CN105776493B - A kind of preparation method of the laminated metal compound for Organic Pollutants in Wastewater processing - Google Patents

A kind of preparation method of the laminated metal compound for Organic Pollutants in Wastewater processing Download PDF

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CN105776493B
CN105776493B CN201610163559.5A CN201610163559A CN105776493B CN 105776493 B CN105776493 B CN 105776493B CN 201610163559 A CN201610163559 A CN 201610163559A CN 105776493 B CN105776493 B CN 105776493B
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metal compound
sodium hydroxide
laminated metal
solution
salt
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CN105776493A (en
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周吉峙
高原
舒伟康
魏凤
钱光人
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Removal Of Specific Substances (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

The present invention relates to a kind of preparation methods of laminated metal compound for Organic Pollutants in Wastewater processing in aquatic ecological restoration field.Using coprecipitation, pH value is kept in a certain range, ferrous iron, ferric iron, doped metal ion are mixed into gained according to a certain percentage.Laminated metal compound of the invention effectively enhances the stability of original material structure, while being also greatly facilitated the generation of free radical in system, can quickly and effectively realize the removal to Organic Pollutants in Wastewater, shortens the reaction time, improves contaminant removal efficiency.

Description

A kind of preparation of the laminated metal compound for Organic Pollutants in Wastewater processing Method
Technical field
The invention belongs to underground water pollutions in environment protection field to repair scope, more particularly to one kind for organic dirt in waste water Contaminate the laminated metal compound of object processing.
Background technique
There is no effective minimizing technologies for hardly degraded organic substance in water for traditional method for treating water.With water ring The aggravation of border resource pollution, the pollutant kind for needing processing difficult to degrade is more and more in water environment, this just needs to find one The method that kind can rapidly and efficiently remove water pollutant, especially organic pollutant, while water environment is not caused again secondary Pollution.
Patina is a kind of special layered bi-metal compound, is dispersed with ferrous iron and ferric iron on laminate.Have been reported that finger Out, pure patina has good application effect in heterogeneous class Fenton (Fenton-like) oxidation reaction, to methyl orange, Luo Dan The organic pollutants such as bright B, phenolic compound have good removal effect.Heterogeneous class Fenton oxidation reaction refers to Fe3+, contain Iron mineral and some other transition metal such as Co, Cd, Cu, Ag, Mn, Ni etc. accelerate or substitution Fe2+And hydrogen peroxide is risen and is urged A kind of reaction of change effect has better treatment effect to waste water compared with traditional Fenton oxidation technology.To find out its cause, main If in the reaction system, ferrous iron can be reacted with hydrogen peroxide generates OH, OH because containing ferrous ion in pure patina There is strong oxidizing property, effectively water pollutant can be removed；Furthermore the ferric iron in pure patina can also be reacted with hydrogen peroxide Generating ferrous iron can more efficiently go so that ferrous iron present in more efficient utilization system, generates more OH Except the pollutant in water body.But pure patina itself be again it is unstable, be easy to be oxidized, thus it cannot be guaranteed that in pure patina Ferrous iron can fully in class Fenton's reaction participate in reaction, generate OH, organic pollutant is completely removed.
Studies have shown that the stability of patina can be improved in doped metal ion.It is reported that in patina antimony dopant, Its stability can be improved in the metals such as copper, also has protective effect to the ferrous iron in patina.Meanwhile in liquid phase Fenton-like In, the metal ion of doping can be improved the free radical value volume and range of product generated in Fenton-like, go to organic pollutant Effect is promoted well except having.Therefore by metal ion mixing into patina, namely preparation laminated metal compound, it is water environment The another new direction studied in reparation.
Summary of the invention
The purpose of the present invention is to provide a kind of systems of laminated metal compound for Organic Pollutants in Wastewater processing Preparation Method and its application, it is characterised in that there is following process and step:
A takes divalent iron salt, trivalent iron pan, doped metal salt to make raw material；The molar ratio of three are as follows: doped metal ion: two Valence iron: ferric iron=(0.05 ~ 0.5): 1:0.5；
Divalent iron salt, trivalent iron salt, doped metal salt and appropriate sodium hydroxide are dissolved in no carbon dioxide by b respectively In ionized water；Ferric salt solution will be contained and sodium hydroxide solution is respectively placed in two constant pressure separatory funnels；Ferrous iron will be contained Salting liquid and doping
Metal salt solution is placed in four-hole boiling flask；The concentration of the sodium hydroxide solution is 1 mo1/L；
Liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask, four-hole boiling flask is molten by c respectively under nitrogen protection PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 6.5 ~ 7.5；
Product low-temperature and high-speed is centrifuged by d, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Above-mentioned divalent, trivalent iron salt are sulfate, above-mentioned doped metal salt be nickel chloride, chromium chloride, copper chloride or Cobalt chloride.
Advantages of the present invention:
(1) solid material obtained by not only increases ferrous utilization in heterogeneous class Fenton oxidation reaction system Rate enhances stability of material even more due to the presence of doped metal ion, promotes hydroxyl radical free radical and sulfate radical in system The generation of free radical, to achieve the purpose that rapidly and efficiently to handle Organic Pollutants in Wastewater.
