CN101130169A - Production of complexing iron catalyzer and application of polyphase photocatalysis hydrogen phosphide - Google Patents
Production of complexing iron catalyzer and application of polyphase photocatalysis hydrogen phosphide Download PDFInfo
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- CN101130169A CN101130169A CNA2007100727514A CN200710072751A CN101130169A CN 101130169 A CN101130169 A CN 101130169A CN A2007100727514 A CNA2007100727514 A CN A2007100727514A CN 200710072751 A CN200710072751 A CN 200710072751A CN 101130169 A CN101130169 A CN 101130169A
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- 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
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Abstract
The invention discloses a making method of complex ferric catalyst and application of multi-phased optical catalyzed hydrogen peroxide to solve the problem of low-decomposing speed of the multi-phased optical catalyzed hydrogen peroxide in the water, which comprises the following steps: complexing trivalent ferric ion and complex to form trivalent ferric complex; immersing the predisposed cation exchange resin particle or film in the trivalent complex; vibrating under indoor temperature for 0. 5-24h; separating resin from complex solution; using clean water to wash reciprocally until the ferric doesn't be dissolved out; the complex ferric catalyst can be applied for multi-phased optical catalyzed hydrogen peroxide with decomposing rate to 100%. The invention can increase the mineralization rate of organics with mineralization rate over 705, which simplifies the operation obviously.
Description
Technical field
The present invention relates to the application of a kind of Preparation of catalysts and catalyzing hydrogen peroxide thereof; Be specifically related to a kind of preparation of complexing iron catalyst and the application of multiphase photocatalysis of hydrogen peroxide thereof.
Background technology
Hydrogen peroxide is the green oxidation agent, because product is the oxygen G﹠W, so hydrogen peroxide is widely used in the industry.The method of catalyzing hydrogen peroxide has two kinds, and a kind of is base catalysis, and a kind of is transition metal-catalyzed.The reaction rate of base catalysis hydrogen peroxide is slow, and for regulating the pH value, needs to consume a large amount of alkali; The reaction rate of transition metal-catalyzed hydrogen peroxide is more much bigger than the reaction rate of base catalysis.The ferrous ion catalyzing hydrogen peroxide is that Fenton reagent is exactly transition metal-catalyzed model.Fenton in 1894 proposes under the condition of acid pH=2, ferrous ion can catalyzing hydrogen peroxide oxidation tartaric acid effectively.The Fenton oxidation has lot of advantages, simple as method, oxidation rate is fast, reagent concentration is low, economical and efficient etc., and reagent is environmentally friendly, however optimum pH value 3.0～4.0, when the pH value greater than 4, iron will precipitate with the form of iron hydroxide, this greatly reduces reaction rate, and most biochemical system is in pH＜5.0 o'clock, biologically active will be suppressed, and the pH value significantly reduces and also is not suitable for present soil and phreatic reparation.When preventing that the pH value from raising, the sedimentation problem that iron occurs, some strong complexing agents are added in the reaction system, to stablize iron ion, therefore, occurred being improvement (Modified) the Fenton system of catalyst and being Fenton-like (Fenton-like) system of catalyst with ferric complex compound with ferrous complex compound because the use of complexing agent, make Fenton reagent neutral or near neutral condition under use and become possibility.Some amine carboxylic complexing agents such as DTPA, EDTA, EGTA, NTA, be introduced in the Fenton system, greater than 6 o'clock, catalytic activity was higher in the pH value for EDTA, DPTA in the pH value greater than 7 o'clock optimum activities.Though after the iron complexing, the oxidability of system does not become, reaction rate than before the complexing not slowly many.In macromolecule loading multiphase photocatalysis of hydrogen peroxide field, ferric iron directly combines with ion exchange resin, perhaps coordinations such as ferric iron and histidine, bipyridyl, do not see about with the report of inorganic part coordination.The effect of part is to make ferric iron stable, its oxidation-reduction potential is reduced, but organic ligand is easily oxidized, and also unstable with the ionic bond coordination with the compound of covalent bond coordination.
