CN106582649A - Iron-cobalt bimetal oxyhydroxide and preparing method thereof - Google Patents
Iron-cobalt bimetal oxyhydroxide and preparing method thereof Download PDFInfo
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- CN106582649A CN106582649A CN201611170431.8A CN201611170431A CN106582649A CN 106582649 A CN106582649 A CN 106582649A CN 201611170431 A CN201611170431 A CN 201611170431A CN 106582649 A CN106582649 A CN 106582649A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
- 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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Abstract
The invention discloses an iron-cobalt bimetal oxyhydroxide and a preparing method thereof. The preparing method comprises the steps of preparing an iron-cobalt salt aqueous solution and a strong alkaline solution with a certain concentration and certain matching, using a magnetic stirrer to make the mixed salt solution of iron and cobalt be in a power mixed state, gradually dropwise adding the strong alkaline solution into the mixed solution, and continuously stirring to make the stirred solution mixed and precipitated; after fully precipitating, continuing dropwise adding the strong alkaline solution, adjusting the pH value of the suspension liquid to be larger than or equal to 10 (in the preparing process, the control over pH exerts a significant influence on catalytic activity of the catalyst and the generation of the granularity), after conducting still standing for 1-2 hours, putting the solution into an incubator to be subjected to activation for some time; after the activation treatment, using deionized water to wash the precipitate after the activation to be at constant pH, and obtaining the iron-cobalt bimetal oxyhydroxide after drying. The prepared iron-cobalt bimetal oxyhydroxide can further improve the catalytic ability of monometal oxyhydroxide.
Description
Technical field
The present invention relates to a kind of ferrum cobalt dual-metal oxyhydroxide and preparation method thereof.
Background technology
Ozonation technique is, with ozone as oxidant, to make ozone molecule or oxidisability more strong by the dissolving in water
Free radical and water in complicated Organic substance reacted, make organic macromolecule be degraded into small molecule, or open ring molecule
Ring simultaneously further makes the process of its oxidative degradation.Because ozonization water treatment technical finesse Organic substance effect is good, secondary pollution is few,
Therefore ozonation technique is study hotspot in recent years in water treatment field.But during using independent ozonation technique, by ozone oxygen
The impact of change ability and mass-transfer efficiency, the utilization rate of ozone is very low, therefore to the degradation efficiency of organic pollution also than relatively low.Urge
It is the high-level oxidation technology for receiving much concern in recent years to change ozonation technology, compared with independent ozonation technology, is catalyzed smelly
The reaction rate of oxygen oxidation system faster, it is higher to the clearance of pollutant.O3 catalytic oxidation includes urging for homogeneous and multiphase
Change ozonisation system, heterogeneous catalytic ozonation reaction has the advantages that catalyst is easily reclaimed, but the primary limitation of the technique is
The catalytic reaction site deletion of catalyst, catalysis activity are low, stability is poor and secondary pollution problems.
Oxyhydroxide (oxyhydroxide) refers to the chemical combination being made up of with a certain metal ion oxonium ion, hydroxide ion
Thing, can see that hydrate is converted in oxide process, partially dehydrated intermediate product.Transition metal oxyhydroxide is urged
Agent is a kind of novel environmental functional material developed in recent years, can be applied in water process as ozone catalyst.Should
Class catalyst source is abundant, cheap, and in the process of micro-polluted surface water and subsoil water, application prospect is boundless.Mesh
Before, the species of such catalyst is more single, only has extensive research to monometallic oxyhydroxide and reports.
The content of the invention
It is an object of the invention to provide a kind of ferrum cobalt dual-metal oxyhydroxide and preparation method thereof.Can further carry
The catalytic capability of high monometallic oxyhydroxide.
For achieving the above object, the technical scheme is that：
A kind of preparation method of ferrum cobalt dual-metal oxyhydroxide, with trivalent iron salt, divalent cobalt and highly basic as raw material, adopts
It is complete with sluggish precipitation precipitation, the postactivated 36～50h of pH are adjusted, then precipitate washing is drying to obtain into ferrum cobalt dual-metal hydroxyl
Base oxide.
