CN114832813B - Silver-based water treatment monoatomic catalyst and preparation method thereof - Google Patents
Silver-based water treatment monoatomic catalyst and preparation method thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/30—Ion-exchange
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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
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- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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Abstract
The invention discloses a silver-based water treatment monoatomic catalyst and a preparation method thereof. Based on the mass of ASA resin, the mass percentage of zirconium hydrogen phosphate is 5-10%, and the mass percentage of silver source is 0.01-0.1%. The catalyst is environment-friendly and low in cost, and can be used for efficiently catalyzing and reducing water pollutants such as p-nitrophenol, methyl orange, o-nitroaniline and the like.
Description
Technical Field
The invention relates to a silver-based water treatment monoatomic catalyst and a preparation method thereof, belonging to the field of environmental protection catalytic materials and water pollution control.
Background
The p-nitrophenol, methyl orange, o-nitroaniline and the like are used as common dyes, 10% -20% of the common dyes are discharged into the water environment in the use process, and the waste water containing the p-nitrophenol, methyl orange, o-nitroaniline and the like has high toxicity and contains carcinogenic, mutagenic and teratogenic substances; high chromaticity, and can inhibit photosynthesis of plants in an aquatic system: the COD value is high, and the water body is rich in nutrition. Based on the harm, the wastewater containing the dye such as p-nitrophenol, methyl orange, o-nitroaniline and the like is a difficult problem to be treated in the current water treatment technology. Common treatment methods include adsorption, membrane separation, common oxidation, biological methods, etc., but these methods have the disadvantages of complicated process flow, high equipment requirements, high cost, destruction of microenvironment, etc. The catalytic reduction method is a method capable of thoroughly solving the problem of water pollution and even changing waste into valuables, sodium borohydride is utilized to thoroughly reduce p-nitrophenol, methyl orange and o-nitroaniline into chemical products, and the catalytic material can be recycled and reused, so that the secondary pollution to the environment caused by residues in the wastewater is avoided. However, wastewater containing dyes such as p-nitrophenol, methyl orange, o-nitroaniline, etc. is generally alkaline and has a large pH change. In the existing catalytic treatment methods, most catalytic materials only degrade more than 90% of the dye under acidic conditions. Therefore, development of novel catalytic materials with strong pH adaptability and high efficient degradation effect on dyes such as methyl orange, p-nitrophenol, o-nitroaniline and the like is greatly focused by vast scientific researchers, and the catalytic materials are of great significance in treating the dyes such as methyl orange, p-nitrophenol, o-nitroaniline and the like.
Disclosure of Invention
The invention aims to provide a novel catalyst with strong pH adaptability and high-efficiency degradation effect on dyes such as methyl orange, p-nitrophenol, o-nitroaniline and the like aiming at the current situation and problems in the water pollution treatment field.
The technical scheme of the invention is as follows: the invention utilizes the excellent ion exchange performance of zirconium hydrogen phosphate to fix Ag by ion exchange + Then the mixture is mixed with ASA resin to prepare sheet material, and carbonized to avoid zirconium hydrogen phosphate and Ag + Agglomeration is generated under the high-temperature reaction to form agglomerated particles, and finally, the high-temperature in-situ reduction is utilized to eliminate active carbon formed by carbonization of ASA resin, and Ag can be simultaneously reduced + Reduction to monoatomic Ag 0 Thereby reacting to produce the silver-based monoatomic catalyst. The silver-based monoatomic catalyst is developed by taking ASA resin, zirconium hydrogen phosphate and a silver source as main raw materials, and aims to form a novel monoatomic catalyst which has strong pH adaptability and has high-efficiency degradation effect on dyes such as methyl orange, p-nitrophenol, o-nitroaniline and the like.
The specific technical scheme is as follows:
the silver-based water treatment monoatomic catalyst takes silver-loaded zirconium hydrogen phosphate and ASA resin as raw materials, the silver-loaded zirconium hydrogen phosphate and ASA resin are mixed and then are prepared into an ASA material by a melt blending method, the ASA material is carbonized at a high temperature in a nitrogen atmosphere, and finally the silver-based water treatment monoatomic catalyst is generated by reduction in a hydrogen atmosphere; wherein, the mass percentage of zirconium hydrogen phosphate is 5-10 percent based on the mass of ASA resin.
