WO2006081774A1 - MÉTHODE DE DÉGRADATION CATALYTIQUE DE COMPOSÉS DE TYPE p-NITROBENZÈNE À L'AIDE DE NANO-Cu2O PAR VOIE MÉCANIQUE - Google Patents

MÉTHODE DE DÉGRADATION CATALYTIQUE DE COMPOSÉS DE TYPE p-NITROBENZÈNE À L'AIDE DE NANO-Cu2O PAR VOIE MÉCANIQUE Download PDF

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Publication number
WO2006081774A1
WO2006081774A1 PCT/CN2006/000199 CN2006000199W WO2006081774A1 WO 2006081774 A1 WO2006081774 A1 WO 2006081774A1 CN 2006000199 W CN2006000199 W CN 2006000199W WO 2006081774 A1 WO2006081774 A1 WO 2006081774A1
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WIPO (PCT)
Prior art keywords
cuprous oxide
nano
friction
degradation
nitrobenzene
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PCT/CN2006/000199
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English (en)
Chinese (zh)
Inventor
Aiqian Zhang
Nan Meng
Shuokui Han
Yun Chen
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Nanjing University
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Publication of WO2006081774A1 publication Critical patent/WO2006081774A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/32—Hydrocarbons, e.g. oil
    • C02F2101/322—Volatile compounds, e.g. benzene
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/08—Nanoparticles or nanotubes
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/33—Wastewater or sewage treatment systems using renewable energies using wind energy
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the invention relates to a method for degrading p-nitrobenzene in water, and more particularly to a method for mechanically degrading p-nitrobenzene by nano-sized cuprous oxide.
  • P-nitrobenzene is a typical toxic organic pollutant in the surface water environment. Because it is low in water and difficult to degrade, it is difficult to remove it from water. At present, the main methods for treating nitrobenzene in water are physical methods, chemical methods and biological methods.
  • the chemical methods mainly include photo-assisted Fenton reaction, heterogeneous photocatalysis, photoelectrocatalysis, and electrochemical methods.
  • Titanium is used as a catalyst to degrade quinone phenol by Heterogeneous photocatalytic degradation of nitrophenols (Journal of Photochemistry and Photobiology A: Chemistry 155 (2003) 207 - 214 ); Mehmeta. Outran et al. Completion Destruction of p-Nitrophenol in Aqueous Medium by Electro - Fenton Method, Environ. Sci. Technol. 2000, 34, 3474-3479 ) 0 iguel Rodriguez et al., under UV irradiation, H 2 0 2 and Fe 3+ photodegradation of nitrobenzene degradation (Influence of H202 and Fe (III) in the photodegradation [J] .
  • the biological method is mainly to degrade p-nitrophenol by microorganisms.
  • Liu Zhi et al. Degradation of p-nitrophenol by methyl parathion-degrading bacterium DLL-E4 (Pseudomonas put i da) (Degradation of p-nitrophenol by methyl sulfonium-degrading bacteria DLL E 4 , China Environmental Science 2003 04)) Gao Shixiang et al.
  • Wu Jianfeng et al reported that a bacterial CNB1 strain of Comaraonas capable of degrading p-chloronitrobenzene was isolated from activated sludge treated with chloronitrobenzene production plant wastewater, and the bacteria were degraded. The characteristics of chloronitrobenzene were studied (Isolation, identification and degradation characteristics of Comacon ⁇ CNB1 degrading p-chloronitrobenzene, Journal of Microbiology 2004, Vol. 44, No. 1). However, the biological treatment method is not efficient, and the culture of the strain is difficult, and the reaction environment is high and difficult to achieve.
  • a method for treating p-nitrophenol production wastewater is disclosed in a method for treating and recycling a wastewater of p-nitrophenol production (Patent Application No. 200410014570. 2), and the process is as follows: Pretreatment, adsorption of nitroxide in the wastewater, back-blowing using sodium chloride, desorption and adsorption of p-nitroxon 3 ⁇ 4 phenol.
  • the method can recover p-nitrophenol, and the caustic soda and hydrochloric acid required for the production of p-nitrophenol can be recycled.
  • the shortcoming of this method is that the process is complicated and the working conditions are more limited.
