CN111036221A - Preparation method of metal supported catalyst for removing ammonia nitrogen in water by moderate catalytic ozonation - Google Patents
Preparation method of metal supported catalyst for removing ammonia nitrogen in water by moderate catalytic ozonation Download PDFInfo
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- CN111036221A CN111036221A CN201911301188.2A CN201911301188A CN111036221A CN 111036221 A CN111036221 A CN 111036221A CN 201911301188 A CN201911301188 A CN 201911301188A CN 111036221 A CN111036221 A CN 111036221A
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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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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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
- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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Abstract
The invention provides a preparation method of a metal supported catalyst for removing ammonia nitrogen in water by moderate catalytic ozonation, which comprises the following preparation steps: step (1): the catalyst carrier is activated carbon, the activated carbon is washed by deionized water for 3 times, then soaked for 8 to 12 hours, filtered at 100 to 105 ℃ and dried for 12 hours; step (2): adding the pretreated activated carbon into a mixed salt solution of magnesium sulfate, cobalt nitrate and cerium nitrate with the concentration of 0.1-1 mol/L, wherein the molar ratio of the magnesium sulfate to the cobalt nitrate to the cerium nitrate is 4:1: 0.1-2, stirring for 2 hours, and standing for 6-8 hours; and (3) stirring the mixed salt solution in the step (2), slowly dripping ammonia water until the pH value reaches 8-9, filtering and cleaning for 3 times, drying for 2-8 hours at 100-105 ℃, and calcining for 3-5 hours at 300-600 ℃ to obtain the composite tri-metal loaded activated carbon catalyst. By applying the technical scheme, the ammonia nitrogen can be efficiently removed, and most of the removed ammonia nitrogen can be converted into the catalyst of nitrogen.
Description
Technical Field
The invention relates to the technical field of environmental engineering water treatment, in particular to a preparation method of a metal supported catalyst for removing ammonia nitrogen in water by moderate catalytic ozonation.
Background
With the continuous development of urban socioeconomic and the increasing population, the pollutant emission is increased. The urban inland rivers flow through urban blocks, and bear the functions of flood running and partial sewage collection, and due to a plurality of reasons such as construction and management systems, the urban inland rivers are generally in the condition that rainwater and sewage are incompletely shunted and partial rainwater and sewage are mixed and discharged into natural water bodies. In addition, the hydrodynamic conditions of part of the river water are poor, the pollutant carrying capacity is serious, the environmental capacity is low, and the water is black and smelly, so that the environmental problems caused by the pollution are more and more obvious. The evaluation indexes of the urban black and odorous water body classification mainly comprise transparency, Dissolved Oxygen (DO), oxidation-reduction potential (ORP) and ammonia Nitrogen (NH)3-N). Wherein, the effective removal of ammonia nitrogen is a key factor for restricting whether the black and odorous water body reaches the standard. Therefore, aiming at the treatment target of the black and odorous water body, the development of a water environment treatment technology capable of effectively removing ammonia nitrogen is urgent. Common methods for removing ammonia nitrogen include adsorption, chemical oxidation and biochemical methods. The adsorption method has convenient use, can achieve better ammonia nitrogen treatment effect by using materials with high adsorption capacity, is beneficial to ammonia nitrogen recovery, but the reproducibility and the safety of the adsorption material need to be improvedFurther study was carried out. The biological method mainly utilizes biological metabolic activity to oxidize ammonia nitrogen into nitrate nitrogen through nitration and denitrification reaction and then reduce the nitrate nitrogen into nitrogen to achieve the aim of removing ammonia, has the advantages of low energy consumption and the like, and has the defects of large occupied area of treated structures, large initial investment, long start-up period, long hydraulic retention time and the like. The chemical oxidation method has the problems of no selection and excessive oxidation, ammonia nitrogen is oxidized into nitrate nitrogen or nitrite nitrogen, a nitrogen source is not really removed from a water body, and the total nitrogen concentration is still high. Therefore, the finding of a moderate oxidation technology to convert ammonia nitrogen in water into nitrogen in one step is a hotspot and difficulty of future research. The ammonia nitrogen moderate catalytic oxidation technology is that the ammonia nitrogen in water is only oxidized into nitrogen by selecting a proper catalyst and controlling the oxidation degree of an oxidant, thereby realizing the removal of the ammonia nitrogen from the water in a gas form. The common method such as the photocatalysis technology has the advantages of low treatment cost and high selectivity of converting into nitrogen; but the reaction rate is slow, and the equipment cost is high; the requirements on the quality and pH of the treated water are high, and are generally more than 9. The electrochemical method has the advantages that chlorine free radicals can directly oxidize ammonia nitrogen into nitrogen, but sodium chloride is required to be added as electrolyte, the application range is limited, and the treatment amount is limited. The method for adding chlorine at the break point has the advantages of convenient use, good treatment effect and better selectivity (N)2) However, the cost of the treatment reagent is high, the applicable pH range is small, and the breaking point controllable operation requirement is high. The ozone catalytic oxidation method has strong oxidability and wide application range, and can select a catalyst with high selectivity to realize the conversion of most of ammonia nitrogen to nitrogen. And the catalyst is expected to be applied to actual engineering by enhancing the treatment effect and the mechanical and chemical stability of the catalyst.
