CN103041856A - Novel adsorption catalyst for nitrogen removal of sewage and preparation method thereof - Google Patents
Novel adsorption catalyst for nitrogen removal of sewage and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a novel adsorption catalyst for nitrogen removal of sewage and a preparation method thereof. The preparation method comprises the following steps of: firstly, mixing FeC13 solution with tannin solution according to a certain proportion, and regulating pH of the mixed solution to 7.0 by adding NaHCO3; then carrying out centrifuging, distilled water washing and recentrifuging on the neutral mixed solution; and carrying out freeze drying on solid matters obtained by centrifugal separation so as to obtain a novel ferric tannate adsorption catalysis material. The novel adsorption catalyst for the nitrogen removal of the sewage and the preparation method thereof have the advantages of simplicity in operation, economy, applicability and the like; due to a prepared ferric tannate adsorption catalyst, NH4<+>- and NO2<->-N in water can be simultaneously absorbed and converted into N2; and the adsorption catalyst has the advantages of rich pore structures, high stability, good adsorption and nitrogen removal catalyzing effects and wide applicable range and can be widely applied to the nitrogen removal of the sewage.
Description
Technical field
The invention belongs to sewage treatment area, be specifically related to a kind of Novel adsorption Catalysts and its preparation method for sewage water denitrification.
Background technology
Containing the nutriments such as ammonia nitrogen, nitrous acid nitrogen in the sewage, is the one of the main reasons that causes the receiving water body eutrophication.Sewage denitrification method comprises physico-chemical process and biochemical process at present.Biological denitrification method is subject to the impact of the conditions such as the C/N of sewage and temperature, and the microorganism incubation time is long, the denitrification reaction process is slow, and required bioreactor volume is larger, and energy consumption is higher.Physical-chemical process mainly comprises absorption method and catalysis method.Need the problem of regenerating after simple absorption method exists adsorbent saturated, and there is the high in cost of production problem in simple catalysis method.Therefore, developing the Novel adsorption catalyst that has simultaneously absorption and catalysis is one of key method that solves the wastewater efficient Denitrogenation.
Have at present with Fe, Fe
2+, Fe
3+Remove NH
4 +-N, NO
3 --N, NO
2 -The adsoption catalysis method of-N, but take the Fe element of these forms as catalyst, exist the converted product of Fe to separate difficult problem with water outlet.Find in the research that tannic acid has the polyphenol hydroxyl structure, two adjacent phenolic hydroxyl groups can form stable five-membered ring chelate-ferric tannate (water insoluble) with form and the metal ion of negative oxygen ion.The chemical stability of ferric tannate is good, can adsorb simultaneously NH
4 +-N and NO
2 --N, and catalysis its be converted into N
2, be a kind of adsoption catalysis denitrogenation material with large development potentiality.Therefore, develop a kind of novel ferric tannate adsoption catalyst that is used for sewage water denitrification, efficient processing nitrogenous effluent, control water are polluted and has great importance.
Summary of the invention
It is wide to the purpose of this invention is to provide a kind of applicability, and technique is simple, the Novel adsorption Catalysts and its preparation method that is used for the sewage water denitrification processing of easy operating.
The described Novel adsorption catalyst of processing for sewage water denitrification is ferric tannate;
The preparation method of described Novel adsorption catalyst for sewage water denitrification comprises following steps:
1) tannic acid and FeCl
3Reaction: with tannic acid and FeCl
36H
2O all is formulated as the solution of same concentrations, according to certain volume ratio, while stirring with FeCl
3Solution joins in the tannic acid solution, fully reacts 10～20min;
Described tannic acid and FeCl
3Solution concentration is 0.001～0.02mol/L;
Described tannic acid and FeCl
3Volume ratio during solution reaction is 1: 40～1: 10;
Contain black-and-blue floccule in the described reacted mixed liquor;
2) NaHCO
3The preparation of solution: with NaHCO
3Solid is dissolved in the distilled water, is mixed with the NaHCO that concentration is 0.65mol/L
3Solution;
3) NaHCO conditioned reaction pH of mixed value: with step 2)
3Solution slowly joins step with dropper
1) tannic acid and FeCl in
3In the reacted mixed liquor that contains black-and-blue floccule, slowly add while stirring and measure the pH value of mixed liquor with pH meter, when the pH of mixed liquor value reaches 7.0, stop dropping;
4) once centrifugal: with step 3) in the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000-4000rpm in centrifuge;
5) black-and-blue sediment obtains containing black-and-blue sedimentary mixed liquor with distilled water washing 3-4 time washing: with step 4);
The distillation water yield of adding during described each washing is black-and-blue sedimentary 2-5 times;
6) contain the centrifugal 5min of black-and-blue sedimentary mixed liquor 3000-4000rpm in centrifuge secondary centrifuging: with step 5) after the washing;
7) the black-and-blue sediment that obtains after centrifugal drying: with step 6) is-40～-50 ℃ of dry 20-24h in vacuum freeze drier, drying pressure is 40Pa, can obtain dry ferric tannate sample, dried sample places normal temperature preservation in the sealing bag.