The preparation method of the silver-based water treatment monoatomic catalyst comprises the following steps:
(1) Adsorption of active components
Mixing silver salt with deionized water to form silver salt solution, and placing zirconium hydrogen phosphate in the silver salt solution6-12 h, making zirconium hydrogen phosphate undergo the process of ion exchange in solution so as to fully adsorb Ag + Then taking out and drying to obtain the Ag adsorbed Ag + Zirconium hydrogen phosphate of (a); the method comprises the steps of carrying out a first treatment on the surface of the
(2) Preparation of ASA Material
Based on the quality of ASA resin, the Ag adsorbed by the catalyst prepared in the step (1) + Mixing zirconium hydrogen phosphate and ASA resin, carrying out melt blending for 2-4 hours in an open type plastic mixer at 160-200 ℃, and then pressing the mixture into a sheet with the thickness of 0.5-1.5 mm on a flat vulcanizing machine;
(3) Preparation of the catalyst
Placing the ASA sheet prepared in the step (2) in an atmosphere furnace, and adding N into the ASA sheet 2 High-temperature carbonization is carried out for the protective atmosphere, and then the nitrogen is switched into H with the volume concentration of 1 to 3 percent 2 /N 2 Reduction reaction is carried out to prepare the ZrO 2 Is carrier, ag 0 Monoatomic catalysts as active components.
The method comprises the following steps: in the step (1), the mass ratio of zirconium hydrogen phosphate, silver salt and deionized water is 5-10: 0.01 to 0.1:1 to 30.
The method comprises the following steps: the drying temperature in the step (1) is 80-100 ℃, and the drying time is 8-16 h.
The method comprises the following steps: the silver salt in the step (1) is silver nitrate.
The method comprises the following steps: the high-temperature carbonization temperature in the step (3) is 600-800 ℃, and the carbonization time is 4-8 h.
The method comprises the following steps: the reduction reaction temperature in the step (3) is 600-800 ℃, and the reduction time is 8-12 h. The preparation method comprises the following steps: the reduction reaction temperature is 600-800 ℃, and the reduction time is 8-12 h.
The catalytic reaction conditions and results of the present invention: 1g of silver-based water-treated monoatomic catalyst powder was charged into a catalyst performance evaluation reaction apparatus, wherein ultraviolet-visible light spectrometer model was Microplate reader M, molecular Devices, san Jose, calif. The reaction solution was introduced to evaluate the activity. The concentration of each solution was: 50mL of methyl orange (100 mg/L when needed), 50mL of p-nitrophenol (139 mg/L when needed), 50mL of o-nitroaniline (100 mg/L when needed), 50mL of sodium borohydride (3.78 g/L). The efficiency of the catalyst for removing methyl orange, p-nitrophenol and o-nitroaniline in 5min under normal temperature and normal pressure is 100 percent.
The beneficial effects are that:
the catalyst prepared by the invention can efficiently catalyze and reduce water pollutants such as p-nitrophenol, methyl orange, o-nitroaniline and the like. Compared with the prior art, the catalyst system utilizes zirconium hydrogen phosphate with high specific surface area and excellent ion exchange performance to adsorb active component precursors, then utilizes ASA resin to fix the active component precursors, avoids active component or carrier agglomeration, and then utilizes in-situ reduction to prepare the silver-based monoatomic catalyst. The silver-based monoatomic catalyst disclosed by the invention is environment-friendly in components, simple in preparation process, low in cost, high in cost performance, and high in application and popularization value and wide in market prospect.