In recent years, most of researches on catalysts for removing ammonia nitrogen through ozone catalytic oxidation are single metal oxides, double metal oxides and supported catalysts. According to investigation, some metal oxides (such as MgO) can have high ammonia nitrogen removal rate under the action of ozone, but most of the removed ammonia nitrogen is converted into nitrate nitrogen; while some metal oxides (e.g. Co)3O4) Although most of the removed ammonia nitrogen can be converted into nitrogen, the ammonia nitrogen removal efficiency is very low, and the ammonia nitrogen removal rate is only 20-30% after the reaction is carried out for 1-2h. In addition, the rare earth element Ce has typical metal characteristics, can lose the electron and show the valence of +3 or +4, and is accompanied with electron gain and loss in the conversion of different valence states, so that the Ce has high activity as a catalyst, and the rare earth element Ce can improve the activity of the catalyst and play a role in stabilizing the crystal structure so as to improve the mechanical strength of the catalyst. However, the activity of cerium oxide and the cerium/cobalt or cerium/magnesium bimetallic oxide to the catalytic removal of ammonia nitrogen by ozone is low, and the catalytic activity of the cobalt, magnesium and cerium trimetallic oxide doped with cerium is greatly reduced compared with that of the cobalt/magnesium bimetallic oxide. And any two metal oxides of cobalt, magnesium and cerium are loaded on the carrier active carbon to obtain the bimetal composite oxide modified active carbon, which has low efficiency for moderately catalyzing and oxidizing ammonia nitrogen, and most of the bimetal composite oxide modified active carbon is still excessively oxidized into nitrate nitrogen.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a metal supported catalyst for moderately catalyzing and ozonizing to remove ammonia nitrogen in water, which can realize high-efficiency ammonia nitrogen removal and can convert most of removed ammonia nitrogen into nitrogen.
In order to solve the technical problem, the invention provides a preparation method of a metal supported catalyst for moderately catalyzing ozonization to remove ammonia nitrogen in water, which is characterized by comprising the following preparation steps:
step (1): activation pretreatment of the catalyst carrier: the catalyst carrier is activated carbon, the activated carbon is washed by deionized water for 3 times, then soaked for 8 to 12 hours, filtered at 100 to 105 ℃ and dried for 12 hours;
step (2): adding the pretreated activated carbon into a mixed salt solution of magnesium sulfate, cobalt nitrate and cerium nitrate with the concentration of 0.1-1 mol/L, wherein the molar ratio of the magnesium sulfate to the cobalt nitrate to the cerium nitrate is 4:1: 0.1-2, stirring for 2 hours, and standing for 6-8 hours;
and (3) stirring the mixed salt solution in the step (2), slowly dripping ammonia water until the pH value reaches 8-9, ageing for 30 minutes, filtering and cleaning for 3 times, drying for 2-8 hours at 100-105 ℃, and calcining for 3-5 hours at 300-600 ℃ to obtain the composite trimetal loaded activated carbon catalyst.
In a preferred embodiment, the mixed salt solution in step (2) is prepared by measuring different volumes of 1mol/L magnesium sulfate solution, 1mol/L cobalt nitrate solution and 1mol/L cerium nitrate solution and mixing.
In a preferred embodiment, the amount of activated carbon added is 20 g/L.
In a preferred embodiment, the composite trimetal-loaded activated carbon catalyst is added into an ammonium chloride reaction solution, 50mg/L ozone gas is introduced, and the reaction is carried out at the temperature of 20-25 ℃ for 1-3 hours, wherein the ammonia nitrogen concentration in the ammonium chloride reaction solution is 20-50 mg/L, and the initial pH value is 6-9.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the invention provides a preparation method of a metal supported catalyst for removing ammonia nitrogen in water by moderate catalytic ozonation.