Summary of the invention
The objective of the invention is in order to solve the low problem of multiphase photocatalysis of hydrogen peroxide decomposition rate in the method for treating water, and a kind of preparation of complexing iron catalyst and the application of multiphase photocatalysis of hydrogen peroxide thereof are provided.The present invention has reduced the oxidation-reduction potential of iron with inorganic part fluorine and oxalic acid and ferric iron coordination, has increased ion exchange resin to organic absorption property, and has increased the decomposition rate to hydrogen peroxide, and organic clearance is improved greatly.The preparation method of complexing iron catalyst of the present invention is as follows: earlier ferric ion and complex compound are pressed 1～2: 1 mol ratio complexing formation ferric complex; The proportioning that adds 7～8g cationic ion-exchange resin particle or film by every mole of ferric ion is dipped in pretreated cationic ion-exchange resin particle or film in the ferric complex; 0.5～24h at room temperature vibrates; filter then; after cationic ion-exchange resin after the above-mentioned processing or film clean repeatedly with clear water; up to the stripping that does not have iron, promptly make the complexing iron catalyst.The complexing iron catalyst that said method makes is applied to multiphase photocatalysis of hydrogen peroxide, adopts ultraviolet light or visible light radiation in the reaction, and catalyst is the complexing iron catalyst, and oxidant is a hydrogen peroxide; Technical parameter in the course of reaction is as follows: the dosage of complexing iron catalyst is 50～200mg/L, and the dosage of hydrogen peroxide is 10～110mmol/L, and the mol ratio of hydrogen peroxide and organic pollution is 1～100: 1, reaction time 5min～2h.
Described ferric ion can load on charcoal fiber, zeolite, the silica gel, and the load capacity of trivalent iron salt is 1～10wt.% (weight).Also can add copper ion or manganese ion in ferric ion, ferric iron accounts for the 80～99wt.% (weight) of metal ion gross weight.Described ferric ion is provided by trivalent iron salt; Trivalent iron salt is ferric sulfate, iron chloride, ferric nitrate or ferric perchlorate.
Described complex compound is pyrimidine, porphyrin, disodium ethylene diamine tetraacetate, natrium citricum, sodium tartrate, sodium fluoride or sodium oxalate.
Described cationic ion-exchange resin particle is 001 * 7 or D001.Described cation exchange resin membrane is Nafion 117.
Heterogeneous smooth complexing iron catalyst catalyzing hydrogen peroxide is used for handling the organic matter of feedwater, city secondary effluent, pharmacy waste water.
But the complexing agent among the present invention is not limited to above-mentioned example, the part of strong complexing is arranged all in protection scope of the present invention with iron.
Iron and complex compound coordination are that the oxidation-reduction potential of iron is reduced, the accelerated decomposition hydrogen peroxide, iron as reducing agent by hydrogen peroxide oxidation, chemical valence raises becomes quadrivalent iron, hydrogen peroxide is reduced the generation hydroxyl radical free radical, and the high price iron of generation has oxidability, also can strengthen the decomposition of hydrogen peroxide simultaneously, so the active specy in the course of reaction is the acting in conjunction of hydroxyl radical free radical and high price iron.
The complexing iron catalyst of the present invention's preparation can improve the decomposition rate of hydrogen peroxide, decomposition rate reaches 100%, the organic matter in the water is had good adsorption and oxidation usefulness, under ultraviolet light or visible light radiation, can increase organic salinity, make its mineralization rate reach 70%.Among the present invention method simple, be convenient to operation.
The specific embodiment
The specific embodiment one: the preparation method of the complexing iron catalyst of present embodiment is as follows: earlier ferric ion and complex compound are pressed 1～2: 1 mol ratio complexing formation ferric complex; The proportioning that adds 7～8g cationic ion-exchange resin particle or film by every mole of ferric ion is dipped in pretreated cationic ion-exchange resin particle or film in the ferric complex; 0.5～24h at room temperature vibrates; filter then; after cationic ion-exchange resin after the above-mentioned processing or film clean repeatedly with clear water; up to the stripping that does not have iron, promptly make the complexing iron catalyst.
Described cationic ion-exchange resin particle grain size is 0.05～1.2mm.
The specific embodiment two: present embodiment and the specific embodiment one are different is that the mol ratio of ferric ion and complex compound is 1.2～1.8: 1.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one are different is that the mol ratio of ferric ion and complex compound is 1.5: 1.Other is identical with the specific embodiment one.
The specific embodiment four: what present embodiment and the specific embodiment one were different is that every mole of ferric ion adds 7.5g cationic ion-exchange resin particle or film.Other is identical with the specific embodiment one.