Description of the drawings:
FIG. 1 is a schematic view of a reaction apparatus for evaluating the performance of the catalysts used in examples 1 to 3 and comparative example 1;
FIG. 2 is a graph of the activity data of the catalyst prepared in example 1;
FIG. 3 is a graph of the activity data of the catalyst prepared in example 2;
FIG. 4 is a graph of the activity data of the catalyst prepared in example 3;
FIG. 5 is a graph showing the activity data of the catalyst prepared in comparative example 1;
FIG. 6 is a graph showing the activity data of the catalyst prepared in comparative example 2.
Detailed Description
The invention is further illustrated below with reference to examples, but the scope of the invention is not limited thereto: example 1
(1) Adsorption of active components
Weighing 0.01g of silver nitrate and 1g of deionized water, mixing to form a silver salt dilute solution, placing 5g of zirconium hydrogen phosphate in the silver salt dilute solution for adsorption for 6 hours, performing ion exchange on the zirconium hydrogen phosphate in the solution, and fully adsorbing Ag + Then taking out and drying at 80 ℃ for 16 hours to obtain the Ag adsorbed on the silver + Zirconium hydrogen phosphate of (a);
(2) Preparation of ASA Material
Weighing 100g of ASA resin and the Ag adsorbed by the ASA resin prepared in the step (1) + Is melt blended for 2 hours in an open mill (SK-160B, shanghai rubber works) at 180 ℃ and then pressed into 1mm sheet in a press vulcanizer (XLB-D350×350×2, shanghai first rubber works);
(3) Preparation of the catalyst
Placing the ASA sheet prepared in the step (2) in an atmosphere furnace, and adding N into the ASA sheet 2 Carbonizing for 8H at 600 ℃ in a protective atmosphere, and switching nitrogen to H with volume concentration of 1% 2 /N 2 And in-situ reduction reaction is carried out for 12 hours at 600 ℃ to prepare the ZrO 2 Is carrier, ag 0 A monoatomic catalyst as an active component;
(4) Catalytic Activity test
1g of silver-based water-treated monoatomic catalyst powder was charged into a catalyst performance evaluation reaction apparatus, in which an ultraviolet-visible light spectrometer model Microplate reader M, molecular Devices, san Jose, CA was added to the reaction solution for activity evaluation. The concentration of each solution was: 50mL of methyl orange (100 mg/L, as needed), 50mL of sodium borohydride (3.78 g/L). As shown in FIG. 2, the catalyst has the methyl orange removal efficiency reaching 100% in 4.5min at normal temperature and pressure, namely the color of the solution is changed from yellow to colorless and transparent, and the corresponding spectrum peak (about 460 nm) of the methyl orange is basically disappeared.
Example 2:
(1) Adsorption of active components
Weighing 0.1g of silver nitrate and 30g of deionized water, mixing to form a silver salt dilute solution, placing 10g of zirconium hydrogen phosphate in the silver salt dilute solution for adsorption for 6 hours, performing ion exchange on the zirconium hydrogen phosphate in the solution, and fully adsorbing Ag + Then taking out and drying at 100deg.C for 16h to obtain Ag adsorbed thereon + Zirconium hydrogen phosphate of (a);
(2) Preparation of ASA Material
Weighing 100g of ASA resin and the Ag adsorbed by the ASA resin prepared in the step (1) + Zirconium hydrogen phosphate mixing at 180℃in an open mill (SK-160B, shanghai rubber machine)Factory) was melt blended for 4 hours, and then pressed into 1 mm-sized sheets on a flat vulcanizing machine (XLB-d350×350×2, shanghai first rubber plant);
(3) Preparation of the catalyst
Placing the ASA sheet prepared in the step (2) in an atmosphere furnace, and adding N into the ASA sheet 2 Carbonizing for 4H at 800 ℃ in a protective atmosphere, and switching nitrogen to H with 3% volume concentration 2 /N 2 And in-situ reduction reaction is carried out for 8 hours at 800 ℃ to prepare the ZrO 2 Is carrier, ag 0 A monoatomic catalyst as an active component;
(4) Catalytic Activity test
1g of silver-based water-treated monoatomic catalyst powder was charged into a catalyst performance evaluation reaction apparatus, wherein ultraviolet-visible light spectrometer model was Microplate reader M, molecular Devices, san Jose, calif. The reaction solution was added to evaluate the activity. The concentration of each solution was: 50mL of p-nitrophenol (139 mg/L, as needed), 50mL of sodium borohydride (3.78 g/L). As shown in FIG. 3, the efficiency of removing the p-nitrophenol by the catalyst reaches 100% in 4min at normal temperature and pressure, namely the color of the solution is changed from yellow to colorless and transparent, and the corresponding spectrum peak (about 400 nm) of the p-nitrophenol is basically disappeared.