(2) The catalyst carrier is activated carbon, and the combined process of the activated carbon and the ozone is mature, so that the catalyst is beneficial to future practical application.
(3) The catalyst prepared by the invention is suitable for neutral pH, can be directly used for removing ammonia nitrogen in most natural water bodies and sewage, and does not need to adjust the pH value.
Drawings
FIG. 1 is an SEM image of an unsupported activated carbon in a preferred embodiment of the invention;
fig. 2 is an SEM image of a composite trimetallic supported catalyst in a preferred embodiment of the invention.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
Example 1:
a preparation method of a metal supported catalyst for removing ammonia nitrogen in water by moderate catalytic ozonation, which refers to figures 1 to 2; the preparation steps are as follows:
step (1): activation pretreatment of the catalyst carrier: the catalyst carrier is powdered activated carbon, and the adding amount of the powdered activated carbon is 20 g/L; washing the powdered activated carbon with deionized water for 3 times, then soaking for 8-12 h, filtering at 100-105 ℃ and drying for 12 h;
step (2): adding the pretreated powdered activated carbon into a mixed salt solution of magnesium sulfate, cobalt nitrate and cerium nitrate with the concentration of 0.1-1 mol/L, wherein the molar ratio of the magnesium sulfate to the cobalt nitrate to the cerium nitrate is 4:1: 0.1-2, stirring for 2 hours, and standing for 6-8 hours; the mixed salt solution is prepared by measuring magnesium sulfate solutions with different volumes and concentrations of 1mol/L, 1mol/L cobalt nitrate solution and 1mol/L cerium nitrate solution and mixing;
and (3) stirring the mixed salt solution in the step (2), slowly dripping ammonia water until the pH value reaches 8-9, ageing for 30 minutes, filtering and cleaning for 3 times, drying for 2-8 hours at 100-105 ℃, and calcining for 3-5 hours at 300-600 ℃ to obtain the composite trimetal loaded activated carbon catalyst.
Adding the composite trimetal loaded activated carbon catalyst into an ammonium chloride reaction solution, introducing 50mg/L ozone gas, reacting for 1-3 hours at the temperature of 20-25 ℃, wherein the ammonia nitrogen concentration in the ammonium chloride reaction solution is 20-50 mg/L, and the initial pH value is 6-9.
Specifically, in this example, 50mg/L of an ammonium chloride reaction solution was prepared from ammonium chloride under normal temperature and pressure conditions, 200mL of the prepared ammonium chloride reaction solution was taken out of the reactor, 0.2g of the composite metal oxide-modified activated carbon obtained in example 1 was further added, the initial pH of the mixed solution was 8.14, and ozone was introduced for 2 hours. Meanwhile, a blank experiment is set under the same conditions, namely, ozone is independently introduced for 2 hours without adding a catalyst. And testing the concentrations of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen after the reaction.
The experimental results are as follows: the ammonia nitrogen removal rate was 72.56%, wherein 87.17% of the ammonia nitrogen was converted into nitrogen. While the ammonia nitrogen removal rate of the ozone without the catalyst is only 8.70 percent, and only 25.42 percent of ammonia nitrogen in the ozone is converted into nitrogen.
Example 2
In this embodiment, under normal temperature and pressure conditions, 50mg/L of ammonium chloride reaction solution is prepared from ammonium chloride, 200mL of the prepared ammonium chloride reaction solution is taken out of the reactor, 0.2g of the composite metal oxide modified activated carbon obtained in example 1 is further added, the initial pH of the mixed solution is 8.09, and ozone is introduced for 3 hours. Meanwhile, a blank experiment is set under the same condition, namely, the ozone is independently introduced for 3 hours without adding the catalyst. And testing the concentrations of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen after the reaction.
The experimental results are as follows: the ammonia nitrogen removal rate was 89.18%, wherein 93.33% of the ammonia nitrogen was converted to nitrogen. While the removal rate of ammonia nitrogen of ozone without adding a catalyst is only 15.70 percent, and only 33.14 percent of ammonia nitrogen in the ozone is converted into nitrogen.
