AU2020203664B2 - Magnetic selenium doped iron-sulfur composite and preparation method and application thereof - Google Patents
Magnetic selenium doped iron-sulfur composite and preparation method and application thereof Download PDFInfo
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- 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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- 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
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- 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
- B01J20/0262—Compounds of O, S, Se, Te
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- 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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
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Abstract
The invention discloses a magnetic selenium doped iron-sulfur composite. The chemical
formula of the composite is Fe(1-x)SeyS(1-y), wherein x=0.42-0.58, and y=0.01-0.2. The
preparation method comprises the steps that ferrous salt and thiourea are taken and dissolved
into water to form a first solution; soluble selenite is taken and dissolved into an ethylene
glycol solution to form a second solution; the first solution and the second solution are mixed
uniformly and added into a reaction kettle for a hydrothermal reaction, and a product of the
hydrothermal reaction is subjected to magnetic separating, washing and drying, and the
magnetic selenium doped iron-sulfur composite is obtained. The magnetic selenium doped
iron-sulfur composite has the excellent sulfur resistance, water resistance and the like, and
still has the high mercury removal efficiency in complex actual smelting flue gas.
1
DRAWINGS
4
e Fe
3 S,
3
Se
Se Fe
0
0 5 10 15 20
Energy (keV)
FIG. 3
100
90
80
70
60
50
40
30
20
10
01
FIG. 4
2
Description
4 e Fe 3 S, 3
Se
Se Fe
0 5 10 15 20 Energy (keV)
FIG. 3
100 90 80 70 60 50 40 30 20 10 01
FIG. 4
[0001] The invention relates to the field of mercury pollution emission control and flue gas
treatment, in particular to a magnetic selenium doped iron-sulfur composite applicable to the
capture of gaseous mercury in flue gas in the smelting industry and a preparation method
thereof.
[0002] Mercury is a heavy metal that has a great harm to human health and the ecological
environment; how to control atmospheric mercury emissions has become one of the hotspots
in the world. China emits a large amount of atmospheric mercury, and the smelting industry is
one of the main sources of atmospheric mercury pollution in China. During the
high-temperature combustion process, most of the mercury in the fuel or ore volatilizes into
the flue gas and exists in three forms: element state (Hg), oxidation state (Hg2 ), and
particulate state (HgP). Among them, Hg 2 and HgP are removed in wet purification process
and flue gas dust removal process, respectively, and Hg° is difficult to be removed in
conventional flue gas purification facilities due to its high chemical stability and insoluble
properties. Therefore, the efficient removal of Hg° in flue gas is the key and difficult point of
smelting flue gas mercury reduction.
[0003] In smelting and other industries, KI solution or HgCl2 solution absorption method are
often used to remove Hg° in flue gas at present; however, after the mercury-containing flue
gas is treated by this method, the mercury content in the flue gas fluctuates greatly, and the
mercury concentration is still high, and the operating cost is high. In order to achieve the
efficient removal of Hgo in flue gas, Hgo is adsorbed and converted into HgP by an adsorbent,
and then concentrated and captured by the existing flue gas dust collection system. At present,
some preparation methods and applications of mercury removal adsorbents have been
DESCRIPTION disclosed in certain patents. For example, Chinese patent ZL 201811095159.0 discloses an
activation and regeneration method of a metal sulfide mercury removal adsorbent, wherein
soluble divalent copper ion activated metal sulfide is used to treat mercury-containing flue
gas; the adsorbent after adsorbing mercury can be regenerated by high-temperature roasting
combined with activation of divalent copper; Chinese patent ZL201811376780.4 discloses a
method for catalytic oxidation of cobalt sulfide/biomass carbon composite material to remove
gaseous mercury in flue gas, wherein cobalt sulfide/biomass carbon composite material is
used to catalyze and oxidize elemental mercury in flue gas; Chinese patent
ZL201610944690.5 discloses a method for preparing a composite high-activity
mercury-removing adsorbent, wherein copper chloride is used to modify fly ash and copper
oxide is loaded on attapulgite to achieve efficient adsorption of elemental mercury. Although
the above adsorbents can remove mercury in smelting flue gas; however, the high cost of
preparation and non-recyclability of cobalt-sulfur compounds have led to higher mercury
removal costs; in addition, although traditional copper chloride modified fly ash has a low
cost; however, its active copper adsorption site is susceptible to the concentration of sulfur
dioxide in oxygen. These shortcomings limit application scope. Therefore, there is an urgent
need to develop a novel sulfur-resistant, efficient, and inexpensive adsorbent material to
achieve efficient adsorption and removal of mercury in a high-sulfur atmosphere.