The specific embodiment five: the present embodiment and the specific embodiment one are not both cationic ion-exchange resin pretreatment of particles method: till at first with clear water resin being washed, free from admixture muddy to the limpid nothing of water outlet; Then in exchange column, alternately soaked successively 2～4 hours with 3～5% HCl and NaOH, between soda acid with the drip washing of mixed bed high-purity deionized water to water outlet near neutral, so repeat 2～3 times, each soda acid consumption is 2 times of resin volume; The last HCl solution of handling application 4～5% carries out; Drain acid solution, promptly finish the cationic ion-exchange resin pretreatment of particles with clear water drip washing to neutrality.Other is identical with the concrete specific embodiment one.
The specific embodiment six: what present embodiment and the specific embodiment one were different is the cation exchange resin membrane preprocess method: under 75 ℃ of conditions, cation exchange resin membrane is incubated 1 hour in 5% (weight) hydrogen peroxide and 10% (weight) sulfuric acid solution, cleans with distilled water then and promptly finish the cation exchange resin membrane preliminary treatment three times.Other it identical with the specific embodiment one.
The specific embodiment seven: what present embodiment and the specific embodiment one were different is that ferric ion is loaded on charcoal fiber, zeolite, the silica gel, and the load capacity of trivalent iron salt is 1～10wt.% (weight).Other is identical with the specific embodiment one.
The specific embodiment eight: what present embodiment was different with the specific embodiment one or eight is to have added copper ion or manganese ion in ferric ion, and ferric iron accounts for the 80～99wt.% (weight) of metal ion gross weight.Other is identical with the specific embodiment one or eight.
The specific embodiment nine: what present embodiment and the specific embodiment one were different is that ferric ion is provided by trivalent iron salt; Trivalent iron salt is ferric sulfate, iron chloride, ferric nitrate or ferric perchlorate.Other is identical with the specific embodiment one.
The specific embodiment ten: what present embodiment and the specific embodiment one were different is that complex compound is pyrimidine, porphyrin, disodium ethylene diamine tetraacetate, natrium citricum, sodium tartrate, sodium fluoride or sodium oxalate.Other is identical with the specific embodiment one.
The specific embodiment 11: present embodiment and the specific embodiment one are different is that the cationic ion-exchange resin particle is 001 * 7 or D001.Other is identical with the specific embodiment one.
The specific embodiment 12: what present embodiment and the specific embodiment one were different is that cation exchange resin membrane is Nafion 117.Other is identical with the specific embodiment one.
The specific embodiment 13: present embodiment complexing iron catalyst is applied to multiphase photocatalysis of hydrogen peroxide, adopts ultraviolet light or visible light radiation in the reaction, and catalyst is the complexing iron catalyst, and oxidant is a hydrogen peroxide; Technical parameter in the course of reaction is as follows: the dosage of complexing iron catalyst is 50～200mg/L, and the dosage of hydrogen peroxide is 10～110mmol/L, and the mol ratio of hydrogen peroxide and organic pollution is 1～100: 1, reaction time 5min～2h.
The organic resolution ratio of present embodiment reaches 100%, and organic mineralization rate reaches more than 70%.Organic percent of decolourization is 100%, and the COD clearance reaches more than 90%.
The specific embodiment 14: present embodiment and the specific embodiment 13 are different is that to be added into dosage in reaction be oxygen, ozone or both mixing of 10～1000mmol/L.Other reactions steps is identical with the specific embodiment 13.
When present embodiment add be oxygen and ozone mixture the time, oxygen and ozone are by arbitrarily than mixing.
The specific embodiment 14: what present embodiment and the specific embodiment 13 were different is the organic matter that heterogeneous smooth complexing iron catalyst catalyzing hydrogen peroxide is used for handling feedwater, city secondary effluent, pharmacy waste water.
The specific embodiment 15: in the present embodiment with the NaF of 0.1mmol/L and the Fe (NO of 0.1mmol/L
3)
3Each 10mL equal-volume mixes, and adds the 50mgD001 cationic ion-exchange resin, and room temperature is put into constant temperature oscillator, shakes 12 hours, filters then, and is clean with distilled water flushing ion exchange resin, obtains the complexing iron catalyst; To be applied to multiphase photocatalysis of hydrogen peroxide through the complexing iron catalyst that above-mentioned reaction makes, technical parameter in the course of reaction is as follows: 0.5mmol/L dye of positive ion malachite green (MG) 100mL, add the 10mmol/L hydrogen peroxide, and pH is 6, under sunshine, reacted 1 hour.
The percent of decolourization of MG reaches 100% in the present embodiment, and the COD clearance is 90%.
