CN112191226A - Method for preparing mercury removal adsorbent by modifying low-temperature plasma and application - Google Patents

Method for preparing mercury removal adsorbent by modifying low-temperature plasma and application Download PDF

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CN112191226A
CN112191226A CN202010896557.3A CN202010896557A CN112191226A CN 112191226 A CN112191226 A CN 112191226A CN 202010896557 A CN202010896557 A CN 202010896557A CN 112191226 A CN112191226 A CN 112191226A
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carbon
temperature plasma
based material
low
transition metal
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许洋
崔伟
张庆竹
杜林�
徐菲
李延伟
张世博
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Shandong University
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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
    • B01J20/06—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
    • 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
    • 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
    • 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
    • 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

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  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention discloses a method for preparing a demercuration adsorbent by modifying low-temperature plasma and application thereof, comprising the following steps: and crushing and screening the carbon-based material and the transition metal oxide, mixing the materials according to a set proportion, introducing oxygen, and performing low-temperature plasma treatment to obtain the mercury removal adsorbent. Meanwhile, the transition metal oxide and the carbon-based material are treated to generate a synergistic effect between the transition metal oxide and the carbon-based material, so that the dispersity of the active component is improved, more oxygen radicals are promoted to be released and effectively utilized, the utilization rate of the active radicals can be improved, and the energy utilization rate of low-temperature plasma is increased, which is the key for improving the mercury removal efficiency.