Example 3:
(1) Adsorption of active components
Weighing 0.1g of silver nitrate and 10g of deionized water, mixing to form a silver salt dilute solution, placing 5g of zirconium hydrogen phosphate in the silver salt dilute solution for adsorption for 12 hours, and performing ion exchange on the zirconium hydrogen phosphate in the solution to fully adsorb Ag + Then taking out and drying at 100deg.C for 8 hr to obtain Ag adsorbed thereon + Zirconium hydrogen phosphate of (a);
(2) Preparation of ASA Material
Weighing 100g of ASA resin and the Ag adsorbed by the ASA resin prepared in the step (1) + Is melt-blended in an open mill (SK-160B, shanghai rubber works) at 180℃for 4 hours, and is subsequently pressed into 1 mm-thick sheets in a press vulcanizer (XLB-D350X 350X 2, shanghai first rubber works);
(3) Preparation of the catalyst
Placing the ASA sheet prepared in the step (2) in an atmosphere furnace, and adding N into the ASA sheet 2 Carbonizing for 4H at 800 ℃ in a protective atmosphere, and switching nitrogen to H with 3% volume concentration 2 /N 2 And in-situ reduction reaction is carried out for 12 hours at 600 ℃ to prepare the ZrO 2 Is carrier, ag 0 A monoatomic catalyst as an active component;
(4) Catalytic Activity test
1g of silver-based water-treated monoatomic catalyst powder was charged into a catalyst performance evaluation reaction apparatus, wherein ultraviolet-visible light spectrometer model was Microplate reader M, molecular Devices, san Jose, calif. The reaction solution was added to evaluate the activity. The concentration of each solution was: 50mL of o-nitroaniline (100 mg/L, as needed), 50mL of sodium borohydride (3.78 g/L). As shown in FIG. 4, the catalyst has the efficiency of removing the o-nitroaniline within 5min at normal temperature and pressure reaching 100 percent, namely the color of the solution is changed from yellow to colorless and transparent, and the corresponding spectrum peak (about 415 nm) of the o-nitroaniline is basically disappeared.
Comparative example 1
(1) Preparation of the catalyst
The conditions were the same as in example 2 except that ASA resin was not added during the preparation of ASA material;
(2) Catalytic Activity test
1g of a silver-based catalyst powder was charged into a catalyst performance evaluation reaction apparatus, in which ultraviolet-visible light spectrometer model was Microplate reader M, molecular Devices, san Jose, calif. The reaction solution was added to evaluate the activity. 50mL of p-nitrophenol (139 mg/L, as needed), 50mL of sodium borohydride (3.78 g/L). As shown in fig. 5, the efficiency of removing methyl orange by the catalyst reaches about 100% in 15min at normal temperature and pressure;
(3) Contrast effect
As can be seen from comparison with example 1, if ASA resin is not mixed to form ASA sheet during the preparation of the catalyst, the ASA sheet is directly reduced at high temperature, the active components of the catalyst are agglomerated, and single atoms are difficult to generate, so that the catalytic effect is obviously reduced.