Beneficial effect:
The present invention compared with prior art, its remarkable advantage is: (1) novel denitrogenation adsoption catalyst ferric tannate is by tannic acid and FeCl
3The preparation of generation chemical reaction, the Fe with catalytic activity is loaded on the tannic acid, and the ferric tannate of formation can adsorb NH simultaneously
4 +-N, NO
2 --N.(2) strength and stability that self has of Novel adsorption catalyst ferric tannate can not be discharged into harmful substance in the water body adsorbent and forms secondary pollution, and the adsorbent advantages of good adsorption effect, in absorption, but catalyzing N H
4 +-N and NO
2 -The N reaction generates nitrogen, therefore can utilize for a long time.(3) NH in the waste water
4 +-N, NO
2 -After-N was adsorbed by ferric tannate, both reacted and generate N
2Speed significantly raise.
Novel adsorption catalyst---ferric tannate absorption property and interpolation the relationship between quantities
Ferric tannate has abundant pore structure, contains a large amount of hydroxyls in its molecular structure, has good absorption property.Under the same condition of water quality, the dosage of ferric tannate affects its absorption NH
4 +The power of-N performance.
Get 0.1g, 0.5g, the 1.0g ferric tannate is added to respectively in the 50ml waste water, NH in the water sample
4 +-N concentration is 408mg/L.The tool plug triangular flask that will contain aggregate sample places shaking table, acts on 180min under 35 ℃, 200rpm condition, gets water sample one time every 30min, with NH in the nessler reagent colorimetric method for determining water sample
4 +The variation of-N content.Find that by measuring along with the increase of ferric tannate dosage, ferric tannate is to NH
4 +The equilibrium adsorption capacity of-N obviously reduce, reach the needed time of adsorption equilibrium shorten afterwards first remain unchanged, denitrification percent obviously improves.30.5,11.5,8.7mg/g wherein, when the dosage of ferric tannate was respectively 0.1g, 0.5g, 1.0g, its equilibrium adsorption capacity was respectively:; 90,30,30min reaching the needed time of adsorption equilibrium is respectively:; Denitrification percent when reaching adsorption equilibrium is respectively: 15.9%, 28.4%, 43.2%.
Novel adsorption catalyst---the relation of ferric tannate absorption property and wastewater temperature
Fe
3+Facile hydrolysis, in water with the form (Fe (OH) of multinuclear hydroxyl compound
2+, Fe (OH)
2 +, Fe
3(OH)
2 5+) exist, so easier absorption NO
2 --N.Under the equal adsorbent dosage condition, the temperature effect ferric tannate of waste water is to NO
2 -The absorption property of-N.
Get the 0.1g ferric tannate and be added to respectively in the 50ml waste water NO in the water sample
2 --N concentration is 485mg/L.The tool plug triangular flask (two) that will contain aggregate sample places shaking table, acts on 240min under 33 ℃ and 55 ℃, 200rpm condition, gets water sample one time every 30min, with NO in aminobenzenesulfonic acid-N-(1-naphthyl)-ethylenediamine colorimetric method for determining water sample
2 -The variation of-N content.Find that by measuring along with the rising of temperature, ferric tannate is to NH
4 +The equilibrium adsorption capacity of-N obviously raise, reach the needed time of adsorption equilibrium obviously shorten, denitrification percent obviously improves.Wherein, when temperature was 33 ℃, 55 ℃, its equilibrium adsorption capacity was respectively: 23.6,61.3mg/g; Reaching the needed time of adsorption equilibrium is respectively: 150,90min; Denitrification percent when reaching adsorption equilibrium is respectively: 15.4%, 46.9%.
