CN107029667A - A kind of Fe3O4RGO Ag composites and preparation method and application - Google Patents
A kind of Fe3O4RGO Ag composites and preparation method and application Download PDFInfo
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
A kind of Fe3O4RGO Ag composites, the composite passes through the load active component Fe on carrier graphene oxide GO3O4Obtained with Ag.Disclosed herein as well is Fe simultaneously3O4The preparation method and applications of rGO Ag composites.The characteristics of present invention utilizes big redox graphene specific surface area and many functional groups, noble silver and magnetic material iron of the load with more preferable absorption property, the removal efficiency of nonvalent mercury reaches more than 90%；And the magnetic coupling sorbing material used in the present invention can be separated and recovered by Magneto separate means, recycled after high temperature regeneration, while reclaiming purity very high mercury metal, operating cost can not only be substantially reduced, and direct economic benefit can be obtained.
Description
Technical field
The invention belongs to atmospheric environment protection field, and in particular to a kind of Fe3O4- rGO-Ag composites and preparation method thereof
With application, Adsorption purifying smoke is carried out to the nonvalent mercury in waste gas using it, and realize the recovery of adsorbent and repeat to make
With.
Background technology
Heavy metal Hg has the features such as persistence, cumulative bad, easy migration and high biological enrichment, is advised by united nations environment
Draw administration and be classified as global pollution thing, the harm to environmental and human health impacts is very big.1950s occurs attached in Japanese Minamata bay
Near organic mercury poisoning event, is referred to as " minamata disease " event, is once serious mercury pollution disaster.Also sent out in China in recent years
Many mercury pollution accidents, such as Kweiyang Lake Baihua mercury pollution accident, Beibei, chongqing accident of mercury pollution, Ankang Xunyang mercury ore are given birth to
Mercury pollution etc., so the emission control for strengthening mercury is extremely important.
Causing the main human factor of air mercury pollution has a lot, and the discharge of wherein industrial smoke and waste gas is to need to pay attention to
One of artificial source.The mercurous waste gas produced in the coal fire discharged flue gas of Industrial Boiler and industrial processes is main with particulate Hg
(HgP), gaseous state bivalent mercury (Hg2+) and gaseous state nonvalent mercury (Hg0) three kinds of forms are present, conventional smoke eliminator has collaboration de-
Mercury is acted on：Dust arrester can effectively remove HgP；Hg2+It is soluble in water, it can be removed by flue gas desulfurization device.However, due to Hg0Easily
Volatilize and be insoluble in water, it is difficult to be removed by existing pollution control equipment.Therefore, Hg0Efficient removal technology turn into current flue gas
The emphasis and difficult point of demercuration.
Current flue gas nonvalent mercury minimizing technology can be largely classified into two classes：One class is by existing fume treatment auxiliary pair
Mercury is removed, and nonvalent mercury catalysis is bivalent mercury by such as SCR, is then desulfurized system removal；Equations of The Second Kind is by duct sorbent injection
Adsorbent is removed.For the application of adsorbent, the activated carbon scope of application is most wide, but due to the cost mistake of its control mercury
Height, it is no in actual industrial enterprise at present to be promoted well.(one kind is used for coal-fired flue-gas to patent CN 102553522A
The oxidisability adsorbent of mercury removal) proposed on the basis of activated carbon using the mixture of montmorillonite and activated carbon as carrier, load
Copper chloride and manganese chloride carry out the absorption removal of mercury as active component, and its principle is first by the Elemental Mercury Hg contained in flue gas0Inhaling
Attached dose of surface oxidation turns into Hg+Or Hg2+, then again by mercury absorption in adsorbent surface, so that mercury is removed from flue gas, should
Method adsorbent can not be recycled, and operating cost is high；A kind of patent CN200910244547.5 (sides of flue gas desulfurizing and hydrargyrum-removing
Method) propose using this method using lime/Ca (OH)2It is real using circulation desulfurization ash as auxiliary desulfurizing agent as desulfurizing agent
The desulfuration demercuration of existing flue gas, this method belongs to calcium base class adsorbent, although can reach while removing the mesh of oxysulfide and mercury
, but the removal efficiency of itself is not high, it is necessary to improve its removal efficiency using certain method, and desulfurated plaster
It is contaminated.In addition, also patent CN201110030287.9, CN200610102077.5, CN 102430328 B, CN
102515162 A etc. report some new adsorbents, but high-efficient mercury removing can be realized simultaneously and recycle and have no
Report.