(2) solid material preparation process is simple, does not have secondary pollution generation in treatment process.Through laboratory practical application It was found that be apparently higher than pure patina to the degradation effect of pollutant.
Mechanism of the invention:
(1) the stratiform Fe formed is utilized2+/Fe3+Or Fe2+/Mn+/Fe3+The structure of (M is doping metals) compound-material Characteristic, i.e. laminate are positively charged, so that ferrous iron is in ferric ion and doping in heterogeneous class Fenton oxidation reaction system Under the catalytic action of metal ion (such as Ni), it can be reacted with hydrogen peroxide and generate more hydroxyl radical free radicals, thus in waste water Organic pollutant quickly removed.
(2) the stratiform Fe formed is utilized2+/Fe3+Or Fe2+/Mn+/Fe3+(M is extra implant metal) compound-material Architectural characteristic, i.e. interlayer have sulfate anion intercalation, so that in the heterogeneous class Fenton oxidation containing great amount of hydroxy group free radical In reaction system, it is free to generate micro sulfate radical under the catalytic action of doped metal ion (such as Ni) for sulfate anion Base achievees the purpose that efficiently to remove pollutant so as to more thoroughly remove the organic pollutant in waste water.
Detailed description of the invention
Fig. 1 is the XRD characterization map of the laminated metal compound in the embodiment of the present invention 1.
Fig. 2 is laminated metal compound Pyrogentisinic Acid's removal ability lab diagram in the embodiment of the present invention 1.
Fig. 3 is laminated metal compound Pyrogentisinic Acid's removal ability lab diagram in the embodiment of the present invention 2.
Fig. 4 is the XRD characterization map of the laminated metal compound in the embodiment of the present invention 6.
Fig. 5 is laminated metal compound Pyrogentisinic Acid's removal ability lab diagram in the embodiment of the present invention 6.
Specific embodiment
The present invention is proposed to utilize and be mixed on the basis of furtheing investigate hydroxyl radical free radical and potentiometric titrations mechanism of production Efficient benefit of the ferrous iron in heterogeneous class Fenton oxidation reaction system is realized in the catalytic action of miscellaneous metal ion (such as W metal) With the generation of free radical in promotion system improves contaminant removal efficiency in water body.
Below by embodiment, to the technical solution in the present invention carry out clearly, be described entirely by.
Embodiment 1
In the embodiment of the present invention, a kind of preparation side of the laminated metal compound for Organic Pollutants in Wastewater processing Method, the specific steps are as follows:
(1) according to Ni2+: Fe2+: Fe3+Molar ratio 0.1:1:0.5 weighs six water nickel chlorides, ferrous sulfate heptahydrate, x water sulfuric acid Iron solid and appropriate sodium hydroxide；
(2) six water nickel chlorides, ferrous sulfate heptahydrate, ferric sulfate solid and appropriate sodium hydroxide are dissolved in no dioxy respectively Change in carbon deionized water.Ferric sulfate solid solution and sodium hydroxide solution are respectively placed in constant pressure separatory funnel, by seven water sulphur Sour ferrous iron solution and six water nickel chloride solutions are placed in four-hole boiling flask, and the concentration of the sodium hydroxide solution is 1 mo1/L；
(3) under nitrogen protection, the liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask respectively, four-hole boiling flask is molten PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 6.8；
(4) product low-temperature and high-speed is centrifuged, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Laminated metal compound in embodiment 1 is tested, test result is as follows:
Test 1
Using phenol as target contaminant, under conditions of concentration is 50 mg/L, with the laminated metal chemical combination in embodiment 1 Object is handled water body under conditions of adding hydrogen peroxide.Measure in 90 min can remove 80% phenol (in terms of TOC, under Together).And the pure patina of identical molar ratio synthesis, under same dose (with sample meter, similarly hereinafter), pure patina can only remove 60% Phenol.
Embodiment 2
In the embodiment of the present invention, a kind of preparation side of the laminated metal compound for Organic Pollutants in Wastewater processing Method, the specific steps are as follows:
(1) according to Ni2+: Fe2+: Fe3+Molar ratio 0.2:1:0.5 weighs six water nickel chlorides, ferrous sulfate heptahydrate, x water sulfuric acid Iron solid and appropriate sodium hydroxide；
(2) six water nickel chlorides, ferrous sulfate heptahydrate, ferric sulfate solid and appropriate sodium hydroxide are dissolved in no dioxy respectively Change in carbon deionized water.Ferric sulfate solid solution and sodium hydroxide solution are respectively placed in constant pressure separatory funnel, by seven water sulphur Sour ferrous iron solution and six water nickel chloride solutions are placed in four-hole boiling flask, and the concentration of the sodium hydroxide solution is 1 mo1/L；
(3) under nitrogen protection, the liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask respectively, four-hole boiling flask is molten PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 6.8；
(4) product low-temperature and high-speed is centrifuged, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Laminated metal compound in embodiment 2 is tested, test result is as follows:
Test 2
Using phenol as target contaminant, under conditions of concentration is 50 mg/L, with the laminated metal chemical combination in embodiment 2 Object is handled water body under conditions of adding hydrogen peroxide.Measure in 90 min removable 90% phenol.And identical mole Than the pure patina of synthesis, under same dose, pure patina can only remove 60% phenol.
Embodiment 3
In the embodiment of the present invention, a kind of preparation side of the laminated metal compound for Organic Pollutants in Wastewater processing Method, the specific steps are as follows:
(1) according to Ni2+: Fe2+: Fe3+Molar ratio 0.5:1:0.5 weighs six water nickel chlorides, ferrous sulfate heptahydrate, x water sulfuric acid Iron solid and appropriate sodium hydroxide；
