support type cuprous oxide catalysis agent, is characterized in that the step of method is as follows:
1) mantoquita, magnesium salts and aluminium salt are dissolved in water respectively, be configured to the solution that concentration is 1 ~ 2mol/L, by three kinds of solution mixing, mole sum of Cu and Mg two kinds of ions and the mol ratio of Al ion is kept to be 2 ~ 4, in constant temperature 70 ~ 80 DEG C of water-baths, instill a certain amount of NaOH, keep pH value to be 12 ~ 13, reaction 2 ~ 3h, aging 12 ~ 24h, forms the precipitation with layer structure in this process;
2) after aging end, wherein adding 2 ~ 5mol reducing agent to often going up in the system of stating, stirring 2 ~ 3h, ethanol washing, filtration, vacuum 65 ~ 75 DEG C of dryings, namely obtain the agent of loaded nano cuprous oxide catalysis.
2. the preparation method of a kind of support type cuprous oxide catalysis as claimed in claim 1 agent, is characterized in that described mantoquita is CuCl 2, Cu (NO 3) 2, CuSO 4in one.
3. the preparation method of a kind of support type cuprous oxide catalysis as claimed in claim 1 agent, is characterized in that described magnesium salts is MgCl 2, Mg (NO 3) 2in one.
4. the preparation method of a kind of support type cuprous oxide catalysis as claimed in claim 1 agent, is characterized in that described aluminium salt is AlCl 3, Al 2(SO 4) 3in one.
5. the preparation method of a kind of support type cuprous oxide catalysis as claimed in claim 1 agent, is characterized in that described reducing agent is the one in ascorbic acid, hydrazine hydrate.
CN201310624500.8A 2013-11-28 2013-11-28 Method for preparing supported cuprous oxide catalyst Active CN103623821B (en)

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Publication number Priority date Publication date Assignee Title
CN104226239A (en) * 2014-10-10 2014-12-24 武汉工程大学 Hydrotalcite/cuprous oxide nanocomposite material and application thereof
CN109046352A (en) * 2018-07-13 2018-12-21 陶春梅 A kind of method that catalysis prepares tumor vessel blocking agent pharmaceutical intermediate
CN109046357A (en) * 2018-08-27 2018-12-21 上海大学 A kind of preparation method of metal oxide-LDH loaded catalyst
CN108822953B (en) * 2018-08-31 2021-03-23 台州学院 Efficient regeneration treatment method for waste lubricating oil
CN110467215B (en) * 2019-08-06 2021-02-26 西安交通大学 Preparation method of shape-controllable iron and zinc ion co-doped cuprous oxide crystal
CN110372030B (en) * 2019-08-07 2022-11-18 中国科学院理化技术研究所 Zinc-aluminum hydrotalcite rich in cuprous ions and preparation method and application thereof
CN110396607A (en) * 2019-09-03 2019-11-01 中南大学 A kind of processing method of waste and old ternary lithium ion battery powder
CN115318290B (en) * 2022-08-12 2023-11-03 同济大学 Three-dimensional sea urchin-like structure Cu/Cu 2 O-Al 2 O 3 Nanocomposite material, preparation method and application thereof

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KR100594634B1 (en) * 2003-06-04 2006-07-03 김선재 Synthesizing Process for Advanced Photocatalytic Titanium Dioxide Composited Nanopowders
CN102464322B (en) * 2010-11-02 2014-01-29 中国科学院化学研究所 Cuprous oxide clay nano-sized composition and preparation method thereof
CN103372434A (en) * 2012-04-27 2013-10-30 陈金毅 Preparation method and application of rectorite/cuprous oxide nanocomposite

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