  • Cuprous oxide is a P-type semiconductor. It is an important inorganic chemical raw material and has a wide range of applications in the fields of antifouling paints, pigments and welding industries. Due to its small forbidden band width, only 2.0-2.2 eV, it is easy to generate photo-generated carriers under the illumination of sunlight, and has excellent stability. It is widely used in petrochemical catalysis and photovoltaic cells. Applications. In 1998, Michikazu Hara and others first reported that cuprous oxide can decompose water under visible light, which is believed to have the potential to convert solar energy into 3 ⁇ 4 energy (Michikazu Hara et al , Cu 2 0 as a photocatalyst for overall water splitting under visible) Light Irradiation, Chem.
  • T. Mahalingam et al. reported the preparation of cuprous oxide films as electrodes for photoelectrochemical solar cells (T. Mahal ingam et. al, Characterization of pulse plated Cu20 thin films, Surface and Coatings Technology 168 (2003) 111-114).
  • Mechanical catalysis is a catalytic method in which mechanical energy is converted into chemical energy by a catalyst to promote the reaction.
  • the principle is to rapidly rub the catalyst at the bottom of the vessel by a stir bar of different materials to generate electrons and promote the reaction.
  • Go Hitoki et al. first reported the use of oxides such as cuprous oxide as a catalyst to catalyze the decomposition of water by mechanical friction to produce hydrogen, and proposed a new way to generate clean energy (Go Hitoki, Catalysis Today 63 (2000) 175 - 181 , Mechano-catalytic overall water splitting on some mixed oxides). Subsequently, the research group successively published related articles on mechanical catalysis, but both applied to decompose water to achieve energy conversion, and did not apply to the field of decomposition of organic pollutants.
  • P-nitrobenzene is a typical toxic organic pollutant in surface water environment. Because it is low in water and difficult to degrade, it is difficult to remove it from water.
  • the object of the present invention is to provide a method for effectively degrading p-nitrobenzene in water, and mechanically catalyzing the degradation of p-nitrobenzene in water by using nano-sized cuprous oxide, which can effectively remove p-nitrobenzene in water. Class of substances. , Technical solutions
  • a method for mechanically catalyzing the degradation of p-nitrobenzene by nano-sized cuprous oxide the steps of which include -
  • the nano-sized cuprous oxide has a particle size ranging from 50 to 500 nm. During the reaction, due to the friction, the particle size of the relatively large particle size of cuprous oxide will become smaller, and the final particle size of cuprous oxide will be between 50 and 200 nra. Cuprous oxide acts only as a catalyst during the reaction.
  • the concentration of p-nitrobenzene waste water is 20 ⁇ : I00mg/L, the degradation effect is better than other concentrations; the optimum treatment wastewater concentration is 60 ⁇ 100mg/L.
  • the concentration is too high, the effect of degradation is lowered, and when the concentration is too low, the treatment cost is relatively high.
  • Nano-sized cuprous oxide can be prepared by a glucose reduction method and an improved electrolysis method.
  • the specific operation of preparing the nano-sized cuprous oxide by the glucose reduction method is as follows: 1000 ml of distilled water is added, and 0.3 mL of a film solution of 0.1 mL of a 13 ml/0 film solution is added, and the mixture is placed in a microwave oven. Power irradiation rapidly warmed the mixed solution to 95 °C. The mixture was quickly cooled to room temperature with an ice water bath, and the obtained cuprous oxide sol was poured into a 250 ml centrifuge tube, centrifuged at 4500 r/min for 30 min, taken out, and the supernatant was transferred to a 150 ml beaker for use.
  • Improved electrolytic method for preparing nano-sized cuprous oxide 250 g of NaCl, 0.5 g of NaOH, 0.1 g of N3 ⁇ 4Cr 2 0 7 was dissolved in 1000 ml of water, and an O. lg stabilizer was added, and the dissolution was ultrasonically promoted as an electrolyte.
  • the copper piece is polished and ultrasonically cleaned as an electrode.
