CN102039125A - Preparation and application method of supported bimetallic catalyst for removing nitrate in water - Google Patents
Preparation and application method of supported bimetallic catalyst for removing nitrate in water Download PDFInfo
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- CN102039125A CN102039125A CN2009100935516A CN200910093551A CN102039125A CN 102039125 A CN102039125 A CN 102039125A CN 2009100935516 A CN2009100935516 A CN 2009100935516A CN 200910093551 A CN200910093551 A CN 200910093551A CN 102039125 A CN102039125 A CN 102039125A
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Abstract
The invention discloses a preparation and application method of catalyst for removing nitrate in water, which belong to the field of water treatment technology application. In the invention, one precious metal, such as palladium, platinum, gold, rhodium, ruthenium and one non-precious metal such as copper, tin, indium, zinc, silver particles are loaded on the surface of activated carbon to obtain a catalyst which can reduce nitrate in water. The catalytic reduction of nitrate can be achieved by electrochemical method using the catalyst. The anode and cathode of an electrolytic cell are separated by a proton exchange membrane, and the catalyst is filled in the cathode chamber. Under a direct current condition, the catalyst can reduce nitrate by using hydrogen generated in the cathode. The catalyst in the invention achieves the advantages of high activity, good stability and low cost. In addition, the method of the invention which is used for removing the nitrate in water has the advantages of simple operation and convenient management.
Description
Technical field
The present invention relates to a kind of preparation and using method thereof of removing the bimetallic loaded catalyst of nitrate in the water, specifically be bimetallic to be carried on be prepared into catalyst on the active carbon, but this catalyst catalytic electrochemical reduction nitrate belongs to the application of water technology.
Background technology
In recent years, along with Increase of population and expanding economy, the nitrogenous effluent that all trades and professions produced, the amount of discarded object all increase fast, in addition to its unreasonable disposal, cause the water body of many countries (underground water, surface water) in the world to be subjected to the pollution of nitrate, China is no exception, and the trend that goes from bad to worse is arranged.At present, the most of areas of China are subjected to azotate pollution to some extent as the underground water of drinking water source, and its concentration of indivedual areas has surpassed 100mg-N/L.
If the nitrate of human body Excessive Intake, easily cause methemoglobinemia, can cause hypoxia death when serious, and effects such as that the nitrosamine that produces in nitrate and nitrite conversion process etc. also have is carcinogenic, teratogenesis and mutagenesis, nitrate also has in various degree toxic to other animals and plants simultaneously.In view of the generality and the harmfulness of azotate pollution, extremely urgent to the improvement of azotate pollution.
The method of removing nitrate in the water body mainly contains: physics method, bioanalysis and chemical method.Although preceding two kinds of methods have obtained application in recent years in practice, the required expense of nitrate that the physics method is removed in the underground water is too high, and removes and do not have selectivity, removes not thoroughly, and the transfer of nitrate pollutants or concentrated has just taken place.The biological denitrification method is converted into nitrogen by the reduction of microorganism with nitrate, be present main method of denitration, but still the shortcoming that exists some to be difficult to overcome is low as capacity of resisting impact load, has secondary pollution, complex process etc.Chemical catalysis is swift in response, and easy operating has vast potential for future development.Chemical reduction method mainly comprises metal simple-substance reducing process, hydrogen catalysis reducing process and electrochemical reducing.The metal simple-substance reducing process is to be that reducing agent is a nitrogen with nitrate reduction with metal simple-substances such as iron, aluminium, zinc, and its reaction condition is difficult to control, easily produces accessory substance and causes secondary pollution.The hydrogen catalysis reducing process is to be reducing agent with hydrogen, under the effect of catalyst nitrate is reduced, and its reaction speed is fast, can avoid the secondary pollution to water.But the solubility of hydrogen in water is low, and inflammable and explosive, and the transportation difficulty has inconvenience when using.Electrochemical reducing is a kind of method of denitration that just develops out in recent years, and the present electrode of studying mostly is precious metal material, as palladium, platinum, gold electrode; The perhaps noble metal electrode of surface modification, it costs an arm and a leg, and rarely has the example of practical engineering application.
Summary of the invention
The objective of the invention is: prepare a kind of have high activity, high stability, the bimetallic activated-carbon catalyst of area load, combined with electrochemical denitration method and hydrogen catalysis denitration method, this catalyst is filled in the cathode chamber of electrochemical reactor, utilize the hydrogen catalytic reduction nitrate nitrogen that produces in the electrochemical process, thereby realize removing the purpose of nitrate in the water.