Description

Method for preparing mercury removal adsorbent by modifying low-temperature plasma and application
Technical Field
The invention belongs to the technical field of flue gas purification, and particularly relates to a method for preparing a mercury removal adsorbent by modifying low-temperature plasma and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
According to a newly published report on the global mercury assessment in 2018 by the environmental planning agency of the United nations, the emission of the global artificial mercury in 2015 is as high as 2220 tons (13.27 percent increase compared with 2010), wherein the emission of the mercury in the fire coal accounts for about 21 percent of the total emission of the global artificial mercury. In coal-fired flue gas, mercury mainly exists in three forms: elemental mercury (Hg)0) Mercury (Hg) in its oxidized state2+) And particulate mercury (Hg)P). Wherein Hg is2+Is very soluble in water, so that can be removed by a wet desulphurization device in a power plant, and Hg is easily removedPCan be captured by dust-removing devices (electrostatic dust-collector and bag-type dust-collector), and Hg0Because the smoke purifier is insoluble in water and high in volatility, the smoke purifier cannot remove the water and the high in volatility. The active carbon injection technology (ACI) is currently considered to remove Hg from flue gas0The most mature and effective method, but the activated carbon has the defects of small adsorption capacity and low adsorption rate. At present, the more common method is to perform impregnation modification on activated carbon, however, the traditional chemical impregnation process is complicated, time-consuming and costly, and may cause environmental pollution problems.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a method for preparing a mercury removal adsorbent by modifying low-temperature plasma based on a synergistic effect and application thereof.
To solve the above technical problem, one or more of the following embodiments of the present invention provide the following technical solutions:
in a first aspect, the invention provides a method for preparing a demercuration adsorbent by low-temperature plasma modification, which comprises the following steps:
and crushing and screening the carbon-based material and the transition metal oxide, mixing the materials according to a set proportion, introducing oxygen, and performing low-temperature plasma treatment to obtain the mercury removal adsorbent.
In a second aspect, the invention provides a demercuration adsorbent prepared by the method for preparing the demercuration adsorbent by low-temperature plasma modification.
In a third aspect, the invention provides application of the demercuration adsorbent in demercuration of flue gas.
Compared with the prior art, one or more technical schemes of the invention have the following beneficial effects:
(1) under the action of oxygen low-temperature plasma, oxygen is decomposed to generate active component oxygen free radicals, and compared with the carbon-based material which is treated independently, transition metal oxide is further added, so that the transition metal oxide can be converted into oxide with a higher valence state under the action of the oxygen free radicals. The increase of the valence state of the metal oxide can promote the decomposition rate of oxygen free radicals to be further improved, and meanwhile, in the later mercury removal process, the high-valence metal oxide can also oxidize elemental mercury, so that the mercury removal efficiency is improved.
(2) Compared with the method for processing the transition metal oxide alone, the addition of the carbon-based material can enable more oxygen radicals to be loaded on the carbon-based material to modify the carbon-based material, so that the utilization rate of the oxygen radicals is improved, namely the energy utilization rate of the low-temperature plasma is increased.
(3) Meanwhile, the transition metal oxide and the carbon-based material are treated to generate a synergistic effect between the transition metal oxide and the carbon-based material, so that the dispersity of the active component is improved, more oxygen radicals are promoted to be released and effectively utilized, the utilization rate of the active radicals can be improved, and the energy utilization rate of low-temperature plasma is increased, which is the key for improving the mercury removal efficiency.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Figure 1 is a flow diagram of the preparation of the demercuration sorbent of example 1.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In a first aspect, the invention provides a method for preparing a demercuration adsorbent by low-temperature plasma modification, which comprises the following steps:
and crushing and screening the carbon-based material and the transition metal oxide, mixing the materials according to a set proportion, introducing oxygen, and performing low-temperature plasma treatment to obtain the mercury removal adsorbent.
In some embodiments, the carbon-based material is activated carbon or biocoke.
In some embodiments, the transition metal oxide is ferrous oxide, cerium oxide, cobalt oxide, or manganese oxide.
In some embodiments, the mass ratio of the transition metal oxide to the carbon-based material is from 1:20 to 20: 1.
Further, the mass ratio of the transition metal oxide to the carbon-based material is 1:10-10: 1.
Furthermore, the mass ratio of the transition metal oxide to the carbon-based material is 1: 1-4.
In some embodiments, the time for the low temperature plasma treatment is 1-100 min.
Further, the time of low-temperature plasma treatment is 1-10 min.
In a second aspect, the invention provides a demercuration adsorbent prepared by the method for preparing the demercuration adsorbent by low-temperature plasma modification.
In a third aspect, the invention provides application of the demercuration adsorbent in demercuration of flue gas.
Example 1
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the biological coke and the ferrous oxide by a crusher;
(2) the biological coke and ferrous oxide are mixed according to the mass ratio of 1:1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, and treating for 3min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O is 48%, the content of ferrous oxide is 31.88%, and the content of ferric oxide is 68.12%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 72%.
Example 2
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the activated carbon and the manganese oxide by a crusher;
(2) mixing activated carbon and manganese oxide according to a mass ratio of 2: 1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, treating for 5min under the action of low-temperature plasma, and testing to obtain carbon-based material with oxygen-containing functional group C ═ O content of 61%, manganese sesquioxide content of 40.96% and manganese dioxide content of 59.04%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 87%.
Example 3
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the active carbon and the cerium oxide by a crusher;
(2) mixing activated carbon and cerium oxide according to a mass ratio of 2: 1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, and treating for 5min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 63%, the content of cerium oxide is 27.35%, and the content of cerium dioxide is 72.65%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 89%.
Example 4
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the biological coke and the cerium oxide by a crusher;
(2) mixing biological coke and cerium oxide according to a mass ratio of 1:1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, and treating for 10min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 67%, the content of cerium oxide is 24.64%, and the content of cerium dioxide is 75.36%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 91%.
Example 5
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the activated carbon and the manganese oxide by a crusher;
(2) mixing activated carbon and manganese oxide according to a mass ratio of 1:1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, and treating for 10min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 65%, the content of manganous oxide is 35.47%, and the content of manganese dioxide is 64.53%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 90%.
Example 6
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the activated carbon and the cobalt oxide by a crusher;
(2) mixing active carbon and cobalt oxide according to a mass ratio of 10:1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) and introducing oxygen into the reactor, and treating for 20min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 68%, the content of cobalt oxide is 26.21%, and the content of cobaltous oxide is 73.79%.
(4) The mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 92%.
Example 7
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the activated carbon and the ferrous oxide by a crusher;
(2) mixing activated carbon and ferrous oxide according to a mass ratio of 1:10, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, and treating for 20min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 51%, the content of ferrous oxide is 28.73%, and the content of ferric oxide is 71.27%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 90%.
Example 8
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the activated carbon and the manganese oxide by a crusher;
(2) mixing the activated carbon and the manganese oxide according to the mass ratio of 20:1, mixing, and then putting the mixture into a dielectric barrier discharge reactor;
(3) introducing oxygen into the reactor, and treating for 50min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 71%, the content of manganese sesquioxide is 25.79%, and the content of manganese dioxide is 74.21%;
(4) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 93%.
Comparative example 1
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening the activated carbon by a crusher, and putting the screened activated carbon powder into a dielectric barrier discharge reactor;
(2) introducing oxygen into the reactor, and treating for 10min under the action of low-temperature plasma, wherein the content of oxygen-containing functional groups C ═ O on the carbon-based material is 43%;
(3) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The consumption of the active carbon is 2.0g, and the total flow of the simulated smoke is 4L/min. The mercury removal efficiency of the obtained activated carbon was 64%.
Comparative example 2
The preparation method of the demercuration adsorbent comprises the following steps:
(1) crushing and screening ferrous oxide by a crusher, and putting the screened ferrous oxide powder into a dielectric barrier discharge reactor;
(2) introducing oxygen into the reactor, and treating for 10min under the action of low-temperature plasma, wherein the content of ferrous oxide is 46.33%, and the content of ferric oxide is 53.67%;
(3) the mercury removal performance test is carried out, and the reaction condition is that the initial mercury concentration is 70 mu g/m3The dosage of the adsorbent is 2.0g, and the total flow of the simulated flue gas is 4L/min. The mercury removal efficiency of the resulting sorbent was 62%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for preparing a demercuration adsorbent by low-temperature plasma modification is characterized by comprising the following steps: the method comprises the following steps:
and crushing and screening the carbon-based material and the transition metal oxide, mixing the materials according to a set proportion, introducing oxygen, and performing low-temperature plasma treatment to obtain the mercury removal adsorbent.
2. The method of claim 1, wherein: the carbon-based material is activated carbon or biological coke.
3. The method of claim 1, wherein: the transition metal oxide is ferrous oxide, cerium oxide, cobalt oxide or manganese oxide.
4. The method of claim 1, wherein: the mass ratio of the transition metal oxide to the carbon-based material is 1:20-20: 1.
5. The method of claim 4, wherein: the mass ratio of the transition metal oxide to the carbon-based material is 1:10-10: 1.
6. The method of claim 5, wherein: the mass ratio of the transition metal oxide to the carbon-based material is 1: 1-4.
7. The method of claim 1, wherein: the time of low-temperature plasma treatment is 1-100 min.
8. The method of claim 7, wherein: the time of low-temperature plasma treatment is 1-10 min.
9. A demercuration adsorbent, characterized in that: prepared by the process of any one of claims 1 to 8.
10. Use of the demercuration adsorbent of claim 9 in the demercuration of flue gases.
CN202010896557.3A 2020-08-31 2020-08-31 Method for preparing mercury removal adsorbent by modifying low-temperature plasma and application Pending CN112191226A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114177879A (en) * 2021-12-15 2022-03-15 中国科学院大学 Preparation method of nano-selenium plasma modified ceramic nano-mercury adsorption material