The content of the invention
The composite adsorption of nonvalent mercury in industrial smoke or waste gas can be effectively removed it is an object of the invention to provide a kind of
Agent --- Fe3O4- rGO-Ag composites are that another object of the present invention is this hair there is provided its application there is provided its preparation method
The 3rd bright goal of the invention.
Based on above-mentioned purpose, this invention takes following technical scheme：A kind of Fe3O4- rGO-Ag composites, this is combined
Material passes through the load active component Fe on carrier graphene oxide GO3O4Obtained with Ag.
In the composite, the percentage by weight of each component is：Graphene oxide 23.6%~57.8%；Fe3O4
33.1%~67.4%；Ag 1%~10%.
Described Fe3O4The preparation method of-rGO-Ag composites, comprises the following steps：
1) first carrier graphene oxide GO and iron precursor water solution are blended in ethylene glycol, add polyethylene glycol
Reaction, after reaction terminates, reaction solution Magneto separate after ethanol eccentric cleaning obtains crude product A, and crude product A is again through washing, dry Fe3O4-
RGO composites；Wherein, the amount ratio of graphene oxide GO, the presoma of iron, ethylene glycol and polyethylene glycol is 1g：(2
~10) g：(200~800) ml：(5~20) g；
2) by Fe3O4- rGO composites are immersed in the precursor water solution of silver, temperature rising reflux, afterwards cooling, Magneto separate
Crude product B is obtained, crude product B is through washing, being drying to obtain Fe3O4- rGO-Ag composites, silver-colored presoma and Fe3O4- rGO composite woods
The mass ratio of material is (0.015~0.17)：1.
Step 1) in, the temperature of reaction is 180 DEG C~220 DEG C, and the time of reaction is 10~12h, and obtained crude product A is through water
20~24h is dried in vacuo after washing at 50 DEG C~80 DEG C.
Step 2) in, the temperature of temperature rising reflux is 120 DEG C, and return time is 20min；Room temperature is cooled to after temperature rising reflux again
Magneto separate is carried out, obtained crude product B is first through washing again ultrasonic disperse in water in 20~24h of vacuum drying at 50 DEG C~80 DEG C.
The presoma of the iron divides for chlorate, nitrate, carbonate, oxalates, acetate and the other high temperature of iron
Solution is produced more than one or both of salt of metal oxide.
The relative molecular mass of the polyethylene glycol is 200~6000.
The silver-colored presoma is more than one or both of silver chlorate, silver bromide, silver iodide, silver nitrate.
Graphene oxide GO is prepared using Hummers methods.
Described Fe3O4- rGO-Ag composites answering in nonvalent mercury in removing industrial smoke or waste gas as adsorbent
With.Concrete operations are by Fe3O4- rGO-Ag composites are sprayed into mercurous industrial smoke, after absorption nonvalent mercury, are removed using dry type
Dirt device is collected to adsorbent, so as to realize that nonvalent mercury is separated with adsorbent from flue gas, the adsorbent after absorption is passed through
Heating desorption is recycled after Magneto separate.
Because the adsorbent of the present invention has magnetic, the dust and adsorbent that dry dust removal apparatus is collected pass through Magneto separate
Device is separated, and elevated temperature desorption regeneration is carried out to adsorbent, while realizing the recovery of mercury and the recycling of adsorbent.
The industrial smoke temperature can at 50~200 DEG C, the entrance of adsorbent flue gas enter dry dust removal apparatus it
Before；The dry dust removal apparatus being applicable can be bag-type dusting, electric precipitation or electric bag compound dust-collection device.