Heretofore described highly basic is provided simultaneously with following characteristics：1. it is dissolved in water energy to occur to ionize completely, 2. in aqueous solution
The middle anion for ionizing out is entirely hydroxide ion, 3. with acid reaction forming salt and water.Such as sodium hydroxide, potassium hydroxide, hydrogen
Barium monoxide etc..
Heretofore described trivalent iron salt is soluble in water, and is dissolved in after water the salt that can produce ferric ion.
Such as iron sulfate (Fe2(SO4)3), iron chloride (FeCl3), ferric nitrate (Fe (NO3)3) etc..
Heretofore described divalent cobalt is soluble in water, and is dissolved in after water the salt that can produce divalent cobalt ion.
Such as cobaltous sulfate (CoSO4), cobaltous chloride (CoCl2), cobalt nitrate (Co (NO3)2) etc..
Preferably, after ferric salt solution is mixed with divalent cobalt solution, under conditions of stirring, it is added dropwise over highly basic
Solution.
It is further preferred that the concentration of the ferric salt solution is 0.2mol/L～1mol/L.
It is further preferred that the concentration of the divalent cobalt solution is 0.2mol/L～1mol/L.
It is further preferred that the concentration of the strong base solution is 1mol/L～2mol/L.
Preferably, iron ion and the mol ratio of cobalt ion in divalent cobalt are 7～9 in trivalent iron salt:1.
It is further preferred that iron ion and the mol ratio of cobalt ion in divalent cobalt are 7.69 in trivalent iron salt:1.
Preferably, pH >=10 are adjusted.
Preferably, adjust to stand after pH after 1～2h and activated again.
Preferably, the activation temperature is 60 ± 1 DEG C.
Preferably, using deionized water by the precipitate after activation wash to pH it is constant after be dried.
Ferrum cobalt dual-metal oxyhydroxide prepared by a kind of above-mentioned preparation method.
Beneficial effects of the present invention are：
1. the ferrum cobalt dual-metal oxyhydroxide that prepared by the present invention, is not the letter of ferrum oxyhydroxide and cobalt oxyhydroxide
The mixture that single mixing is obtained, but a kind of amorphous structure compound, with special bimetal element bridge crosslinking structure, granule
Even compact and even particle size distribution.
2. the ferrum cobalt dual-metal oxyhydroxide that prepared by the present invention can promote ozone to change into hydroxyl radical free radical, increase water body
The generating rate and quantity of middle free radical, ozone removes the ability of organic pollutants and can be enhanced nearly 30 percentage points.
Description of the drawings
Fig. 1 is ferrum cobalt dual-metal hydroxyl oxygen prepared by ferrous metal oxyhydroxide, cobalt metal oxyhydroxides and embodiment 1
The XRD spectra of compound；
Fig. 2 is the curve of Nitrobenzol in ferrum cobalt dual-metal oxyhydroxide catalytic ozonation water；
Fig. 3 is the curve of Nitrobenzol and ferrum nickel bimetal hydroxyl oxygen in ferrum cobalt dual-metal oxyhydroxide catalytic ozonation water
The contrast curve of the curve of Nitrobenzol in compound catalytic ozonation water.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment the invention will be further described.
Embodiment 1
Prepare 200mL 0.2655mol/L Fe (NO3)3With 0.0345mol/L Co (NO3)2Ferrum-cobalt saline solution, match somebody with somebody
1mol/L NaOH solutions processed.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise over into the ferrum-cobalt saline solution of above-mentioned preparation
In so as to uniform mixed precipitation.After precipitating completely, pH to 11 is adjusted, stand 1.5h, be put into activation 48h in couveuse, activation temperature
Spend for 60 DEG C.Supernatant is removed after standing, the precipitate for obtaining is close to using deionized water wash to pH neutral and no longer
Till change, by 60 DEG C of drying of precipitate, ferrum cobalt dual-metal oxyhydroxide (Fe-CoOOH) is obtained.