Example 3
In this embodiment, under normal temperature and pressure conditions, 50mg/L of ammonium chloride reaction solution is prepared from ammonium chloride, 200mL of the prepared ammonium chloride reaction solution is taken out of the reactor, 0.4g of the composite metal oxide modified activated carbon obtained in example 1 is further added, the initial pH of the mixed solution is 8.11, and ozone is introduced for 2 hours. Meanwhile, a blank experiment is set under the same condition, namely, the ozone is independently introduced for 2 hours without adding the catalyst. And testing the concentrations of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen after the reaction.
The experimental results are as follows: the ammonia nitrogen removal rate is 85.15%, wherein 89.78% of ammonia nitrogen is converted into nitrogen. While the removal rate of ammonia nitrogen of ozone without adding a catalyst is only 10.12%, and only 23.47% of ammonia nitrogen in the ozone is converted into nitrogen.
Example 4
In this embodiment, under normal temperature and pressure conditions, 20mg/L of ammonium chloride reaction solution is prepared from ammonium chloride, 200mL of the prepared ammonium chloride reaction solution is taken out of the reactor, 0.2g of the composite metal oxide modified activated carbon obtained in example 1 is further added, the initial pH of the mixed solution is 8.30, and ozone is introduced for 2 hours. Meanwhile, a blank experiment is set under the same condition, namely, the ozone is independently introduced for 2 hours without adding the catalyst. And testing the concentrations of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen after the reaction.
The experimental results are as follows: the ammonia nitrogen removal rate is 87.21%, wherein 86.11% of ammonia nitrogen is converted into nitrogen. While the ammonia nitrogen removal rate of the ozone without the catalyst is only 18.69%, and only 27.48% of ammonia nitrogen in the ozone is converted into nitrogen.
The above description is only a preferred embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any person skilled in the art can make insubstantial changes in the technical scope of the present invention within the technical scope of the present invention, and the actions infringe the protection scope of the present invention are included in the present invention.
Claims (4)
1. A preparation method of a metal supported catalyst for moderately catalyzing and ozonizing to remove ammonia nitrogen in water is characterized by comprising the following preparation steps:
step (1): activation pretreatment of the catalyst carrier: the catalyst carrier is activated carbon, the activated carbon is washed by deionized water for 3 times, then soaked for 8 to 12 hours, filtered at 100 to 105 ℃ and dried for 12 hours;
step (2): adding the pretreated activated carbon into a mixed salt solution of magnesium sulfate, cobalt nitrate and cerium nitrate with the concentration of 0.1-1 mol/L, wherein the molar ratio of the magnesium sulfate to the cobalt nitrate to the cerium nitrate is 4:1: 0.1-2, stirring for 2 hours, and standing for 6-8 hours;
and (3) stirring the mixed salt solution in the step (2), slowly dripping ammonia water until the pH value reaches 8-9, ageing for 30 minutes, filtering and cleaning for 3 times, drying for 2-8 hours at 100-105 ℃, and calcining for 3-5 hours at 300-600 ℃ to obtain the composite trimetal loaded activated carbon catalyst.
2. The method for preparing the metal supported catalyst for moderately catalyzing and ozonizing removal of ammonia nitrogen in water according to claim 1, wherein the mixed salt solution in the step (2) is prepared by measuring magnesium sulfate solutions with different volumes and concentrations of 1mol/L, 1mol/L cobalt nitrate solution and 1mol/L cerium nitrate solution and mixing.
3. The method for preparing the metal supported catalyst for moderately catalyzing and ozonizing ammonia nitrogen in water according to claim 1, wherein the adding amount of the activated carbon is 20 g/L.
4. The method for preparing the metal-supported catalyst for moderately catalyzing and ozonizing ammonia nitrogen in water according to claim 1, wherein the composite trimetal-supported activated carbon catalyst is added into an ammonium chloride reaction solution, 50mg/L ozone gas is introduced, and the reaction is carried out at 20-25 ℃ for 1-3 hours, wherein the ammonia nitrogen concentration in the ammonium chloride reaction solution is 20-50 mg/L, and the initial pH value is 6-9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113371941A (en) * | 2021-06-23 | 2021-09-10 | 中南大学 | Application of microbial carbon-loaded metal ammonia nitrogen oxidation ozone catalyst in degradation of high-concentration ammonia nitrogen wastewater |
| CN115739101A (en) * | 2022-09-07 | 2023-03-07 | 南京大学 | Controllable preparation method of bimetal supported ozone catalyst and water treatment application thereof |
| CN115739101B (en) * | 2022-09-07 | 2024-05-28 | 南京大学 | Controllable preparation method of bimetal supported ozone catalyst and water treatment application thereof |
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