[0004] In view of the shortcomings of the prior art, the objective of the invention is to
provide a magnetic selenium doped iron-sulfur composite for mercury removal in flue gas,
which is particularly suitable for the adsorption and removal of gaseous elemental mercury in
high-sulfur smelting flue gas. Another objective of the invention is to provide a preparation
method of the magnetic selenium doped iron-sulfur composite to obtain such mercury
removal adsorption materials at low cost.
[0005] In order to solve the technical issues above, the invention provides the technical
solutions as follows: a magnetic selenium doped iron-sulfur composite, wherein the chemical
formula thereof is Fe(1-x)SeyS(1-y), wherein x=0.42-0.58, and y=0.01-0.2.
[0006] Preferably, x=0.42-0.50, and y=0.05-0.15.
[0007] A preparation method of the magnetic selenium doped iron-sulfur composite above,
comprising the following steps:
[0008] 1) ferrous salt and thiourea are taken and dissolved into water to form a first solution;
soluble selenite is taken and dissolved into an ethylene glycol solution to form a second
solution;
[0009] 2) the first solution and the second solution are mixed uniformly and added into a
reaction kettle for a hydrothermal reaction, and a product of the hydrothermal reaction is
subjected to magnetic separating, washing and drying, and the magnetic selenium doped
iron-sulfur composite is obtained.
[0010] Preferably, the molar ratio of ferrous salt, thiourea and selenite in the mixed solution
of the first solution and the second solution is 1:(1.5-2): (0.1-0.5).
[0011] Preferably, the mixing volume ratio of the first solution and the second solution is
1:(1-2).
[0012] Preferably, the reaction temperature of the hydrothermal reaction is 160-220°C, and
the reaction time is 16-24 hours.
[0013] Preferably, the ferrous salt is one or more of ferrous sulfate, ferrous nitrate and ferrous
chloride, and the soluble selenite is one or two of sodium selenite and potassium selenite.
[0014] The invention further provides an application of the magnetic selenium doped
iron-sulfur composite above in mercury removal, in particular in mercury removal in
smelting flue gas.
[0015] Preferably, the smelting flue gas is treated by the wet dust collection process, and the
magnetic selenium doped iron-sulfur composite is sprayed into the flue gas at the early stage
of the wet dust collection process.
[0016] The magnetic selenium doped iron-sulfur composite of the invention is suitable for the
capture of gaseous elemental mercury and divalent mercury in industrial flue gas. The
appropriate temperature range should be selected during capture, and it can be carried out at
-250 °C ; preferably, the flue gas temperature during the mercury removal process is
160-220°C.
[0017] The magnetic selenium doped iron-sulfur composite of the invention can be
formulated by Fe(1-x)SeyS(1-y), wherein x=0.42-0.58, and y0.01-0.2. The prepared
DESCRIPTION composite is a selenium doped pyrrhotite structure, which has high adsorption activity for
flue gas mercury and high resistance to sulfur dioxide, water vapor and other components in
flue gas. The composite is directly sprayed into the flue gas and recovered in the wet dust
removal system, and the obtained dust can be separated by a magnetic separation method of
selenium doped iron-sulfur composite, thereby achieving directional capture of mercury in
the flue gas. The adsorption mechanism of the prepared magnetic selenium doped iron-sulfur
composite Fe(1-x)SeyS(1-y) to gaseous mercury is: through lattice replacement, the highly
active selenium loaded on the composite can be directly combined with elemental mercury in
the flue gas to form a stable selenium mercury compound, thereby finally achieving efficient
selective adsorption and capture of mercury in the high-sulfur flue gas.
[0018] Compared with the prior art, the advantages of the invention are mainly as follows:
[0019] (1) The magnetic selenium doped iron-sulfur composite has excellent sulfur resistance,
water resistance and the like, and still has high mercury removal efficiency in complex
smelting flue gas.