The ferrum cobalt dual-metal oxyhydroxide of acquisition is carried out into XRD signs, as shown in figure 1, showing the double gold of ferrum cobalt for preparing
Category hydroxyl oxidize composition granule is a kind of amorphous structure compound, is not the letter of ferrum oxyhydroxide and cobalt oxyhydroxide
Single mixing, with special bimetal element bridge crosslinking structure, granule even compact and even particle size distribution.
The ferrum cobalt dual-metal oxyhydroxide of above-mentioned preparation is removed into the Experimental Characterization of Nitrobenzol as catalyst, such as
Under.
O will be passed through in 1000mL deionized waters3/O2Mixed gas, stop aeration after 30s, make to contain in deionized water
The ozone of 0.95mg/L, adding the nitro benzene aquatic solution of 100mg ferrum cobalt dual-metal oxyhydroxides and 2mL 50mg/L (makes to mix
Nitro phenenyl concentration is 100 μ g/L in solution after conjunction), at ambient temperature magnetic agitation reacts 20min, Nitrobenzol clearance
Characterization result is as shown in Figures 2 and 3.
Comparative example 1
Prepare 200mL 0.3mol/L Fe (NO3)3Aqueous solution, prepares 1mol/L NaOH solutions.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise in the molysite aqueous solution of above-mentioned preparation,
Make its uniform mixed precipitation.After precipitating completely, pH to 11 is adjusted, stand 1.5h, be put into activation 48h, activation temperature in couveuse
For 60 DEG C.Supernatant is removed after standing, the precipitate of acquisition is close to neutral using deionized water wash to pH and is no longer become
Turn to only, by 60 DEG C of drying of precipitate, obtain the oxyhydroxide (FeOOH) of ferrum.
The oxyhydroxide of the ferrum of above-mentioned preparation is removed the Experimental Characterization of Nitrobenzol as catalyst, it is as follows.
O will be passed through in 1000mL deionized waters3/O2Mixed gas, stop aeration after 30s, make to contain in deionized water
The ozone of 0.95mg/L, the nitro benzene aquatic solution of the oxyhydroxide and 2mL50mg/L that add 100mg ferrum (makes mixed
Nitro phenenyl concentration is 100 μ g/L in solution), at ambient temperature magnetic agitation reacts 20min, the sign knot of Nitrobenzol clearance
Fruit is as shown in Figure 2.
Comparative example 2
Prepare 200mL 0.3mol/L Co (NO3)2Aqueous solution, prepares 1mol/L NaOH solutions.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise in the cobalt saline solution of above-mentioned preparation,
Make its uniform mixed precipitation.After precipitating completely, pH to 11 is adjusted, stand 1.5h, be put into activation 48h, activation temperature in couveuse
For 60 DEG C.Supernatant is removed after standing, the precipitate of acquisition is close to neutral using deionized water wash to pH and is no longer become
Turn to only, by 60 DEG C of drying of precipitate, obtain the oxyhydroxide of cobalt.
The oxyhydroxide of the cobalt of above-mentioned preparation is removed the Experimental Characterization of Nitrobenzol as catalyst, it is as follows.
O will be passed through in 1000mL deionized waters3/O2Mixed gas, stop aeration after 30s, make to contain in deionized water
The ozone of 0.95mg/L, the nitro benzene aquatic solution of the oxyhydroxide and 2mL 50mg/L that add 100mg cobalts (makes mixed
Nitro phenenyl concentration in solution is 100 μ g/L), at ambient temperature magnetic agitation reacts 20min, the sign of Nitrobenzol clearance
As a result it is as shown in Figure 2.
Show that ferrum cobalt dual-metal oxyhydroxide prepared by embodiment 1 can greatly be carried by the characterization result of Fig. 2
High ozone removes the ability of organic pollutants, and the removal ability of p-nitrophenyl lifts nearly 30%, the more independent ferrum of catalytic capability
Oxyhydroxide or the oxyhydroxide of independent cobalt all increase.
