CN110327874A - A kind of compound Fe-Ce oxide dearsenification adsorbent of core-shell structure and its preparation method and application - Google Patents
A kind of compound Fe-Ce oxide dearsenification adsorbent of core-shell structure and its preparation method and application Download PDFInfo
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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Abstract
The invention discloses a kind of compound Fe-Ce oxide dearsenification adsorbents of core-shell structure, are with magnetic Nano Fe3O4For kernel, in magnetic Nano Fe3O4Surface is coated with compound iron cerium oxide layer；The molar ratio of ferro element and Ce elements is 1:(0.04~0.12 in Fe-Ce oxide layer).The preparation method of dearsenification adsorbent of the invention: by magnetic Nano Fe3O4, m-phenylene diamine (MPD) and formaldehyde be added in solution, carry out home position polymerization reaction, obtain sample A；Sample A is subjected to high temperature cabonization, obtains sample B；Ferric nitrate and cerous nitrate mixed solution are supported on sample B by infusion process, obtain sample C；Sample C is subjected to oxidizing roasting, obtains dearsenification adsorbent.The compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention can realize the Direct Acquisition to gaseous state arsenic in larger temperature range, and to the adsorption efficiency of arsenic up to 80% or more, and after adsorbing arsenic high stability, reduce the secondary pollution of arsenic.
Description
Technical field
It is suitable for handling the production of non-ferrous metal metallurgy pyrometallurgical smelting process the invention belongs to absorbent fields more particularly to one kind
The adsorbent of raw arsenical fume.
Background technique
Since arsenic has severe toxicity, the problem of efficient control of arsenic pollution discharge has become urgent need to resolve how is realized.I
" national arsenate minerals technical policy ", " planning of heavy metal pollution integrated control " 12th Five-Year Plan " ", " heavy metal pollution that state puts into effect
Prevent and treat unified plan (2011-2015) ", in a series of file such as " " 13 " ecological environmental protection planning " clearly by arsenic
It is classified as main prevention and control object, arsenate minerals have become the great livelihood issues of domestic and international focus and China.In metal
In mineral smelting process, most of arsenic element is oxidized and is volatized into flue gas with the formation of arsenic trioxide in ore, into
And form arsenical fume.
Arsenic mainly removes during dedusting and wet scrubbing in flue gas during smelting at present, arsenic be transferred to from flue gas cigarette ash and
In waste acid, there are still arsenic pollution risks, and therefore, the Direct Acquisition and Selective Separation that gaseous state arsenic is captured from flue gas become control
The main direction of studying of arsenic pollution processed.Chinese patent 201711220671.9 discloses a kind of preparation side of flue gas dearsenification adsorbent
Adsorbent is prepared in method, the processes such as, granulation uniformly mixed using calcium oxide, metallurgical slag, zeolite and flyash, heating；In
State's patent 201810285567.6 discloses a kind of arsenic adsorbent and its preparation method and application, to there is alumina support to use iron
Element dipping and high-temperature roasting, are prepared into gaseous state arsenic adsorbent.Although the absorption to gaseous state arsenic may be implemented in above-mentioned adsorbent, but
Adsorbent after arsenic-adsorbing is still mixed with flue dust or waste acid, it is difficult to the problem of controllably separating, and being faced with arsenic secondary pollution.This
Outside, traditional adsorbent material is not high to the adsorption capacity and the rate of adsorption of gaseous state arsenic, it is difficult to meet the needs of in actual industrial.Cause
This needs the adsorbent material for developing stable, efficient and easy recycling.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The preparation method of efficient dearsenification adsorbent and the application method of adsorbent capture gaseous state arsenic can be recycled in kind, is suitble to Combustion in High Temperature High Sulfur smelting
Refine the efficient capture and separation of gaseous state arsenic in flue gas.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of compound Fe-Ce oxide dearsenification adsorbent of core-shell structure, is with magnetic Nano Fe3O4For kernel, received in magnetism
Rice Fe3O4Surface is coated with compound iron cerium oxide layer；The molar ratio of ferro element and Ce elements is 1 in Fe-Ce oxide layer:
(0.04~0.12).
The present invention also provides a kind of preparation methods of above-mentioned dearsenification adsorbent, comprising the following steps:
(1) by magnetic Nano Fe3O4, m-phenylene diamine (MPD) and formaldehyde be added in solution, ultrasonic mixing is uniform, in mechanical stirring
Lower carry out home position polymerization reaction, obtains sample A；
(2) sample A is subjected to high temperature cabonization, obtains the sample B of porous carbon material package；
(3) ferric nitrate and cerous nitrate mixed solution are supported on sample B by infusion process, are dried, are loaded
The sample C of iron cerium；
(4) sample C is carried out to oxidizing roasting under oxidizing atmosphere to get the dearsenification adsorbent is arrived.