[0020] (2) The magnetic selenium doped iron-sulfur composite of the invention has the
characteristics of high efficiency, low cost, and environmental friendliness during the
mercury removal process, and efficient selective adsorption and capture of mercury in
high-sulfur flue gas (SO 2 concentration within 15v%) can be realized.
[0021] (3) The magnetic selenium doped iron-sulfur composite of the invention can be
widely applied in the field of non-ferrous smelting flue gas mercury removal, and has a wide
range of application; at the same time, it can be directly applied to the existing flue gas
treatment equipment without changing the existing treatment process.
[0022] In order to more clearly explain the embodiments of the invention or the technical
solutions in the prior art, the drawings of the embodiments or the prior art will be briefly
introduced hereinafter.
[0023] FIG. 1 is a hysteresis graph of FeS1.72 prepared in Comparative Embodiment 1 and
Feo.s2Seo.oSo.94 prepared in Embodiment 1 of the invention.
[0024] FIG. 2 is an SEM of Feo.s2Seo.o6So.94 prepared in Embodiment 1 of the invention.
[0025] FIG. 3 is an EDX graph of Feo.2Seo.o6So.94 prepared in Embodiment 1 of the invention.
[0026] FIG.4 is a graph of the effect of different selenium loadings on the removal of
elemental mercury;
[0027] FIG. 5 is a graph of the effect of different adsorption temperatures on the mercury
removal efficiency of Feo.2Seo.6So.94.
[0028] In order to facilitate the understanding of the invention, the invention will be
described more fully and meticulously with reference to the drawings and preferred
embodiments of the specification hereinafter, but the protection scope of the invention is not
limited to the following specific embodiments.
[0029] Unless otherwise defined, all technical terms used below have the same meaning as
commonly understood by those skilled in the art. The technical terms used in the
specification are only for describing specific embodiments, and are not intended to limit the
protection scope of the invention.
[0030] Unless otherwise specified, various raw materials, reagents, instruments and
equipment used in the invention can be purchased from the market or can be prepared by
existing methods.
[0031] Embodiment 1
[0032] The embodiment provides a preparation method of the magnetic selenium doped
iron-sulfur composite mercury removal material, comprising the following steps:
[0033] 1) 0.01 mol of ferrous nitrate and 0.032 mol of thiourea are taken into 30 mL of
deionized water and are stirred for 10 min to be fully dissolved, to form a first solution;
[0034] 2) 0.008 mol of sodium selenite are taken into 30 mL of ethylene glycol solution and
are ultrasonically stirred for 10 min to be fully dissolved, to form a second solution;
[0035] 3) the first solution and the second solution are mixed and are ultrasonically stirred for
min, and added into the PTFE lining of a 100 mL of reaction kettle, then it is sealed and
placed into an oven, and is reacted at 180°C for 18 h; after reaction, it is naturally cooled to
room temperature, and then the mixed solution is taken out, and the synthesized selenium
doped iron-sulfur composite is obtained by centrifugal separation and magnetic separation;
DESCRIPTION then, carbon disulfide and ethanol are used to wash the selenium doped iron-sulfur composite to remove excess elemental sulfur and selenium, and finally the sample is dried. After chemical analysis, the molar mass ratio of Fe, Se and S elements in the sample is measured, and the sample is determined and labeled as Fe.s2Seo.o6 So. 94
[0036] Embodiment 2
[0037] The process of this embodiment is basically the same as that of Embodiment 1, comprising the following steps:
[0038] 1) 0.01 mol of ferrous nitrate and 0.025 mol of thiourea are taken into 30 mL of deionized water and are stirred for 10 min to be fully dissolved, to form afirst solution;
[0039] 2) 0.015 mol of sodium selenite are taken into 30 mL of ethylene glycol solution and are ultrasonically stirred for 10 min to be fully dissolved, to form a second solution;
[0040] 3) the first solution and the second solution are mixed and are ultrasonically stirred for min, and added into the PTFE lining of a 100 mL of reaction kettle, then it is sealed and placed into an oven, and is reacted at 200°C for 18 h; after reaction, it is naturally cooled to room temperature, and then the mixed solution is taken out, and the synthesized selenium doped iron-sulfur composite is obtained by centrifugal separation and magnetic separation; then, carbon disulfide and ethanol are used to wash the selenium doped iron-sulfur composite to remove excess elemental sulfur and selenium, and finally the sample is dried.