Simple grapheme material is general for complicated industrial smoke zeroth order mercury adsorption features, adsorption mechanism of the invention
It is：First, graphene oxide is in load Fe3O4During be reduced simultaneously, obtained redox graphene (rGO) ratio
Surface area is big and functional group is more, Fe to be loaded3O4After silver, amalgam absorption effect occurs under 50~200 DEG C of flue-gas temperature for Ag
Really, the Adsorption of flue gas nonvalent mercury, Fe are promoted3O4Load can promote the chemically stable of adsorbed mercury, and both are same
When in the presence of can have certain Anti-Jamming to the sulfur dioxide component in flue gas.Secondly, load capacity is to material final performance
Influence it is also more crucial, experiment find, if Fe3O4The too low stabilization for being unfavorable for Magneto separate and adsorbate of load capacity, load capacity
It is too high nonvalent mercury to be hindered to enter inside graphene combined with Ag；The Ag too low then adsorption capacity of load capacity and adsorption activity drop
Low, load capacity crosses the cost of conference increase adsorbent and Ag loss.
Compared with prior art, the invention has the advantages that：
1st, the characteristics of present invention utilizes big redox graphene specific surface area and many functional groups, load has more preferably absorption
The noble silver and magnetic material iron of performance, the removal efficiency that nonvalent mercury can be achieved reach more than 90%；
2nd, after the magnetic coupling sorbing material used in the present invention can be separated and recovered by Magneto separate means, recycle
High temperature regeneration, while reclaiming purity very high mercury metal, can not only substantially reduce operating cost, and can obtain direct economical
Benefit.
Embodiment
Technical scheme is described further with reference to specific embodiment.
The present embodiment is implemented under the premise of with technical solution of the present invention, gives detailed embodiment and specific behaviour
Make process, but protection scope of the present invention is not limited to following embodiments.
The main object of the present invention is that industrial smoke or waste gas containing nonvalent mercury are efficiently removed using the method for absorption
Mercury, reclaim and recycle adsorbent.Therefore the present invention program implementation process in, emphasis with realize high-efficient mercury removing, reclaim simultaneously
Recycling adsorbent is target.
Heretofore described room temperature refers specifically to 20~30 DEG C.
Embodiment 1
A kind of Fe3O4- rGO-Ag composites, the composite on graphene oxide carrier GO by loading Fe3O4With
Ag is obtained.In the composite, the percentage by weight of each component is：Graphene oxide 42.5%；Fe3O448.4%；Ag
9.1%.
Described Fe3O4The preparation method of-rGO-Ag composites, comprises the following steps：
1) graphene oxide GO is prepared with Hummers methods, by 100mg GO ultrasonic disperses in 50ml ethylene glycol, added
0.40g FeCl3·6H2O, room temperature is at the uniform velocity stirred after 2h, adds 1g PEG, reactor is transferred to after stirring, anti-at 220 DEG C
Answer 10h, solution is through ethanol eccentric cleaning 3~5 times, and Magneto separate goes the removal of impurity to obtain crude product A, crude product A after washing 3~5 times through being placed in
50 DEG C of dry 24h obtain Fe in vacuum drying chamber3O4- rGO composites；Wherein, graphene oxide GO, the presoma of iron, ethylene glycol
Amount ratio with polyethylene glycol is 1g：4g：500ml：10g.
2) the above-mentioned Fe of 20mg are weighed3O4- rGO composites, ultrasonic disperse adds 0.2mL mass in 20mL ultra-pure waters
Fraction is 1% silver nitrate solution, is uniformly mixed, is warming up to 120 DEG C and the 20min that flows back, is cooled to room temperature, Magneto separate is obtained
To crude product B, crude product B ultrasonic disperses after 4~5 times are washed in ultra-pure water, then are placed in 50 DEG C of dryings in vacuum drying chamber
24h, produces Fe3O4- rGO-Ag composites, silver-colored presoma and Fe3O4The mass ratio of-rGO composites is 0.16：1.
Using：By described Fe3O4- rGO-Ag composites zeroth order in industrial smoke or waste gas is removed as adsorbent
Application in mercury.Concrete operations are by Fe3O4- rGO-Ag composites are sprayed into mercurous industrial smoke, after absorption nonvalent mercury, profit
Adsorbent is collected with dry dust removal apparatus, so as to realize that nonvalent mercury is separated with adsorbent from flue gas, after absorption
Adsorbent heats desorption after Magneto separate and recycled.
Embodiment 2
A kind of Fe3O4- rGO-Ag composites, the composite on graphene oxide carrier GO by loading Fe3O4With
Ag is obtained.In the composite, the percentage by weight of each component is：Graphene oxide 23.9%；Fe3O467.4%；Ag
8.7%.