The relation of Novel adsorption catalyst---ferric tannate and nitrogen gas generation speed
NH in the ferric tannate energy while adsorbed water body
4 +-N and NO
2 --N.The suction-operated of ferric tannate can improve NH
4 +-N and NO
2 -The inorganic nitrogen that the reaction density of-N, the active group that itself contains can improve again two kinds of forms reacts to each other and generates the speed of nitrogen.
Get the 0.2g ferric tannate and be added in the 200ml waste water, and the blank experiment is set simultaneously.NH in the water sample
4 +-N and NO
2 --N concentration is respectively 494mg/L, 540mg/L.The tool plug triangular flask (two) that will contain aggregate sample places shaking table, under 30 ℃, 200rpm condition, act on 24h, get water sample one time every 3h, use respectively the NH in nessler reagent colorimetric method and aminobenzenesulfonic acid-N-(1-naphthyl)-ethylenediamine colorimetric method for determining water sample
4 +-N and NO
2 -The variation of-N content.Found that by measuring under the equal experiment condition, the generating rate of nitrogen is than high by 93.7% in the blank system in the ferric tannate system.
The specific embodiment
Preparation method below by a kind of Novel adsorption catalyst of processing for sewage water denitrification among specific embodiment narration the present invention.Unless stated otherwise, used technological means is method known in those skilled in the art among the present invention.In addition, embodiment is interpreted as illustrative, but not limits the scope of the invention, and the spirit and scope of the invention are only limited by claims.To those skilled in the art, under the prerequisite that does not deviate from essence of the present invention and scope, various changes that the material component in these embodiments and consumption are carried out or change and also belong to protection scope of the present invention.
Embodiment 1
1) with tannic acid and FeCl
36H
2O all is formulated as the solution that concentration is 0.001mol/L, while stirring with FeCl
3Solution joins in the tannic acid solution, tannic acid solution and FeCl
3The volume ratio of solution is 1: 40, fully reacts 20min, contains black-and-blue floccule in the reacted mixed liquor;
2) with NaHCO
3Solid is dissolved in the distilled water, is mixed with the NaHCO that concentration is 0.65mol/L
3Solution;
3) with step 2) in NaHCO
3Solution slowly joins step 1 with dropper) middle tannic acid and FeCl
3In the reacted mixed liquor that contains black-and-blue floccule, slowly add while stirring and measure the pH value of mixed liquor with pH meter, when the pH of mixed liquor value reaches 7.0, stop dropping;
4) with step 3) in the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 4000rpm in centrifuge;
5) with step 4) in black-and-blue sediment with the washing of the distilled water of 2 times of volumes, wash altogether 3 times, obtain containing black-and-blue sedimentary mixed liquor;
6) with step 5) in the washing after the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 4000rpm in centrifuge;
7) with step 6) in black-and-blue sediment-40 ℃ of dry 24h in vacuum freeze drier of obtaining after centrifugal, drying pressure is 40Pa, can obtain dry ferric tannate sample, dried sample places in the sealing bag normal temperature to preserve.
Embodiment 2
1) with tannic acid and FeCl
36H
2O all is formulated as the solution that concentration is 0.01mol/L, while stirring with FeCl
3Solution joins in the tannic acid solution, tannic acid solution and FeCl
3The volume ratio of solution is 1: 25, fully reacts 10min, contains black-and-blue floccule in the reacted mixed liquor;
2) with NaHCO
3Solid is dissolved in the distilled water, is mixed with the NaHCO that concentration is 0.65mol/L
3Solution;
3) with step 2) in NaHCO
3Solution slowly joins step 1 with dropper) middle tannic acid and FeCl
3In the reacted mixed liquor that contains black-and-blue floccule, slowly add while stirring and measure the pH value of mixed liquor with pH meter, when the pH of mixed liquor value reaches 7.0, stop dropping;
4) with step 3) in the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000rpm in centrifuge;
5) with step 4) in black-and-blue sediment with the washing of the distilled water of 4 times of volumes, wash altogether 3 times, obtain containing black-and-blue sedimentary mixed liquor;
6) with step 5) in the washing after the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000rpm in centrifuge;
7) with step 6) in black-and-blue sediment-45 ℃ of dry 20h in vacuum freeze drier of obtaining after centrifugal, drying pressure is 40Pa, can obtain dry ferric tannate sample, dried sample places in the sealing bag normal temperature to preserve.