(2) six water nickel chlorides, ferrous sulfate heptahydrate, ferric sulfate solid and appropriate sodium hydroxide are dissolved in no dioxy respectively Change in carbon deionized water.Ferric sulfate solid solution and sodium hydroxide solution are respectively placed in constant pressure separatory funnel, by seven water sulphur Sour ferrous iron solution and six water nickel chloride solutions are placed in four-hole boiling flask, and the concentration of the sodium hydroxide solution is 1 mo1/L；
(3) under nitrogen protection, the liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask respectively, four-hole boiling flask is molten PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 7 or so；
(4) product low-temperature and high-speed is centrifuged, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Laminated metal compound in embodiment 3 is tested, test result is as follows:
Test 3
Using phenol as target contaminant, under conditions of concentration is 50 mg/L, with the laminated metal chemical combination in embodiment 3 Object is handled water body under conditions of adding hydrogen peroxide.Measure in 90 min removable 95% phenol.And identical mole Than the pure patina of synthesis, under same dose, pure patina can only remove 60% phenol.
Embodiment 4
In the embodiment of the present invention, a kind of preparation side of the laminated metal compound for Organic Pollutants in Wastewater processing Method, the specific steps are as follows:
(1) according to Cu2+: Fe2+: Fe3+Molar ratio 0.2:1:0.5 weighs copper chloride dihydrate, ferrous sulfate heptahydrate, x water sulfuric acid Iron solid and appropriate sodium hydroxide；
(2) copper chloride dihydrate, ferrous sulfate heptahydrate, ferric sulfate solid and appropriate sodium hydroxide are dissolved in no dioxy respectively Change in carbon deionized water.Ferric sulfate solid solution and sodium hydroxide solution are respectively placed in constant pressure separatory funnel, by seven water sulphur Sour ferrous iron solution and six water nickel chloride solutions are placed in four-hole boiling flask, and the concentration of the sodium hydroxide solution is 1 mo1/L；
(3) under nitrogen protection, the liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask respectively, four-hole boiling flask is molten PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 6.8；
(4) product low-temperature and high-speed is centrifuged, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Laminated metal compound in embodiment 4 is tested, test result is as follows:
Test 4
Using phenol as target contaminant, under conditions of concentration is 50 mg/L, with the laminated metal chemical combination in embodiment 4 Object is handled water body under conditions of adding hydrogen peroxide.Measure in 90 min removable 73% phenol.And identical mole Than the pure patina of synthesis, under same dose, pure patina can only remove 60% phenol.
Embodiment 5
In the embodiment of the present invention, a kind of preparation side of the laminated metal compound for Organic Pollutants in Wastewater processing Method, the specific steps are as follows:
(1) according to Cr3+: Fe2+: Fe3+Molar ratio 0.2:1:0.5 weighs chromium chloride hexahydrate, ferrous sulfate heptahydrate, x water sulfuric acid Iron solid and appropriate sodium hydroxide；
(2) chromium chloride hexahydrate, ferrous sulfate heptahydrate, ferric sulfate solid and appropriate sodium hydroxide are dissolved in no dioxy respectively Change in carbon deionized water.Ferric sulfate solid solution and sodium hydroxide solution are respectively placed in constant pressure separatory funnel, by seven water sulphur Sour ferrous iron solution and chromium chloride hexahydrate solution are placed in four-hole boiling flask, and the concentration of the sodium hydroxide solution is 1 mo1/L；
(3) under nitrogen protection, the liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask respectively, four-hole boiling flask is molten PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 6.8；
(4) product low-temperature and high-speed is centrifuged, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Laminated metal compound in embodiment 5 is tested, test result is as follows:
Test 5
Using phenol as target contaminant, under conditions of concentration is 50 mg/L, with the laminated metal chemical combination in embodiment 5 Object is handled water body under conditions of adding hydrogen peroxide.Measure in 90 min removable 68% phenol.And identical mole Than the pure patina of synthesis, under same dose, pure patina can only remove 60% phenol.
Embodiment 6
In the embodiment of the present invention, a kind of preparation side of the laminated metal compound for Organic Pollutants in Wastewater processing Method, the specific steps are as follows:
(1) according to Co3+: Fe2+: Fe3+Molar ratio 0.2:1:0.5 weighs CoCL2 6H2O, ferrous sulfate heptahydrate, x water sulfuric acid Iron solid and appropriate sodium hydroxide；
(2) CoCL2 6H2O, ferrous sulfate heptahydrate, ferric sulfate solid and appropriate sodium hydroxide are dissolved in no dioxy respectively Change in carbon deionized water.Ferric sulfate solid solution and sodium hydroxide solution are respectively placed in constant pressure separatory funnel, by seven water sulphur Sour ferrous iron solution and CoCL2 6H2O solution are placed in four-hole boiling flask, and the concentration of the sodium hydroxide solution is 1 mo1/L；
(3) under nitrogen protection, the liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask respectively, four-hole boiling flask is molten PH value in liquid maintains between 6.0 ~ 7.0, lasting to stir, and until ferrum sulfuricum oxydatum solutum is all added dropwise, controls four-hole boiling flask Middle pH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1 h 7.1；
(4) product low-temperature and high-speed is centrifuged, is washed, is ground up, sieved after freeze-drying, most with no carbon dioxide deionized water The laminated metal compound for wastewater treatment is made eventually.
Laminated metal compound in embodiment 6 is tested, test result is as follows:
Test 6
Using phenol as target contaminant, under conditions of concentration is 50 mg/L, with the laminated metal chemical combination in embodiment 6 Object is handled water body under conditions of adding hydrogen peroxide.Measure in 90 min removable 85% phenol.And identical mole Than the pure patina of synthesis, under same dose, pure patina can only remove 60% phenol.