Catalyst involved in the present invention is the catalyst (A-B/AC) that is carried on active carbon (AC) surface with a kind of (A) in palladium, platinum, gold, rhodium, the ruthenium noble metal and a kind of transition metal (B) as copper, tin, indium, zinc, silver particles, A: B=1 wherein: (0.125-1), A: AC=1: (20-100) (weight ratio).
Catalyst adopts the preparation of wet dip method.At first the corresponding solubility lead compound of the noble metal (A) of metering is dissolved in the hydrochloric acid solution, pretreated active carbon be impregnated in this solution, stir, filter oven dry, high-temperature calcination, be cooled to room temperature, impregnated in then in the gauge water solution that contains transition metal (B), stir, filter, oven dry, high-temperature calcination is cooled to room temperature, at last with its thorough reduction.
Described dip time is 12-24 hour, and bake out temperature is 105-120 ℃, and drying time is 10-18 hour, calcining heat is 200-400 ℃, and calcination time is 1-3 hour, and reduction temperature is 200-300 ℃, recovery time is 2-5 hour, and used reducing atmosphere is a hydrogen.
The method that the catalytic electrochemical that the present invention set up is removed nitrate in the water is as follows:
In reaction unit, adopt PEM to separate between the anode and cathode, have metal (A) and activated-carbon catalyst (B) to be filled in the cathode chamber prepared area load, under logical galvanic situation, pending water enters cathode chamber and catalytic reduction reaction takes place, with nitrate reduction; The cell reaction of water takes place in the anode region.The current strength that is applied between anode and cathode is 20mA-3000mA, the initial pH value of the water of handling be 3-10.
Characteristics of the present invention are:
(1) active carbon of high-ratio surface has absorption property preferably, can make bimetallic more stably be carried on carrier surface with it as carrier, therefore prepared bimetallic carried-type active Pd/carbon catalyst has higher activity, good stability, difficult drop-off in reduction nitrate process.
(2) this catalyst has certain electric conductivity, the energising back can produce little electrolysis on its surface, the hydrogen that little electrolysis produces is that the form with atom is adsorbed on the surface-active position at the beginning of producing, therefore the reduction nitrate nitrogen can be directly used in, and a series of processes such as dissolving-mass transfer-adsorb-be dissociated into atom need not be as added hydrogen, need passed through.
(3) this method with the hydrogen of catholyte water generates as reducing agent, a hydrogen part that produces can be utilized by the electrochemical reduction nitrate anion, another part is as the reducing agent of chemical catalysis reduction nitrate anion, energy consumption, the raising current efficiency of electrochemical method have not only been reduced, but also can overcome added hydrogen in transportation and more otherwise drawbacks easily and safely for chemical catalysis provides required reducing agent.
(4) PEM is divided into cathodic region and anode region with reaction, helps at cathodic region formation reproducibility environment; Proton can be delivered to the cathodic region from the anode region on the other hand, can cushion the pH value in cathodic region.
(5) technology is simple, requires low to operational management.
Embodiment
Embodiment 1
At first the 0.04619g palladium bichloride is dissolved in the appropriate hydrochloric acid solution, adopts the iso volumetric impregnation method, the pretreated Powdered Activated Carbon of 0.554g (PAC) is immersed in the above-mentioned palladium bichloride hydrochloric acid solution, stir, after 24 hours, through 105 ℃ of oven dry 12 hours; 300 ℃ the calcining 2 hours, naturally cool to room temperature after, impregnated in again in an amount of stannic chloride hydrochloric acid solution, make Pd-Sn/AC=1.25% (weight ratio), stir, after 24 hours, through 105 ℃ the oven dry 12 hours; 300 ℃ of calcinings 2 hours, naturally cool to room temperature after, be reducing agent with hydrogen 250 ℃ of reduction 4 hours down, promptly get the activated-carbon catalyst of bimetallic load.
As cathode and anode, as experimental water, the nitrate anion initial concentration is 150mg/L with the sodium nitrate solution (pH=7.11) of deionized water preparation with titanium ruthenium net.The 100ml water sample is injected cathode chamber, and add above-mentioned catalyst 7.5g/L, carry out the electro-catalysis denitration reaction under the condition of current strength 180mA, behind the reaction 90min, the nitrate removal rate reaches 90%.
Embodiment 2
Preparation of Catalyst and use this catalyst to remove the method such as the example 1 of nitrate in water, different is Pd-Sn/PAC=2.5% (weight ratio) wherein.Cathodic region nitrate anion initial concentration is 150mg/L, and initial pH is 7.11, and behind the reaction 90min, the nitrate removal rate reaches 93%.