Embodiment 3
1) with tannic acid and FeCl
36H
2O all is formulated as the solution that concentration is 0.02mol/L, while stirring with FeCl
3Solution joins in the tannic acid solution, tannic acid solution and FeCl
3The volume ratio of solution is 1: 10, fully reacts 10min, contains black-and-blue floccule in the reacted mixed liquor;
2) with NaHCO
3Solid is dissolved in the distilled water, is mixed with the NaHCO that concentration is 0.65mol/L
3Solution;
3) with step 2) in NaHCO
3Solution slowly joins step 1 with dropper) middle tannic acid and FeCl
3In the reacted mixed liquor that contains black-and-blue floccule, slowly add while stirring and measure the pH value of mixed liquor with pH meter, when the pH of mixed liquor value reaches 7.0, stop dropping;
4) with step 3) in the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000rpm in centrifuge;
5) with step 4) in black-and-blue sediment with the washing of the distilled water of 5 times of volumes, wash altogether 4 times, obtain containing black-and-blue sedimentary mixed liquor;
6) with step 5) in the washing after the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000rpm in centrifuge;
7) with step 6) in black-and-blue sediment-50 ℃ of dry 20h in vacuum freeze drier of obtaining after centrifugal, drying pressure is 40Pa, can obtain dry ferric tannate sample, dried sample places in the sealing bag normal temperature to preserve.
Claims (6)
1. a Novel adsorption catalyst that is used for sewage water denitrification is characterized in that described adsoption catalyst is ferric tannate, and described adsoption catalyst is prepared by following method:
1) tannic acid and FeCl
3Reaction: with tannic acid and FeCl
36H
2O all is formulated as the solution of same concentrations, while stirring with FeCl
3Solution joins in the tannic acid solution, fully reacts 10～20min; Contain black-and-blue floccule in the reacted mixed liquor;
2) NaHCO
3The preparation of solution: with NaHCO
3Solid is dissolved in the distilled water, is mixed with the NaHCO that concentration is 0.65mol/L
3Solution;
3) NaHCO conditioned reaction pH of mixed value: with step 2)
3Solution slowly joins step 1 with dropper) middle tannic acid and FeCl
3In the reacted mixed liquor that contains black-and-blue floccule, slowly add while stirring and measure the pH value of mixed liquor with pH meter, when the pH of mixed liquor value reaches 7.0, stop dropping;
4) once centrifugal: with step 3) in the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000-4000rpm in centrifuge;
5) black-and-blue sediment obtains containing black-and-blue sedimentary mixed liquor with distilled water washing 3-4 time washing: with step 4);
6) contain the centrifugal 5min of black-and-blue sedimentary mixed liquor 3000-4000rpm in centrifuge secondary centrifuging: with step 5) after the washing;
7) the black-and-blue sediment that obtains after centrifugal drying: with step 6) is-40～-50 ℃ of dry 20-24h in vacuum freeze drier, drying pressure is 40Pa, can obtain dry ferric tannate sample, dried sample places normal temperature preservation in the sealing bag.
2. the preparation method of the Novel adsorption catalyst for sewage water denitrification claimed in claim 1 is characterized in that, may further comprise the steps:
1) tannic acid and FeCl
3Reaction: with tannic acid and FeCl
36H
2O all is formulated as the solution of same concentrations, while stirring with FeCl
3Solution joins in the tannic acid solution, fully reacts 10～20min; Contain black-and-blue floccule in the reacted mixed liquor;
2) NaHCO
3The preparation of solution: with NaHCO
3Solid is dissolved in the distilled water, is mixed with the NaHCO that concentration is 0.65mol/L
3Solution;
3) NaHCO conditioned reaction pH of mixed value: with step 2)
3Solution slowly joins step 1 with dropper) middle tannic acid and FeCl
3In the reacted mixed liquor that contains black-and-blue floccule, slowly add while stirring and measure the pH value of mixed liquor with pH meter, when the pH of mixed liquor value reaches 7.0, stop dropping;
4) once centrifugal: with step 3) in the centrifugal 5min of the mixed liquor that contains black-and-blue floccule 3000-4000rpm in centrifuge;
5) black-and-blue sediment obtains containing black-and-blue sedimentary mixed liquor with distilled water washing 3-4 time washing: with step 4);
6) contain the centrifugal 5min of black-and-blue sedimentary mixed liquor 3000-4000rpm in centrifuge secondary centrifuging: with step 5) after the washing;
7) the black-and-blue sediment that obtains after centrifugal drying: with step 6) is-40～-50 ℃ of dry 20-24h in vacuum freeze drier, drying pressure is 40Pa, can obtain dry ferric tannate sample, dried sample places normal temperature preservation in the sealing bag.