Comparative example 3
Prepare 200mL 0.3mol/L Fe (NO3)3With 0.04mol/L Ni (NO3)2Ferrum-nickel salt aqueous solution, prepare
1mol/L NaOH solutions.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise over into the ferrum-nickel salt aqueous solution of above-mentioned preparation
In so as to uniform mixed precipitation.After precipitating completely, pH to 11 is adjusted, stand 1.5h, be put into activation 48h in couveuse, activation temperature
Spend for 60 DEG C.Supernatant is removed after standing, the precipitate for obtaining is close to using deionized water wash to pH neutral and no longer
Till change, by 60 DEG C of drying of precipitate, ferrum nickel bimetal oxyhydroxide is obtained.
The ferrum nickel bimetal oxyhydroxide of above-mentioned preparation is removed into the Experimental Characterization of Nitrobenzol as catalyst, such as
Under.
O will be passed through in 1000mL deionized waters3/O2Mixed gas, stop aeration after 30s, make to contain in deionized water
The ozone of 0.95mg/L, adding the nitro benzene aquatic solution of 100mg ferrum nickel bimetal oxyhydroxides and 2mL 50mg/L (makes to mix
Nitro phenenyl concentration is 100 μ g/L in solution after conjunction), at ambient temperature magnetic agitation reacts 20min, Nitrobenzol clearance
Characterization result is as shown in Figure 3.
Shown by the characterization result of Fig. 3, ferrum nickel bimetal oxyhydroxide prepared by comparative example 3 is only capable of removing ozone
The capability improving 10% of Nitrobenzol, is much weaker than the catalytic performance of the ferrum cobalt dual-metal oxyhydroxide of the preparation of embodiment 1.
By the contrast of Fig. 2～Fig. 3, it can be seen that the oxyhydroxide of ferrum can make the clearance of Nitrobenzol lift 20%
Left and right, and ferrum nickel bimetal oxyhydroxide is only capable of lifting 10%, it was demonstrated that the combination of ferrum nickel in ferrum nickel bimetal oxyhydroxide
Do not simply fail to lift the catalytic performance of catalyst, the catalytic performance of catalyst is reduced on the contrary.Ferrum cobalt dual-metal oxyhydroxide
The clearance that Nitrobenzol can be made lifts nearly 30%, shows the synergism by ferrum cobalt so that the catalytic effect of catalyst enters one
Step increases.
Embodiment 2
Prepare 200mL 0.2655mol/L Fe (NO3)3With 0.0345mol/L Co (NO3)2Ferrum-cobalt saline solution, match somebody with somebody
1mol/L NaOH solutions processed.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise over into the ferrum-cobalt saline solution of above-mentioned preparation
In so as to uniform mixed precipitation.After precipitating completely, pH to 10 is adjusted, stand 2h, be put into activation 48h, activation temperature in couveuse
For 60 DEG C.Supernatant is removed after standing, the precipitate of acquisition is close to neutral using deionized water wash to pH and is no longer become
Turn to only, by 70 DEG C of drying of precipitate, obtain ferrum cobalt dual-metal oxyhydroxide (Fe-CoOOH).
Embodiment 3
Prepare 200mL 0.2655mol/L Fe (NO3)3With 0.0345mol/L Co (NO3)2Ferrum-cobalt saline solution, match somebody with somebody
1mol/L NaOH solutions processed.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise over into the ferrum-cobalt saline solution of above-mentioned preparation
In so as to uniform mixed precipitation.After precipitating completely, pH to 13 is adjusted, stand 1h, be put into activation 38h, activation temperature in couveuse
For 60 DEG C.Supernatant is removed after standing, the precipitate of acquisition is close to neutral using deionized water wash to pH and is no longer become
Turn to only, by 50 DEG C of drying of precipitate, obtain ferrum cobalt dual-metal oxyhydroxide (Fe-CoOOH).