[0041] After chemical analysis, the molar mass ratio of Fe, Se and S elements in the sample is measured, and the sample is determined and labeled as Feo.Seo.13 So. 87 .
[0042] Comparative Embodiment 1
[0043] The process of this comparative embodiment is basically the same as that of Embodiment 1, comprising the following steps:
[0044] 1) 0.01 mol of ferrous nitrate and 0.04 mol of thiourea are taken into 30 mL of deionized water and are stirred for 10 min to be fully dissolved; 30 mL of ethylene glycol solution is added to the solution, and they are ultrasonically stirred to form a homogeneous solution;
[0045] 2) the obtained mixed solution is added into the PTFE lining of a 100 mL of reaction kettle, then it is sealed and placed into an oven, and is reacted at 180 °C for 18 h; after reaction, it is naturally cooled to room temperature, and then the mixed solution is taken out,
DESCRIPTION and the synthesized selenium doped iron-sulfur composite is obtained by centrifugal separation and magnetic separation; then, carbon disulfide and ethanol are used to wash the selenium doped iron-sulfur composite to remove excess elemental sulfur and selenium, and finally the sample is dried.
[0046] After chemical analysis, the molar mass ratio of Fe and S elements in the sample is measured, and the sample is determined and labeled as FeSe.72.
[0047] FIG. 1 shows the changes in magnetic characteristics of the samples of FeS1.72 of Comparative Embodiment 1 and Feo.s2Seo.oSo.94 of Embodiment 1. It can be seen from the
figure that although the magnetism of the selenium doped iron-sulfur composite is relatively lower than that of the iron-sulfur composite without selenium, however, the saturation magnetic strength can still reach 5 emg/g, which shows that the selenium doped iron-sulfur composite still has excellent magnetic properties and is a magnetically recycled material. FIG. 2 and FIG. 3 show the SEM and EDX graphs of the sample Feo.s2Seo.o6So.94, respectively. It
can be seen that the Feo.2Seo.oSo.94 composite material is a sphere with a particle size of
about 500 nm, and the sphere indicates that some lamellar samples are adhered. With reference to the analysis of EDX graph, the sample is mainly composed of Fe, Se and S elements, which also proves the successful doping of selenium.
[0048] Comparative Embodiment 2
[0049] The process of this comparative embodiment is basically the same as that of Embodiment 1, comprising the following steps:
[0050] 1) 0.01 mol of ferrous nitrate are taken into 30 mL of deionized water and are stirred for 10 min to be fully dissolved; to form afirst solution;
[0051] 2) 0.03 mol of sodium selenite are taken into 30 mL of ethylene glycol solution and are ultrasonically stirred for 10 min to be fully dissolved, to form a second solution;
[0052] 3) the first solution and the second solution are mixed and are ultrasonically stirred for min, and added into the PTFE lining of a 100 mL of reaction kettle, then it is sealed and placed into an oven, and is reacted at 180°C for 18 h; after reaction, it is naturally cooled to room temperature, and then the mixed solution is taken out, and the synthesized selenium doped iron-sulfur composite is obtained by centrifugal separation and magnetic separation; then, carbon disulfide and ethanol are used to wash the selenium doped iron-sulfur composite
DESCRIPTION to remove excess elemental sulfur and selenium, and finally the sample is dried.
[0053] After chemical analysis, the molar mass ratio of Fe and S elements in the sample is measured, and the sample is determined and labeled as FeSe2.
[0054] Application Embodiment 1
[0055] 100 mg of Feo.s2Seo.6So.94 in Embodiment 1, Feo.s6Seo.13So.87 in Embodiment 2, FeS.72
in Comparative Embodiment 1, and FeSe2 in Comparative Embodiment 2 samples are taken, respectively; the effects of different doping levels on elemental mercury removal in flue gas are observed, and the reaction results are shown in FIG. 4. The experimental conditions are: the elemental mercury concentration in flue gas is 600 [g/m3 , the flue gas flow rate is 800 mL/min, the reaction temperature is 180°C, and the reaction time is 5 h.