The specific embodiment 16: present embodiment is to adopt sodium oxalate to make complexing agent with the different of the specific embodiment 15, and sodium oxalate and ferric mol ratio are 1: 2, and complexing iron catalyst multiphase photocatalysis of hydrogen peroxide is reflected under the sunshine and reacted 5 minutes.
The percent of decolourization of MG reaches 100% in the present embodiment, and the clearance of COD is 97%.
The specific embodiment 17: present embodiment and the specific embodiment 15 different are to adopt 001 * 7 cationic ion-exchange resin, complexing iron catalyst multiphase photocatalysis of hydrogen peroxide to be reflected under the sunshine reaction 10 minutes.
The percent of decolourization of MG is 100% in the present embodiment, and the clearance of COD is 97%.
Claims (10)
1. the preparation of a complexing iron catalyst is characterized in that this preparation method is as follows: earlier ferric ion and complex compound are pressed 1～2: 1 mol ratio complexing formation ferric complex; The proportioning that adds 7～8g cationic ion-exchange resin particle or film by every mole of ferric ion is dipped in pretreated cationic ion-exchange resin particle or film in the ferric complex; 0.5～24h at room temperature vibrates; filter then; after cationic ion-exchange resin after the above-mentioned processing or film clean repeatedly with clear water; up to the stripping that does not have iron, promptly make the complexing iron catalyst.
2. the preparation of complexing iron catalyst according to claim 1, the mol ratio that it is characterized in that ferric ion and complex compound is 1.5: 1.
3. the preparation of complexing iron catalyst according to claim 1 is characterized in that ferric ion is loaded on charcoal fiber, zeolite, the silica gel, and the load capacity of trivalent iron salt is 1～10wt.%.
4. according to the preparation of claim 1 or 3 described complexing iron catalysts, it is characterized in that having added copper ion or manganese ion in ferric ion, ferric iron accounts for 80～99wt.% of metal ion gross weight.
5. the preparation of complexing iron catalyst according to claim 1 is characterized in that ferric ion is provided by trivalent iron salt; Trivalent iron salt is ferric sulfate, iron chloride, ferric nitrate or ferric perchlorate.
6. the preparation of complexing iron catalyst according to claim 1 is characterized in that complex compound is pyrimidine, porphyrin, disodium ethylene diamine tetraacetate, natrium citricum, sodium tartrate, sodium fluoride or sodium oxalate.
7. the preparation of complexing iron catalyst according to claim 1 is characterized in that the cationic ion-exchange resin particle is 001 * 7 or D001.
8. the preparation of complexing iron catalyst according to claim 1 is characterized in that cation exchange resin membrane is Nafion 117.
9. utilize the complexing iron catalyst multiphase photocatalysis of hydrogen peroxide of claim 1 preparation, it is characterized in that the complexing iron catalyst is applied to multiphase photocatalysis of hydrogen peroxide, adopt ultraviolet light or visible light radiation in the reaction, catalyst is the complexing iron catalyst, and oxidant is a hydrogen peroxide; Technical parameter in the course of reaction is as follows: the dosage of complexing iron catalyst is 50～200mg/L, and the dosage of hydrogen peroxide is 10～110mmol/L, and the mol ratio of hydrogen peroxide and organic pollution is 1～100: 1, reaction time 5min～2h.