Described Fe3O4The preparation method of-rGO-Ag composites, comprises the following steps：
1) graphene oxide GO is prepared with Hummers methods, by 200mg GO ultrasonic disperses in 100ml ethylene glycol, plus
Enter 1g Fe (NO3)3·9H2O, room temperature is at the uniform velocity stirred after 2h, is added 2g PEG, reactor is transferred to after stirring, at 220 DEG C
12h is reacted, reaction solution is with after ethanol eccentric cleaning 3~5 times, and Magneto separate goes the removal of impurity to obtain crude product A, and crude product A is through washing 3~5 times
After be placed in 80 DEG C of dry 20h in vacuum drying chamber, obtain Fe3O4- rGO composites；Wherein, the forerunner of graphene oxide GO, iron
The amount ratio of body, ethylene glycol and polyethylene glycol is 1g：5g：500ml：10g；
2) the above-mentioned Fe of 30mg are weighed3O4- rGO composites, ultrasonic disperse adds 0.25mL matter in 30mL ultra-pure waters
The silver bromide solution that fraction is 2% is measured, is uniformly mixed, is warming up to 120 DEG C and the 30min that flows back, is subsequently cooled to room temperature, is used
Magnetism separate method is separated, and obtained crude product B ultrasonic disperses after 4~5 times are washed in ultra-pure water, are finally placed in vacuum
80 DEG C of dry 20h, produce Fe in drying box3O4- rGO-Ag composites, silver-colored presoma and Fe3O4The matter of-rGO composites
Amount is than being 0.1：1.
The recovery of element mercury and the regeneration of adsorbent and circulation be the same as Example 1.
Embodiment 3
A kind of Fe3O4- rGO-Ag composites, the composite on graphene oxide carrier GO by loading Fe3O4With
Ag is obtained.In the composite, the percentage by weight of each component is：Graphene oxide 57.8%；Fe3O433.1%；Ag
9.1%.
Described Fe3O4The preparation method of-rGO-Ag composites is with example 1, and difference is, step 1) in, oxidation
Graphene GO, the presoma of iron, the amount ratio of ethylene glycol and polyethylene glycol are 1g：2g：200ml：5g；Step 2) in, silver
Presoma and Fe3O4The mass ratio of-rGO composites is 0.16：1.
Embodiment 4
A kind of Fe3O4- rGO-Ag composites, the composite on graphene oxide carrier GO by loading Fe3O4With
Ag is obtained.In the composite, the percentage by weight of each component is：Graphene oxide 23.6%；Fe3O467.3%；Ag
9.1%.
The Fe3O4The preparation method be the same as Example 1 of-rGO-Ag composites, difference is, step 1) in, oxidation
Graphene GO, the presoma of iron, the amount ratio of ethylene glycol and polyethylene glycol are 1g：10g：800ml：20g；Step 2) in,
The presoma and Fe of silver3O4The mass ratio of-rGO composites is 0.16：1.
Embodiment 5
A kind of Fe3O4- rGO-Ag composites, the composite on graphene oxide carrier GO by loading Fe3O4With
Ag is obtained.In the composite, the percentage by weight of each component is：Graphene oxide 40.8%；Fe3O458.2%；Ag 1%.
The Fe3O4The preparation method be the same as Example 1 of-rGO-Ag composites, difference is, step 1) in, oxidation
Graphene GO, the presoma of iron, the amount ratio of ethylene glycol and polyethylene glycol are 1g：5g：500ml：10g；Step 2) in, silver
Presoma and Fe3O4The mass ratio of-rGO composites is 0.015：1.
Embodiment 6
A kind of Fe3O4- rGO-Ag composites, the composite on graphene oxide carrier GO by loading Fe3O4With
Ag is obtained.In the composite, the percentage by weight of each component is：Graphene oxide 37.1%；Fe3O452.9%；Ag
10%.
The Fe3O4The preparation method be the same as Example 1 of-rGO-Ag composites, difference is, step 1) in, oxidation
Graphene GO, the presoma of iron, the amount ratio of ethylene glycol and polyethylene glycol are 1g：5g：600ml：15g；Step 2) in, silver
Presoma and Fe3O4The mass ratio of-rGO composites is 0.17：1.