Above-mentioned preparation method, it is preferred that in the step (1), magnetic Nano Fe3O4Partial size be 50~200nm.
Above-mentioned preparation method, it is preferred that in the step (1), the molar ratio of m-phenylene diamine (MPD) and formaldehyde be 1:(1.5~
3), mixed solution pH is 8~9, and the home position polymerization reaction time is 18~30h.
Above-mentioned preparation method, it is preferred that in the step (2), the maturing temperature of high temperature cabonization is 600~700 DEG C, is protected
The warm time is 1.5~3 hours；High temperature cabonization carries out under the protection of nitrogen, and nitrogen flow rate is 0.5~1L/min.
Above-mentioned preparation method, it is preferred that in the step (3), the molar ratio of iron ion and cerium ion be 1:(0.04~
0.12), ferric nitrate and cerous nitrate mixed solution and sample B volume ratio are 1:(1~1.5), dipping temperature is 25~50 DEG C, dipping
Time is 30~60min.
Above-mentioned preparation method, it is preferred that in the step (4), the temperature of oxidizing roasting is 600~800 DEG C, when roasting
Between be 20~40min, oxygen concentration be 20~40%.
The inventive concept total as one, the present invention also provides a kind of above-mentioned or prepared by above-mentioned preparation method de-
Dearsenification adsorbent Direct Uniform is sprayed into cigarette in flue gas dust collection technique front end by application of the arsenic adsorbent in Combustion in High Temperature High Sulfur flue gas
In gas, adsorbent and flue gas after arsenic-adsorbing enter flue dust in dust pelletizing system together, obtain the flue dust of mixing containing arsenic, then pass through
Composite magnetic adsorbent is recycled in magnetic separation separation from the flue dust of mixing containing arsenic.
Above-mentioned application, it is preferred that the temperature that dearsenification adsorbent carries out flue gas when dearsenification is 400~1200 DEG C, in flue gas
Sulfur dioxide concentration is not higher than 10%.
The compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention is with magnetic Fe3O4Particle is kernel, passes through table
Face in-situ polymerization is in Fe3O4Microparticle surfaces form one layer of resin of package, and the porous carbon of surface porosity is formed after high temperature cabonization
Shell, high temperature cabonization process form a variety of functional groups such as amino, carboxyl, have certain adsorption capacity to metal ion, guarantee to pass through
Infusion process realizes the payload of iron cerium, finally by oxidizing roasting, by porous carbon layer oxygenolysis, and the iron cerium conversion adsorbed
At porous high activity x (CeO2)·y(Fe2O3) (wherein x/y is (0.08~0.24): 1) composite oxides, i.e. final product
For with Fe3O4For kernel and with porous x (CeO2)·y(Fe2O3) composite oxides be shell composite adsorbing material, gas in flue gas
State As2O3It can be by CeO2Efficient oxidation is at As2O5, and and Fe2O3It is formed and stablizes ferric arsenate, to realize efficiently catching for gaseous state arsenic
It obtains.Compound adsorbent small size and the rate of adsorption that ensure that arsenic rich in hole physical features, highly active Fe cerium composite oxides
Guarantee the efficient capture of arsenic, the magnetic kernel of composite adsorbing material ensure that the recuperability of adsorbent.
Compared with the prior art, the advantages of the present invention are as follows:
(1) the compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention can be realized in larger temperature range to gas
The Direct Acquisition of state arsenic, and to the adsorption efficiency of arsenic up to 80% or more, and after adsorbing arsenic high stability, reduce arsenic
Secondary pollution.
(2) the compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention can extensively should in smelt and coal-fired flue-gas
Dearsenification field, it is applied widely, while may be directly applied in existing fume treatment auxiliary, have no need to change existing processing work
Skill.
(3) the compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention can be recycled after desorption, reduce
The cost of dearsenification.
(4) present invention has many advantages, such as that preparation process is simple, adsorption efficiency is high, environmentally friendly.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with preferred embodiment and more comprehensively, is meticulously retouched
It states, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
The preparation method of the compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention, comprising the following steps:
(1) taking 30mg partial size is the Fe of 100nm3O4Particulate matter is placed it in containing 0.02mol m-phenylene diamine (MPD) and 0.04mol
It the use of aqueous ammonia conditions mixed solution to pH is 8.5, and reacted 24 hours under continuous mechanical stirring, vacuum in the solution of formaldehyde
It after being dried in drying box, is placed in tube furnace, be carbonized at 650 DEG C 3h under nitrogen protection atmosphere, obtains porous charcoal package
Fe3O4@C adsorbent.