  • the electrolytic cell was placed in an ultrasonic oscillator, copper was used as an electrode, and electrolyzed at a current of 20 raA/cra2 for 8 minutes.
  • the product was centrifuged, washed three times with distilled water, washed three times with acetone, and dried at room temperature to obtain yellow-green oxidation. Cuprous particles, placed in a desiccator for sealing.
  • the addition ratio of nano-sized cuprous oxide is 3 to 4 g/L.
  • the friction device is made of polytetrafluoroethylene material, and the contact surface of the reactor with the friction is ordinary glass, quartz glass, pyrex glass. Increasing the frictional contact area and friction rate helps to increase the reaction rate.
  • Machinery The power of friction can be electromagnetic stirring, electric stirring, in order to save energy and environmental protection, solar energy, wind energy, etc. can be used as power.
  • the friction between the friction device and the bottom surface of the reactor can be achieved by means of rotation, reciprocation or the like.
  • the effect of friction rate on the degradation effect is not obvious. After reaching a certain rate, increasing the friction rate does not improve the conversion rate from mechanical energy to chemical energy.
  • Increasing the contact area of mechanical friction can significantly improve the degradation efficiency. The longer the mechanical friction, the better the degradation effect, but the excessively long time degradation effect is not obvious, and the energy consumption is increased. Under the same conditions, keep the reaction temperature at 30-50 °C, and adjust the pH 5-9 to achieve better degradation.
  • the catalytic degradation rate of p-nitrobenzenes in the wastewater of 20-100 mg/L can reach more than 70%, the method is simple and easy, and the material is easy to obtain. The cost is low. If natural energy is used as mechanical friction power, such as solar energy, wind energy, etc., it is more economical and environmentally friendly, and has industrial application prospects. Fourth, the specific implementation
  • the tempering temperature is 0. 10g / L of the p-nitrophenol solution 200ml was placed in the reactor, adding 0. 80g of improved copper oxide prepared by the hydrolysis method, the solution 11 was 5. 5, maintaining the reaction temperature for the winter water temperature (10 ° C).
  • Example 10 Put a concentration of 0. lQg / L of p-nitrophenol solution 200ml in the reactor, add 0.80g modified copper oxide prepared by the hydrolysis method, the solution! "1 is 5.6, keep the temperature inside the reactor at room temperature in summer (30 °C). Use electromagnetic stirring to rub against the bottom surface.
  • the friction area is 1.02X10— :i m 2 , the friction rate is 600 rpm, and the sample is sampled at 2 ml for high-speed centrifugation. The supernatant is taken for liquid phase. Chromatographic determination. After 2 hours of reaction, the degradation rate of p-nitrophenol reached 70.4%, and the degradation rate reached 91.9% after 4 hours.
  • a p-nitrophenol solution 20 (1 ⁇ 21) having a concentration of 0.07 g/L was placed in the reactor, 0.60 g of cuprous oxide prepared by an improved hydrolysis method was added, and the solution pH was 6.2, and the reaction temperature was maintained at a winter water temperature (10 ° C).
  • the concentration of Na ions reached 0.01 mol/L, and 2 ml of high-speed centrifugation was sampled at a time, and the supernatant was taken for liquid chromatography.
  • Example 17 The basic operation was the same as in Example 15, except that CaCl 2 was used instead of NaCl at a concentration of 0.01-0.05 mol/L, and the effects were basically the same.
  • Example 17
  • cuprous oxide prepared in the above examples was replaced by cuprous oxide prepared by other methods, and the particle size ranged from 50 to 500 nm, and other reaction conditions were unchanged, and similar results were obtained.
  • the temperature of the winter water temperature is maintained at a temperature of 8.0 g. °C).
  • the friction area is 1. 02 X 10 - 3 m 2 , the friction rate is
  • the electric friction is used to cause friction with the bottom surface, and the friction area is 1. 02 X 10 - 3 m 2 , and the friction rate is