Using and effect test
Meanwhile, to verify the removal effect of nonvalent mercury of the present invention, with Fe made from the present embodiment 13O4- rGO-Ag composite woods
Following application is carried out exemplified by material and is tested, due to there is no other solid matters, only sorbing material in flue gas in the experimentation,
Therefore Magneto separate step need not be carried out in subsequent regeneration and cyclic process.Needed if during specific engineer applied
It could be regenerated after Magneto separate.
Using：Take the above-mentioned Fe of 0.5g3O4- rGO-Ag composites, are put into tubular fixed-bed reactor, are passed through and contain
The μ g/m of nonvalent mercury 1003Simulated flue gas, the content of sulfur dioxide is 500ppm.Temperature be 150 DEG C, air speed be 50000h-1's
Under the conditions of carry out adsorption experiment, as a result show, utilize Fe3O4- rGO-Ag adsorbents are to the Adsorption efficiency of nonvalent mercury
94%.Compared with one pack system redox graphene adsorbent (clearance is only 50%~70%), same flue gas condition places an order
Solely load Fe Fe3O4The removal efficiency about 65~75% of-rGO composite Adsorption of Mercury, the Ag-rGO composite woods of independent loaded Ag
The removal efficiency about 70~80% of Adsorption of Mercury is expected, using the method for the present invention by Fe made from Fe, Ag step load3O4-rGO-Ag
Composite is then greatly improved the activity of adsorbent, the removal efficiency of mercury is reached more than 90%.
Temperature influences：Other conditions are constant, the operation temperature of tubular fixed-bed reactor only are down into 75 DEG C, now
Fe3O4- rGO-Ag adsorbents remain to reach 92% to the catalyzed conversion Adsorption efficiency of nonvalent mercury.It can be seen that, according to institute of the present invention
Obtained adsorbent still has higher adsorption activity at a lower temperature.
Regeneration and circulation：Adsorbent after absorption is placed in tube furnace reactor, is heated to 350 DEG C, while being passed through air
It is desorbed, that is, respectively obtains the adsorbent after mercury and regeneration.
1st, under different adsorption temps nonvalent mercury removal effect
To verify the removal effect of present invention nonvalent mercury under different adsorption temps, with Fe made from the present embodiment 23O4-
Following test is carried out exemplified by rGO-Ag composites.
Take the above-mentioned Fe of 0.8g3O4- rGO-Ag composites, are put into tubular fixed-bed reactor, are passed through containing nonvalent mercury
200μg/m3Simulated flue gas, the content of sulfur dioxide is 800ppm.Temperature be respectively set to 50 DEG C, 100 DEG C, 150 DEG C, 200
DEG C, air speed is 50000h-1Under conditions of, carry out adsorption experiment.As a result show, utilize Fe3O4- rGO-Ag adsorbents are in not equality of temperature
It is respectively 93%, 96%, 98%, 92% to the Adsorption efficiency of nonvalent mercury under degree.When illustrating that flue-gas temperature is below 200 DEG C
The removal efficiency of mercury can reach more than 90%.
2nd, silver nitrate consumption is to Fe3O4The influence of-rGO-Ag composite absorption properties
Fe is prepared using method same as Example 13O4After-rGO composites, four parts of 40mg are weighed respectively
Fe3O4- rGO composites, respectively ultrasonic disperse in 20mL ultra-pure waters, successively in four parts of solution add 0.1mL, 0.2mL,
0.4mL, 0.6mL mass fraction are 1% silver nitrate solution, are uniformly mixed, are warming up to 120 DEG C and the 30min that flows back, then
Room temperature is cooled to, is separated with magnetism separate method, Fe is obtained3O4- rGO-Ag composites, the ultrasound after 4~5 times are washed
Be scattered in ultra-pure water, be finally placed in 50 DEG C of dry 24h in vacuum drying chamber, the load capacity that Ag is made is respectively 1.5%, 3%,
6%th, 9% four parts of Fe3O4- rGO-Ag composites.