Citations (5)

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Publication number Priority date Publication date Assignee Title
CN1698931A (en) * 2005-04-07 2005-11-23 上海交通大学 Flue gas hydrargyrum-removing method by catalytic oxidation
CN103285805A (en) * 2013-06-18 2013-09-11 广州博能能源科技有限公司 Mercury removal agent and preparation method thereof
CN104148095A (en) * 2014-09-02 2014-11-19 李灏呈 Denitration and demercuration catalyst and preparation method thereof
CN105688832A (en) * 2016-03-08 2016-06-22 东南大学 Low-cost preparation method for modified tobacco char mercury-removing adsorbent
CN108187614A (en) * 2017-12-26 2018-06-22 华中科技大学 A kind of biomass porous carbon sorbent preparation method and product for flue gas demercuration

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1698931A (en) * 2005-04-07 2005-11-23 上海交通大学 Flue gas hydrargyrum-removing method by catalytic oxidation
CN103285805A (en) * 2013-06-18 2013-09-11 广州博能能源科技有限公司 Mercury removal agent and preparation method thereof
CN104148095A (en) * 2014-09-02 2014-11-19 李灏呈 Denitration and demercuration catalyst and preparation method thereof
CN105688832A (en) * 2016-03-08 2016-06-22 东南大学 Low-cost preparation method for modified tobacco char mercury-removing adsorbent
CN108187614A (en) * 2017-12-26 2018-06-22 华中科技大学 A kind of biomass porous carbon sorbent preparation method and product for flue gas demercuration

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114177879A (en) * 2021-12-15 2022-03-15 中国科学院大学 Preparation method of nano-selenium plasma modified ceramic nano-mercury adsorption material
CN114177879B (en) * 2021-12-15 2023-11-21 中国科学院大学 Preparation method of nano selenium plasma modified ceramic nano mercury adsorption material

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