10. the application of multiphase photocatalysis of hydrogen peroxide according to claim 9 is characterized in that heterogeneous smooth complexing iron catalyst catalyzing hydrogen peroxide is used for handling the organic matter of feedwater, city secondary effluent, pharmacy waste water.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100727514A CN101130169A (en) | 2007-09-05 | 2007-09-05 | Production of complexing iron catalyzer and application of polyphase photocatalysis hydrogen phosphide |
| CN2008101445153A CN101327448B (en) | 2007-09-05 | 2008-07-24 | Preparation of chelated iron catalyst and use thereof for multiphase photocatalysis of hydrogen peroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100727514A CN101130169A (en) | 2007-09-05 | 2007-09-05 | Production of complexing iron catalyzer and application of polyphase photocatalysis hydrogen phosphide |
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| CN101130169A true CN101130169A (en) | 2008-02-27 |
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| CNA2007100727514A Pending CN101130169A (en) | 2007-09-05 | 2007-09-05 | Production of complexing iron catalyzer and application of polyphase photocatalysis hydrogen phosphide |
| CN2008101445153A Expired - Fee Related CN101327448B (en) | 2007-09-05 | 2008-07-24 | Preparation of chelated iron catalyst and use thereof for multiphase photocatalysis of hydrogen peroxide |
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| CN2008101445153A Expired - Fee Related CN101327448B (en) | 2007-09-05 | 2008-07-24 | Preparation of chelated iron catalyst and use thereof for multiphase photocatalysis of hydrogen peroxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102834190A (en) * | 2009-10-09 | 2012-12-19 | 道达尔公司 | Method for oxidising organic compounds |
| CN104470858A (en) * | 2012-07-17 | 2015-03-25 | 索尔维公司 | A process for removal of hydrogen peroxide from an aqueous solution |
| CN108786933A (en) * | 2018-06-19 | 2018-11-13 | 中盐金坛盐化有限责任公司 | A kind of low sodium type cation resin regeneration agent and its preparation method and application |
| CN109569721A (en) * | 2018-12-27 | 2019-04-05 | 南京医科大学 | A kind of preparation method and application of PORPHYRIN IRON modification mesopore silicon oxide composite material |
| CN110038573A (en) * | 2019-05-15 | 2019-07-23 | 沈阳工大蓝金环保产业技术研究院有限公司 | Heterogeneous fenton catalyst Nafion/Fe3+Composite membrane and preparation method thereof |
| CN110240250A (en) * | 2019-06-06 | 2019-09-17 | 南京融众环境工程研究院有限公司 | A kind of method of degrading decabromodiphenyl ether |
| CN110255812A (en) * | 2019-06-05 | 2019-09-20 | 华东理工大学 | A kind of biochemical and advanced oxidation combined method retaining ammonia nitrogen removal antibiotic in livestock and poultry cultivation sewage disposal process |
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| IT1396226B1 (en) * | 2009-11-11 | 2012-11-16 | Ct Di Ricerca Interd Sulla Risonanza Magn Nucl Per L Ambiente L Agro Alimentare Ed I Nuovi Mat Dell | METODOPER SEQUESTING THE ORGANIC CARBON IN A SOIL |
| CN104229974B (en) * | 2014-09-18 | 2016-09-07 | 浙江理工大学 | A kind of method of quick process organic wastewater |
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| CN106946314B (en) * | 2017-04-01 | 2020-06-30 | 东南大学 | Method for efficiently degrading organic wastewater |
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| CN115520952B (en) * | 2021-06-24 | 2024-06-28 | 中国石油化工股份有限公司 | Fenton oxidation treatment method for organic wastewater |
-
2007
- 2007-09-05 CN CNA2007100727514A patent/CN101130169A/en active Pending
-
2008
- 2008-07-24 CN CN2008101445153A patent/CN101327448B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102834190A (en) * | 2009-10-09 | 2012-12-19 | 道达尔公司 | Method for oxidising organic compounds |
| CN102834190B (en) * | 2009-10-09 | 2015-01-14 | 道达尔公司 | Method for oxidising organic compounds |
| CN104470858A (en) * | 2012-07-17 | 2015-03-25 | 索尔维公司 | A process for removal of hydrogen peroxide from an aqueous solution |
| CN108786933A (en) * | 2018-06-19 | 2018-11-13 | 中盐金坛盐化有限责任公司 | A kind of low sodium type cation resin regeneration agent and its preparation method and application |
| CN109569721A (en) * | 2018-12-27 | 2019-04-05 | 南京医科大学 | A kind of preparation method and application of PORPHYRIN IRON modification mesopore silicon oxide composite material |
| CN109569721B (en) * | 2018-12-27 | 2020-07-10 | 南京医科大学 | Preparation method and application of porphyrin iron modified mesoporous silica composite material |
| CN110038573A (en) * | 2019-05-15 | 2019-07-23 | 沈阳工大蓝金环保产业技术研究院有限公司 | Heterogeneous fenton catalyst Nafion/Fe3+Composite membrane and preparation method thereof |
| CN110255812A (en) * | 2019-06-05 | 2019-09-20 | 华东理工大学 | A kind of biochemical and advanced oxidation combined method retaining ammonia nitrogen removal antibiotic in livestock and poultry cultivation sewage disposal process |
| CN110240250A (en) * | 2019-06-06 | 2019-09-17 | 南京融众环境工程研究院有限公司 | A kind of method of degrading decabromodiphenyl ether |
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| Publication number | Publication date |
|---|---|
| CN101327448B (en) | 2010-07-14 |
| CN101327448A (en) | 2008-12-24 |
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