From above-mentioned four parts of Fe3O40.5g is taken to carry out single adsorption experiment in-rGO-Ag composites respectively.It is put into
In tubular fixed-bed reactor, it is passed through containing the μ g/m of nonvalent mercury 1003Simulated flue gas, the content of sulfur dioxide is 500ppm.In temperature
Degree is 150 DEG C, air speed is 50000h-1Under conditions of carry out adsorption experiment, as a result show, load the Fe of different silver contents3O4-
RGO-Ag adsorbents are respectively 91%, 94%, 95%, 97% to the Adsorption efficiency of nonvalent mercury.Illustrate in rational scope
Interior increase Ag content, can improve the absorption property of adsorbent.
Claims (10)
1. a kind of Fe3O4- rGO-Ag composites, it is characterised in that the composite on carrier graphene oxide GO by bearing
Carry active component Fe3O4Obtained with Ag.
2. Fe as claimed in claim 13O4- rGO-Ag composites, it is characterised in that in the composite, the weight of each component
Measuring percentage is：Graphene oxide 23.6%~57.8%；Fe3O433.1%~67.4%；Ag 1%~10%.
3. the Fe described in claim 1 or 23O4The preparation method of-rGO-Ag composites, it is characterised in that including following step
Suddenly：
1）First carrier graphene oxide GO and iron presoma are blended in ethylene glycol, polyethylene glycol reaction, reaction is added
After end, solution Magneto separate after ethanol eccentric cleaning obtains crude product A, and crude product A is again through washing, dry Fe3O4- rGO composite woods
Material；Wherein, the amount ratio of graphene oxide GO, the presoma of iron, ethylene glycol and polyethylene glycol is 1 g：（2~10）g：
（200~800）ml：（5~20）g；
2）By Fe3O4- rGO composites are immersed in the precursor solution of silver, temperature rising reflux, and cooling, Magneto separate are obtained slightly afterwards
Product B, crude product B is through washing, being drying to obtain Fe3O4- rGO-Ag composites, silver-colored presoma and Fe3O4- rGO composites
Mass ratio is（0.015~0.17）：1.
4. Fe as claimed in claim 33O4The preparation method of-rGO-Ag composites, it is characterised in that step 1）In, reaction
Temperature be 180 DEG C~220 DEG C, time of reaction is 10~12h, and obtained crude product A is true at 50 DEG C~80 DEG C after washing
Sky dries 20~24 h.
5. Fe as claimed in claim 33O4The preparation method of-rGO-Ag composites, it is characterised in that step 2）In, heating
The temperature of backflow is 120 DEG C, and return time is 20min；Room temperature is cooled to after temperature rising reflux and carries out Magneto separate again, obtained crude product
B is first through washing again ultrasonic disperse in water in 20~24 h of vacuum drying at 50 DEG C~80 DEG C.
6. Fe as claimed in claim 33O4The preparation method of-rGO-Ag composites, it is characterised in that the forerunner of the iron
Body produces the salt of metal oxide for the chlorate of iron, nitrate, carbonate, oxalates, acetate and other pyrolytics
It is more than one or both of class.
7. Fe as claimed in claim 33O4The preparation method of-rGO-Ag composites, it is characterised in that the polyethylene glycol
Relative molecular mass be 200~6000.
8. Fe as claimed in claim 33O4The preparation method of-rGO-Ag composites, it is characterised in that the silver-colored forerunner
Body is more than one or both of silver chlorate, silver bromide, silver iodide, silver nitrate.
9. Fe as claimed in claim 33O4The preparation method of-rGO-Ag composites, it is characterised in that use Hummers
Method prepares graphene oxide GO.
10. the Fe described in claim 1 or 23O4- rGO-Ag composites are as adsorbent in industrial smoke or waste gas is removed
Application in nonvalent mercury.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108837694A (en) * | 2018-07-02 | 2018-11-20 | 宁夏大学 | A method of removing nonvalent mercury and fixed ion mercury from flue gas |
| CN112774691A (en) * | 2021-01-27 | 2021-05-11 | 宁波方太厨具有限公司 | Preparation method of aldehyde-removing catalyst |
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| CN112774691A (en) * | 2021-01-27 | 2021-05-11 | 宁波方太厨具有限公司 | Preparation method of aldehyde-removing catalyst |
| CN114395413A (en) * | 2022-01-21 | 2022-04-26 | 上海绿强新材料有限公司 | Compound purifying agent for removing sulfur, arsenic and mercury at normal temperature and preparation and application thereof |
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