[0056] It can be seen from FIG. 4 that, compared with FeS1.72 and FeSe2materials, the selenium doped modified iron-sulfide composite has a higher adsorption efficiency for mercury, which shows that the selenium doped iron-sulfur composite mercury removal material has an excellent mercury removal effect.
[0057] Application Embodiment 2
[0058] 100 mg of Feo.s2Seo.oSo.94 sample are taken, the effects of different doping levels on
elemental mercury removal in flue gas are observed, and the reaction results are shown in FIG. 5. The experimental conditions are: the elemental mercury concentration in flue gas is 600 [g/m 3, the flue gas flow rate is 800 mL/min, and the reaction time is 5 h.
[0059] It can be seen from FIG. 5 that when the temperature exceeds 220°C, the adsorption efficiency of mercury decreases significantly; however, when the adsorption temperature is lower than 220°C, the modified selenium doped iron-sulfide can effectively remove mercury; that is, the synthesized modified selenium doped iron-sulfur composite can achieve efficient mercury removal in a wide temperature range.
2020203664
Claim pages are not consecutively numbered. They should be numbered 9 and 10
Claims (10)
1. A magnetic selenium doped iron-sulfur composite being an adsorbent material for
removing mercury from high-sulfur flue gas, wherein the chemical formula thereof is Fe(1
x)SeyS(1-y), wherein x=0.42-0.58, and y=0.01-0.2.
2. The magnetic selenium doped iron-sulfur composite being an adsorbent material for
removing mercury from high-sulfur flue gas according to claim 1, wherein x=0.42-0.50, and
y=0.05-0.15.
3. A preparation method of the magnetic selenium doped iron-sulfur composite being an
adsorbent material for removing mercury from high-sulfur flue gas according to claim 1 or 2,
comprising the following steps:
1) ferrous salt and thiourea are taken and dissolved into water to form a first solution; soluble
selenite is taken and dissolved into an ethylene glycol solution to form a second solution;
2) the first solution and the second solution are mixed uniformly and added into a reaction
kettle for a hydrothermal reaction, and a product of the hydrothermal reaction is subjected to
magnetic separating, washing and drying, and the magnetic selenium doped iron-sulfur
composite is obtained.
4. The preparation method according to claim 3, wherein the molar ratio of ferrous salt,
thiourea and selenite in the mixed solution of the first solution and the second solution is
1:(1.5-2): (0.1-0.5).
5. The preparation method according to claim 3, wherein the mixing volume ratio of the first
solution and the second solution is 1:(1-2).
6. The preparation method according to claim 3, wherein the reaction temperature of the
hydrothermal reaction is 160-220°C , and the reaction time is 16-24 hours.
7. The preparation method according to claim 3, wherein the ferrous salt is one or more of
ferrous sulfate, ferrous nitrate and ferrous chloride, and the soluble selenite is one or two of
Appl. No.2020203664 Amdt. Dated February 24, 2022 Reply to Office action of February 26, 2021 sodium selenite and potassium selenite.
8. An application of the magnetic selenium doped iron-sulfur composite being an adsorbent
material for removing mercury from high-sulfur flue gas according to claim 1 or 2 or
prepared by the preparation method of any one of claims 3 to 7 in mercury removal.
9. The application according to claim 8, wherein the mercury removal refers to mercury
removal in smelting flue gas.
10. The application according to claim 9, wherein the smelting flue gas is treated by the wet
dust collection process, and the magnetic selenium doped iron-sulfur composite is sprayed
into the flue gas at the early stage of the wet dust collection process.
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| CN114100634B (en) * | 2021-12-14 | 2023-11-10 | 宁波碧城生态科技有限公司 | Preparation method, product and application of magnetic multi-component iron-carbon composite Fenton-like catalyst |
| CN115845789A (en) * | 2022-09-13 | 2023-03-28 | 浙江慧科环保科技有限公司 | Preparation method of sulfur deposition type iron-based heavy metal adsorption material |
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| US20160332108A1 (en) * | 2015-05-14 | 2016-11-17 | Chevron U.S.A. Inc. | Process, method, and system for removing mercury from fluids |
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