3. the preparation method of the Novel adsorption catalyst for sewage water denitrification as claimed in claim 2 is characterized in that step 1) described in tannic acid and FeCl
3Solution concentration is 0.001～0.02mol/L.
4. the preparation method of the Novel adsorption catalyst for sewage water denitrification as claimed in claim 2 is characterized in that step 1) described in tannic acid and FeCl
3The volume ratio of solution is 1: 40～1: 10.
5. the preparation method of the Novel adsorption catalyst for sewage water denitrification as claimed in claim 2 is characterized in that step 5) described in during washing each distillation water yield of adding be black-and-blue sedimentary 2-5 doubly.
6. the application processed at sewage water denitrification of the Novel adsorption catalyst for sewage water denitrification claimed in claim 1.
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| CN107840429A (en) * | 2017-11-13 | 2018-03-27 | 江苏环保产业技术研究院股份公司 | A kind of preparation method and its resulting materials and application for being used to remove the organometallic polymer material of Cr VI |
| CN110116000A (en) * | 2019-04-04 | 2019-08-13 | 杭州师范大学 | A kind of sludge carbon-supported catalysts and its preparation method and application |
| CN112007694A (en) * | 2020-09-16 | 2020-12-01 | 河北科技大学 | Embedded catalyst, preparation method thereof and application thereof in wastewater denitrification |
| CN114191988A (en) * | 2021-11-25 | 2022-03-18 | 宜宾学院 | Application of membrane material in simultaneous removal of ammonia nitrogen and nitrite nitrogen in water |
| CN115608334A (en) * | 2022-10-16 | 2023-01-17 | 北京碧水源膜科技有限公司 | NH (hydrogen sulfide) 4+ /NO 2- Composite adsorbent, preparation method thereof and ammonia nitrogen treatment system applying composite adsorbent |
| CN116832868A (en) * | 2023-05-23 | 2023-10-03 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Preparation method and application of iron nano-enzyme with oxidase-like and peroxidase-like properties |
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| CN107840429B (en) * | 2017-11-13 | 2018-10-19 | 江苏环保产业技术研究院股份公司 | A kind of organometallic polymer material and its preparation method and application of removal Cr VI |
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| CN112007694A (en) * | 2020-09-16 | 2020-12-01 | 河北科技大学 | Embedded catalyst, preparation method thereof and application thereof in wastewater denitrification |
| CN114191988A (en) * | 2021-11-25 | 2022-03-18 | 宜宾学院 | Application of membrane material in simultaneous removal of ammonia nitrogen and nitrite nitrogen in water |
| CN115608334A (en) * | 2022-10-16 | 2023-01-17 | 北京碧水源膜科技有限公司 | NH (hydrogen sulfide) 4+ /NO 2- Composite adsorbent, preparation method thereof and ammonia nitrogen treatment system applying composite adsorbent |
| CN115608334B (en) * | 2022-10-16 | 2023-11-28 | 北京碧水源膜科技有限公司 | NH (NH) 4+ /NO 2- Composite adsorbent, preparation method thereof and ammonia nitrogen treatment system applying composite adsorbent |
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| CN116832868B (en) * | 2023-05-23 | 2024-05-28 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Preparation method and application of iron nano-enzyme with oxidase-like and peroxidase-like properties |
| CN117258762A (en) * | 2023-11-09 | 2023-12-22 | 湖南科技大学 | Composite adsorbent, preparation method and application thereof |
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