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Environmental & Geological Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne une méthode de dégradation de composés de type p-nitrobenzène dans l'eau, ladite méthode consistant en la dégradation catalytique du composé de type p-nitrobenzène à l'aide de nano-Cu2O par voie mécanique. Le procédé inclut les étapes suivantes : (1) alimentation d'un réacteur en eaux usées contenant le composé de type p-nitrobenzène ; (2) addition de nano-Cu2O dans le réacteur à une concentration comprise entre 0,50 g/L et environ 4 g/L ; (3) friction entre un dispositif de friction et le fond du réacteur en fournissant une énergie supplémentaire. Selon l'invention, le rendement de dégradation de la solution de composé de type p-nitrobenzène à 20-100 mg/L peut dépasser 70 %.
PCT/CN2006/000199 2005-02-05 2006-02-05 MÉTHODE DE DÉGRADATION CATALYTIQUE DE COMPOSÉS DE TYPE p-NITROBENZÈNE À L'AIDE DE NANO-Cu2O PAR VOIE MÉCANIQUE WO2006081774A1 (fr)

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CNB2005100377935A CN100344547C (zh) 2005-02-05 2005-02-05 纳米级氧化亚铜机械催化降解对硝基苯类物质的方法
CN200510037793.5 2005-02-05

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112517079A (zh) * 2020-12-15 2021-03-19 广州大学 一种铜-酚羟基络合的类芬顿催化剂及其制备方法与应用
CN115739107A (zh) * 2022-11-22 2023-03-07 安徽工业大学 一种二氧化锰纳米复合材料及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102040302B (zh) * 2009-10-21 2012-06-20 中国石油化工股份有限公司 一种硝基氯苯生产废水的处理方法
CN105675696B (zh) * 2016-01-06 2018-03-16 信阳师范学院 痕量快速检测间苯三酚的电化学传感器及其制备方法与应用
CN109850983A (zh) * 2019-04-04 2019-06-07 武汉大学 基于半导体粉料摩擦催化的污染物治理方法
CN114538442B (zh) * 2020-11-19 2023-06-30 武汉大学 基于半导体粉料摩擦催化的二氧化碳还原方法

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JPS5579086A (en) * 1978-12-12 1980-06-14 Moru Eng Kk Electrolytic treating method for waste water
JPS5644098A (en) * 1979-09-18 1981-04-23 Ebara Infilco Co Ltd Treating method of hydrazine content waste water
JPS5644091A (en) * 1979-09-18 1981-04-23 Ebara Infilco Co Ltd Treating method of hydrazine content waste fluid
JPH0550072A (ja) * 1991-08-20 1993-03-02 Mitsubishi Plastics Ind Ltd 水の汚濁防止方法

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Publication number Priority date Publication date Assignee Title
GB571539A (en) * 1943-06-11 1945-08-29 Cincinnati Milling Machine Co Improvements in or relating to mechanical catalysis
JPS5579086A (en) * 1978-12-12 1980-06-14 Moru Eng Kk Electrolytic treating method for waste water
JPS5644098A (en) * 1979-09-18 1981-04-23 Ebara Infilco Co Ltd Treating method of hydrazine content waste water
JPS5644091A (en) * 1979-09-18 1981-04-23 Ebara Infilco Co Ltd Treating method of hydrazine content waste fluid
JPH0550072A (ja) * 1991-08-20 1993-03-02 Mitsubishi Plastics Ind Ltd 水の汚濁防止方法

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Title
HUANG Z. ET AL.: "SOLAR PHOTODEGRADATION OF 4-CHLORO-NITROBENZENE USING CUPROUS OXIDE", ENVIRONMENTAL CHEMISTRY (RESEARCH CENTER FOR ECO-ENVIRONMENT SCIENCES, CHINESE ACADEMY OF SCIENCES), vol. 22, no. 2, March 2003 (2003-03-01), pages 150 - 153 *
LIU H. ET AL.: "SOLAR PHOTOCATALYTIC DEGRADATION OF p-NITROPHENOL ASSISTED BY CUPROUS OXIDE", ENVIRONMENTAL CHEMISTRY (RESEARCH CENTER FOR ECO-ENVIRONMENT SCIENCES, CHINESE ACADEMY OF SCIENCES), vol. 23, no. 5, September 2004 (2004-09-01), pages 490 - 494 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112517079A (zh) * 2020-12-15 2021-03-19 广州大学 一种铜-酚羟基络合的类芬顿催化剂及其制备方法与应用
CN115739107A (zh) * 2022-11-22 2023-03-07 安徽工业大学 一种二氧化锰纳米复合材料及其制备方法
CN115739107B (zh) * 2022-11-22 2024-01-26 安徽工业大学 一种二氧化锰纳米复合材料及其制备方法

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