Claims (2)

1. a kind of preparation method of the laminated metal compound for Organic Pollutants in Wastewater processing, it is characterised in that have such as Under process and step:
A takes divalent iron salt, trivalent iron salt, doped metal salt to make raw material；The molar ratio of three are as follows: doped metal ion: divalent Iron: ferric iron=(0.05~0.5): 1:0.5；
Divalent iron salt, trivalent iron salt, doped metal salt and appropriate sodium hydroxide are dissolved in no carbon dioxide deionization by b respectively In water；Ferric salt solution will be contained and sodium hydroxide solution is respectively placed in two constant pressure separatory funnels；It is molten divalent iron salt will to be contained Liquid and doping metals salting liquid are placed in four-hole boiling flask；The concentration of the sodium hydroxide solution is 1mo1/L；
Liquid in constant pressure separatory funnel is added drop-wise in four-hole boiling flask by c respectively under nitrogen protection, in four-hole boiling flask solution PH value maintain between 6.0~7.0, it is lasting to stir, until ferric salt solution is all added dropwise, control in four-hole boiling flask PH value of solution stops that sodium hydroxide solution is added dropwise, reacts 1h 6.8~7.5；
Product low-temperature and high-speed is centrifuged by d, is washed with no carbon dioxide deionized water, is ground up, sieved after freeze-drying, final to make It must be used for the laminated metal compound of wastewater treatment.
2. a kind of preparation side of laminated metal compound for Organic Pollutants in Wastewater processing as described in claim 1 Method, it is characterised in that the divalent, trivalent iron salt are sulfate；The doped metal salt is nickel chloride, chromium chloride, chlorination Copper or cobalt chloride.
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