Embodiment 3
Preparation of Catalyst and use this catalyst to remove the method such as the example 1 of nitrate in water, different is Pd-Sn/PAC=3% (weight ratio) wherein.Cathodic region nitrate anion initial concentration is 150mg/L, and initial pH is 7.11, and behind the reaction 90min, the nitrate removal rate reaches 95%.
Embodiment 4
Preparation of Catalyst and this catalyst of use are removed the method such as the example 1 of nitrate in water, different is that the nitrate removal rate reached 92% after 40min was carried out in reaction as experimental water (the nitrate anion initial concentration is that 35mg/L, initial pH are 6.96) with actual underground water.
Embodiment 5
At first the 0.04619g palladium bichloride is dissolved in the appropriate hydrochloric acid solution, adopts the iso volumetric impregnation method, the pretreated granular activated carbon of 0.554g (GAC) is immersed in the above-mentioned palladium bichloride hydrochloric acid solution, carry out periodicity and stir, after 24 hours, through 105 ℃ of oven dry 12 hours; 300 ℃ the calcining 2 hours, naturally cool to room temperature after, impregnated in again in an amount of stannic chloride hydrochloric acid solution, make Sn/GAC=1.25% (weight ratio), stir, after 24 hours, through 105 ℃ the oven dry 12 hours; 300 ℃ of calcinings 2 hours, naturally cool to room temperature after, be reducing agent with hydrogen 250 ℃ of reduction 4 hours down, promptly get the activated-carbon catalyst of bimetallic load.
As cathode and anode, electrode spacing is 2cm with titanium ruthenium net; Reactor is divided into negative and positive two Room with PEM, and the Pd-Sn/GAC catalyst filling is in cathode chamber, and volume is 50mL, porosity 40%.The cathode chamber bottom is provided with water distributor, with the sodium nitrate solution (pH=7.11) of deionized water preparation as experimental water, the nitrate anion initial concentration is 150mg/L, intake from the bottom, flow through catalyst layer from bottom to top, hydraulic detention time (HRT) is 40min, is the successive reaction of carrying out electrical catalyze reduction under the condition of 30mA at electric current.The nitrate removal rate reaches more than 90%.
Claims (6)
1. catalyst of removing nitrate in the water, it is characterized in that, with active carbon (AC) is carrier, on this carrier load have noble metal (A) as a kind of and a kind of base metal (B) in palladium, platinum, gold, rhodium, the ruthenium as copper, tin, indium, zinc, silver particles as active constituent, A: B=1 wherein: (0.125-1), A: AC=1: (20-100) (weight ratio).
2. a method for preparing catalyst for preparing nitrate in the removal water as claimed in claim 1 is characterized in that, the corresponding solubility lead compound with noble metal (A) is dissolved in the hydrochloric acid solution earlier, pretreated active carbon be impregnated in this solution, stir, oven dry, high-temperature calcination, be cooled to room temperature, impregnated in then in the gauge water solution that contains transition metal (B), stir, oven dry, high-temperature calcination is cooled to room temperature, at last with its thorough reduction.
3. according to the described method for preparing catalyst of claim 2, it is characterized in that nitrate, acetate, chlorate that the corresponding solubility lead compound of described noble metal (A) is noble metal (A).
4. according to the described method for preparing catalyst of claim 2, it is characterized in that, described dip time is 12-24 hour, bake out temperature is 105-120 ℃, and drying time is 10-18 hour, and calcining heat is 200-400 ℃, calcination time is 1-3 hour, reduction temperature is 200-300 ℃, and the recovery time is 2-5 hour, and used reducing atmosphere is a hydrogen.
5. the method for nitrate in the catalytic electrochemical reductive water is characterized in that,, separates with PEM between the anode and cathode as cathode and anode with conductive material; Fill bimetallic loaded catalyst described in claim 1 in the cathode chamber, logical direct current makes the nitrate reduction in the cathode chamber solution.
6. according to the method for nitrate in the described a kind of electrochemical reduction water of claim 5, it is characterized in that the current strength that is applied is 20mA-3000mA between anode and cathode, the initial pH value of the water of handling be 3-10.