Embodiment 4
Prepare 200mL 0.2655mol/L Fe (NO3)3With 0.0345mol/L Co (NO3)2Ferrum-cobalt saline solution, match somebody with somebody
1mol/L NaOH solutions processed.
Under the conditions of magnetic agitation, the NaOH solution of above-mentioned preparation is added dropwise over into the ferrum-cobalt saline solution of above-mentioned preparation
In so as to uniform mixed precipitation.After precipitating completely, pH to 12 is adjusted, stand 1.5h, be put into activation 44h in couveuse, activation temperature
Spend for 60 DEG C.Supernatant is removed after standing, the precipitate for obtaining is close to using deionized water wash to pH neutral and no longer
Till change, by precipitate natural air drying, ferrum cobalt dual-metal oxyhydroxide (Fe-CoOOH) is obtained.
The characterization result of ferrum cobalt dual-metal oxyhydroxide (Fe-CoOOH) prepared by embodiment 2～4 is made with embodiment 1
Standby ferrum cobalt dual-metal oxyhydroxide (Fe-CoOOH) is similar.
All embodiments and comparative example are not detected by Adsorption of the catalyst to pollutant in the present invention.
Although the above-mentioned accompanying drawing that combines is described to the specific embodiment of the present invention, not to invention protection domain
Restriction, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not required to
The various modifications or deformation made by paying creative work are still within the scope of the present invention.
Claims (10)
1. a kind of preparation method of ferrum cobalt dual-metal oxyhydroxide, is characterized in that, be with trivalent iron salt, divalent cobalt and highly basic
Raw material, it is complete using sluggish precipitation precipitation, the postactivated 36～50h of pH are adjusted, then precipitate washing is drying to obtain into ferrum cobalt
Bimetallic oxyhydroxide.
2. preparation method as claimed in claim 1, is characterized in that, after ferric salt solution is mixed with divalent cobalt solution,
Under conditions of stirring, strong base solution is added dropwise over.
3. preparation method as claimed in claim 2, is characterized in that, the concentration of the ferric salt solution be 0.2mol/L～
1mol/L。
Or, the concentration of the divalent cobalt solution is 0.2mol/L～1mol/L.
4. preparation method as claimed in claim 2, is characterized in that, the concentration of the strong base solution is 1mol/L～2mol/L.
5. preparation method as claimed in claim 1, is characterized in that, iron ion and cobalt ion in divalent cobalt in trivalent iron salt
Mol ratio is 7～9:1, preferably 7.69:1.
6. preparation method as claimed in claim 1, is characterized in that, adjust pH >=10.
7. preparation method as claimed in claim 1, is characterized in that, adjusts and activated again after 1～2h of standing after pH.
8. preparation method as claimed in claim 1, is characterized in that, the activation temperature is 60 ± 1 DEG C.
9. preparation method as claimed in claim 1, is characterized in that, the precipitate after activation be washed to pH using deionized water
It is dried after constant.
10. the ferrum cobalt dual-metal oxyhydroxide that prepared by a kind of preparation method as described in claim 1-9 is arbitrary.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107093746A (en) * | 2017-04-28 | 2017-08-25 | 深圳市航盛新材料技术有限公司 | Iron cobalt carbon composite oxides and preparation method thereof, metal-air battery |
| CN113385174A (en) * | 2021-07-17 | 2021-09-14 | 安徽农业大学 | Cobalt modified hydrated iron oxide catalyst and preparation method and application thereof |
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| CN107093746A (en) * | 2017-04-28 | 2017-08-25 | 深圳市航盛新材料技术有限公司 | Iron cobalt carbon composite oxides and preparation method thereof, metal-air battery |
| CN113385174A (en) * | 2021-07-17 | 2021-09-14 | 安徽农业大学 | Cobalt modified hydrated iron oxide catalyst and preparation method and application thereof |
| CN113385174B (en) * | 2021-07-17 | 2022-08-26 | 安徽农业大学 | Cobalt modified hydrated iron oxide catalyst and preparation method and application thereof |
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