(2) the mixed solution 20mL of different iron cerium molar ratios is prepared, and by itself and the Fe for preparing3O4@C mixing, by iron cerium
Ionic impregnation is to Fe3O4On@C, moisture removal is removed in drying, finally obtains the compound adsorbent of different iron cerium impregnation increments；
(3) composite adsorbent material is placed in tube furnace, the gas that oxygen content is 30% is passed through, with heating rate
650 DEG C are heated to for 10 DEG C/min, then soaking time is 30min, finally obtains the Fe of the core-shell structure of different iron cerium ratios3O4@
x(CeO2)·y(Fe2O3) adsorbent.
The Fe of 20mg difference iron cerium ratio is taken respectively3O4@x(CeO2)·y(Fe2O3) adsorbent, adsorbent and simulation are contained into arsenic
Flue gas is injected to together in the quartz ampoule in Muffle furnace, collects adsorbent in quartzy pipe end installation filter cloth.Item in experimentation
Part are as follows: in simulated flue gas arsenic content be 0.2mg, flue gas flow rate 0.1L/min, flue-gas temperature be 600 DEG C, in flue gas gas at
For 20%O2+ 5%SO2+ 55%N2, the different adsorbents of synthesis are as shown in table 1 to the capture rate of arsenic.
The compound adsorbent of the different iron cerium ratios of table 1 compares arsenic adsorption efficiency
Table 1 is comparison of the different iron ceriums than compound adsorbent to arsenic capture rate.As can be seen from the table, cerium in adsorbent
When content is lower (iron cerium ratio be 1:0.02), the capture rate of arsenic is only 30.6%, suitable cerium can promote arsenic oxidation and
Absorption, the capture rate of arsenic can be significantly improved by improving cerium content.When iron cerium ratio is 1:0.16, arsenic capture rate is instead at this time
Decline, this illustrates that suitable iron cerium compares compound adsorbent and plays a crucial role to the capture rate of arsenic.
Embodiment 2:
The preparation method of the compound Fe-Ce oxide dearsenification adsorbent of core-shell structure of the invention, comprising the following steps:
(1) taking 30mg partial size is the Fe of 100nm3O4Particulate matter is placed it in containing 0.02mol m-phenylene diamine (MPD) and 0.04mol
It the use of aqueous ammonia conditions mixed solution to pH is 8.5, and reacted 24 hours under continuous mechanical stirring, true in the solution of formaldehyde
It after being dried in empty drying box, is placed in tube furnace, be carbonized at 650 DEG C 3h under nitrogen protection atmosphere, obtains porous charcoal package
Fe3O4@C adsorbent；
(2) the mixed solution 20mL that configuration iron cerium molar ratio is 1:0.06, and by itself and the Fe for preparing3O4@C mixing, will
Iron cerium ion is impregnated into Fe3O4On@C, moisture removal is removed in drying, obtains composite material；
(3) composite material is placed in tube furnace, the gas that oxygen content is 30% is passed through, with heating rate for 10
DEG C/min is heated to 650 DEG C, then soaking time is 30min, finally obtains the Fe of core-shell structure3O4@0.12(CeO2)·
(Fe2O3) adsorbent.Take 20mg Fe3O4@0.12(CeO2)·(Fe2O3) adsorbent.
Take the Fe prepared in the present embodiment3O4@0.12(CeO2)·(Fe2O3) 20mg, by adsorbent and simulation arsenical fume
It is injected in the quartz ampoule in Muffle furnace, collects adsorbent in quartzy pipe end installation filter cloth.Experimentation conditional are as follows: simulation
Arsenic content is 0.2mg in flue gas, and flue gas flow rate 0.1L/min, flue-gas temperature is 600 DEG C, by changing smoke components and reaction
Temperature investigates Fe under different condition3O4@0.12(CeO2)·(Fe2O3) to the capture rate of arsenic, concrete outcome is as shown in table 2.
2 different technology conditions of table compare arsenic adsorption efficiency
Table 2 be different atmosphere and capture at a temperature of arsenic acquisition performance comparison, as can be seen from the table, in flue gas oxygen and
The presence of sulfur dioxide all plays facilitation to the capture of arsenic, and there is oxygen and sulfur dioxide in practical flue gas during smelting,
Therefore core-shell structure Fe3O4@0.12(CeO2)·(Fe2O3) compound adsorbent is quite suitable for the capture of arsenic in flue gas during smelting.It catches
Obtaining temperature is also a parameter important in practical application, is all unfavorable for the capture of arsenic when flue-gas temperature is lower and higher, most preferably
Arsenic capture temperature be 600~800 DEG C, the capture rate of arsenic is 80% or more.But reaction temperature is between 400~1200 DEG C
The capture rate of arsenic is still maintained at 60% or more, i.e., still has practical application value.