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Cited By (24)
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|---|---|---|---|---|
| CN102794201A (en) * | 2012-07-18 | 2012-11-28 | 常州大学 | Preparation method of catalyst for promoting conversion of ammonia nitrogen in coking wastewater |
| CN102806092A (en) * | 2012-07-18 | 2012-12-05 | 常州大学 | Preparation method for catalyst for promoting conversion of ammonia nitrogen in pesticide wastewater |
| CN102886271A (en) * | 2012-07-18 | 2013-01-23 | 常州大学 | Method for preparing catalyst for assisting in converting ammonia nitrogen in circuit board sewage |
| FR2993877A1 (en) * | 2012-07-24 | 2014-01-31 | Jean-Francois Bouyssou | Installation, useful for treating an aqueous effluent charged with nitrogen from e.g. aquarium, comprises a reactor comprising catalyst, and a unit for pumping a part of recirculating flow of fluid from fluid chamber towards chamber |
| CN103752270A (en) * | 2014-01-24 | 2014-04-30 | 上海方纶新材料科技有限公司 | Special activated carbon for adsorption separation of chlorine gas and oxygen |
| CN104355369A (en) * | 2014-11-20 | 2015-02-18 | 哈尔滨工业大学 | Device for removing nitrate nitrogen in water and application method of device |
| CN104971739A (en) * | 2015-07-16 | 2015-10-14 | 太原理工大学 | Load type metal catalyst for removing nitrate in underground water and application thereof |
| CN104998640A (en) * | 2015-06-15 | 2015-10-28 | 华南理工大学 | Pd-In/C catalyst and preparation method and application in alcohol oxygenated fuel preparing |
| CN105665024A (en) * | 2016-03-18 | 2016-06-15 | 上海同济科蓝环保设备工程有限公司 | Preparation method of bimetallic catalyst Pd@Cu-BTC removing nitrate in water body and application of bimetallic catalyst |
| CN106554111A (en) * | 2016-11-25 | 2017-04-05 | 南宁市黑晶信息技术有限公司 | A kind of industrial sewage process method |
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| CN107519868A (en) * | 2016-06-20 | 2017-12-29 | 中国科学院金属研究所 | Nanometer palladium-silver catalysis material of nitrate anion and its preparation method and application in a kind of catalysis reductive water |
| CN108467091A (en) * | 2018-04-02 | 2018-08-31 | 沈阳工业大学 | High catalytic activity Cu-Sn-Bi electrodes and its preparation method and application |
| KR20190007754A (en) * | 2017-07-13 | 2019-01-23 | 부산대학교 산학협력단 | A Catalyst for electroreduction of carbon dioxide and An Electrolyzer Cell comprising the same |
| CN109772461A (en) * | 2019-01-25 | 2019-05-21 | 天津大学 | A kind of natural sponge preparation method loading gold silver nanometer particle and its application in terms of being catalyzed p-nitrophenol pollutant |
| CN110980892A (en) * | 2019-10-29 | 2020-04-10 | 东莞理工学院 | Method for removing nitrate nitrogen and nitrite nitrogen in water body by activated cathode nascent hydrogen rapid reduction |
| CN111533220A (en) * | 2020-04-03 | 2020-08-14 | 同济大学 | Novel denitrification system for efficiently removing nitrate in water by utilizing electrocatalytic hydrogen evolution and catalytic hydrogenation and application thereof |
| CN111606495A (en) * | 2020-04-20 | 2020-09-01 | 西安建筑科技大学 | Two-stage catalytic denitrification device and method for removing nitrate in water |
| CN112501640A (en) * | 2020-12-10 | 2021-03-16 | 东莞理工学院 | Battery system for converting nitrate wastewater into ammonia |
| CN112978866A (en) * | 2021-02-09 | 2021-06-18 | 中国科学院生态环境研究中心 | Graphite felt-based bimetallic electrode and preparation method and application thereof |
| CN114011251A (en) * | 2021-12-22 | 2022-02-08 | 南京水滴智能环保装备研究院有限公司 | Conductive film for efficiently removing nitrate in water and preparation method thereof |
| CN114177906A (en) * | 2021-11-09 | 2022-03-15 | 南京大学 | High-efficiency stable photocatalytic denitrification material and preparation method thereof |
| CN114873708A (en) * | 2022-06-08 | 2022-08-09 | 南京大学 | Method for electrocatalytic reduction of N-nitrosodimethylamine |
| CN115125567A (en) * | 2022-07-29 | 2022-09-30 | 江南大学 | Nano alloy electrode for electrocatalytic reduction of nitrate and preparation method and application thereof |
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| CN102806092A (en) * | 2012-07-18 | 2012-12-05 | 常州大学 | Preparation method for catalyst for promoting conversion of ammonia nitrogen in pesticide wastewater |
| CN102886271A (en) * | 2012-07-18 | 2013-01-23 | 常州大学 | Method for preparing catalyst for assisting in converting ammonia nitrogen in circuit board sewage |
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