Comparative example 2
(1) Preparation of the catalyst
Except that zirconium hydrogen phosphate is replaced with anatase TiO 2 Other conditions were the same as in example 3;
(2) Catalytic Activity test
1g of silver-based water-treated monoatomic catalyst powder was charged into a catalyst performance evaluation reaction apparatus, wherein ultraviolet-visible light spectrometer model was Microplate reader M, molecular Devices, san Jose, calif. The reaction solution was added to evaluate the activity. The concentration of each solution was: 50mL of o-nitroaniline (100 mg/L, as needed), 50mL of sodium borohydride (3.78 g/L). As shown in fig. 6, the efficiency of removing o-nitroaniline by the catalyst reaches 100% in 18min at normal temperature and pressure;
(3) Contrast effect
As can be seen by comparing with example 3, the catalyst is prepared by replacing zirconium hydrogen phosphate with anatase TiO 2 Although TiO 2 Can absorb all silver ions in the silver source solution, thereby leading Ag in the catalyst to be 0 The content is higher than in example 3, but also because of TiO 2 It is the adsorption of silver ions and not the displacement of cations in the support that makes it difficult to achieve in situ reduction of silver ions, thereby generating monoatoms. Thus, the catalytic effect is significantly reduced compared to example 3.
Claims (7)
1. A silver-based water treatment monoatomic catalyst, characterized in that: the catalyst takes silver-loaded zirconium hydrogen phosphate and ASA resin as raw materials, the silver-loaded zirconium hydrogen phosphate and ASA resin are mixed and then are prepared into ASA material by a melt blending method, the ASA material is carbonized at high temperature in nitrogen atmosphere, and finally the ASA material is reduced in hydrogen atmosphere to generate a silver-based water treatment monoatomic catalyst; the quality percentage of zirconium hydrogen phosphate is 5% -10% based on the quality of ASA resin.
2. A method for preparing the silver-based water treatment monoatomic catalyst according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) Adsorption of active components
Removing silver saltMixing the sub water to form a silver salt dilute solution, placing zirconium hydrogen phosphate in the silver salt dilute solution for 6-12 h, and performing ion exchange on the zirconium hydrogen phosphate in the solution to fully adsorb Ag + Then taking out and drying to obtain the Ag adsorbed Ag + Zirconium hydrogen phosphate of (a);
(2) Preparation of ASA Material
Based on the quality of ASA resin, the Ag adsorbed by the catalyst prepared in the step (1) + Mixing zirconium hydrogen phosphate and ASA resin, carrying out melt blending for 2-4 hours in an open type plastic mixer at 160-200 ℃, and then pressing the mixture into a sheet with the thickness of 0.5-1.5 mm on a flat vulcanizing machine;
(3) Preparation of the catalyst
Placing the sheet material obtained in the step (2) in an atmosphere furnace, and using N 2 High-temperature carbonization is carried out for the protective atmosphere, and then nitrogen is switched into H with the volume concentration of 1-3 percent 2 /N 2 Reduction reaction is carried out to prepare the ZrO 2 Is carrier, ag 0 Monoatomic catalysts as active components.
3. The method for preparing the catalyst according to claim 2, wherein: in the step (1), the mass ratio of zirconium hydrogen phosphate, silver salt and deionized water is 5-10: 0.01 to 0.1: 1-30.
4. The method for preparing the catalyst according to claim 2, wherein: the drying temperature in the step (1) is 80-100 ℃, and the drying time is 8-16 h.
5. The method for preparing the catalyst according to claim 2, wherein: the silver salt in the step (1) is silver nitrate.
6. The method for preparing the catalyst according to claim 2, wherein: the high-temperature carbonization temperature in the step (3) is 600-800 ℃, and the carbonization time is 4-8 hours.
7. The method for preparing the catalyst according to claim 2, wherein: the reduction reaction temperature in the step (3) is 600-800 ℃, and the reduction time is 8-12 h.
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| US20150238935A1 (en) * | 2014-02-21 | 2015-08-27 | Umm Al-Qura University | METHOD FOR SYNTHESIZING SILVER NANOPARTICLES ON TiO2 USING HYBRID POLYMERS |
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| CN105506767A (en) * | 2015-12-01 | 2016-04-20 | 东华大学 | Antibacterial polypropylene fiber comprising mesoporous zirconium phosphate loaded nano-Ag and preparation method of antibacterial polypropylene fiber |
| CN105921173A (en) * | 2016-04-21 | 2016-09-07 | 河南大学 | Nano-silver composite textile catalyst and application thereof |
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