The Fe for taking 40mg to prepare3O4@0.12(CeO2)·(Fe2O3), adsorbent and simulation arsenical fume are injected to its dress
In the quartz ampoule being placed in Muffle furnace, adsorbent is collected in quartzy pipe end installation filter cloth.Experimentation conditional are as follows: mould
Arsenic content is 0.2mg in quasi- flue gas, and flue gas flow rate 0.1L/min, flue-gas temperature is 600 DEG C, sulfur dioxide concentration 5%, oxygen
Gas concentration is 20%.After this adsorption experiment, adsorbent is regenerated using alkaline hydrolysis adsorption desorption arsenic and process of thermal activation, and
Adsorbent is measured under the same terms to the capture rate of gas phase arsenic, so circulation 5 times, concrete outcome is as shown in table 3.From table 3
It can be seen that the increase with cycle-index in although, compound adsorbent has certain decline to the capture rate of arsenic, passes through 5
After secondary circulation, adsorbent can still remain 64.23% to the adsorption efficiency of arsenic, this also illustrates that core-shell structure prepared by the present invention is multiple
Closing Fe-Ce oxide adsorbent has excellent recycling performance.
3 magnetic coupling Fe of table3O4@0.12(CeO2)·(Fe2O3) sorbent circulation performance
Claims (9)
1. a kind of compound Fe-Ce oxide dearsenification adsorbent of core-shell structure, which is characterized in that the dearsenification adsorbent is with magnetism
Nanometer Fe3O4For kernel, in magnetic Nano Fe3O4Surface is coated with compound iron cerium oxide layer；Iron in the Fe-Ce oxide layer
The molar ratio of element and Ce elements is 1:(0.04~0.12).
2. a kind of preparation method of dearsenification adsorbent as described in claim 1, which comprises the following steps:
(1) by magnetic Nano Fe3O4, m-phenylene diamine (MPD) and formaldehyde be added in solution, ultrasonic mixing is uniform, under mechanical stirring into
Row home position polymerization reaction obtains sample A；
(2) sample A is subjected to high temperature cabonization, obtains the sample B of porous carbon material package；
(3) ferric nitrate and cerous nitrate mixed solution are supported on sample B by infusion process, are dried, obtain load iron cerium
Sample C；
(4) sample C is carried out to oxidizing roasting under oxidizing atmosphere to get the dearsenification adsorbent is arrived.
3. preparation method as claimed in claim 2, which is characterized in that in the step (1), magnetic Nano Fe3O4Partial size be
50~200nm.
4. preparation method as claimed in claim 2, which is characterized in that in the step (1), mole of m-phenylene diamine (MPD) and formaldehyde
Than for 1:(1.5~3), mixed solution pH is 8~9, and the home position polymerization reaction time is 18~30h.
5. preparation method as claimed in claim 2, which is characterized in that in the step (2), the maturing temperature of high temperature cabonization is
600~700 DEG C, soaking time is 1.5~3 hours；High temperature cabonization carries out under the protection of nitrogen, and nitrogen flow rate is 0.5~1L/
min。
6. preparation method as claimed in claim 2, which is characterized in that in the step (3), mole of iron ion and cerium ion
Than for 1:(0.04~0.12), ferric nitrate and cerous nitrate mixed solution and sample B volume ratio are 1:(1~1.5)；Dipping process
Dipping temperature is 25~50 DEG C, and dip time is 30~60min.
7. preparation method as claimed in claim 2, which is characterized in that in the step (4), the temperature of oxidizing roasting is 600
~800 DEG C, calcining time is 20~40min, and oxygen concentration is 20~40%.
8. a kind of as described in claim 1 or by the described in any item dearsenification adsorbents of claim 2~7 in Combustion in High Temperature High Sulfur
Application in flue gas, which is characterized in that in flue gas dust collection technique front end by the penetrating flue gas of dearsenification adsorbent Direct Uniform, inhale
Adsorbent and flue gas after attached arsenic enter flue dust in dust pelletizing system together, obtain the flue dust of mixing containing arsenic, then pass through magnetic separation point
From the recycling composite magnetic adsorbent from the flue dust of mixing containing arsenic.
9. application as claimed in claim 8, which is characterized in that the temperature range of flue gas is when dearsenification adsorbent carries out dearsenification
400~1200 DEG C, sulfur dioxide in flue gas concentration is not higher than 10%.
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| CN111135785A (en) * | 2020-01-07 | 2020-05-12 | 华北电力大学（保定） | Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111135785A (en) * | 2020-01-07 | 2020-05-12 | 华北电力大学（保定） | Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof |
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