CN113023684A - System and method for preparing sulfur by catalytic reduction of high-sulfur flue gas by using carbon/iron sulfide - Google Patents
System and method for preparing sulfur by catalytic reduction of high-sulfur flue gas by using carbon/iron sulfide Download PDFInfo
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- CN113023684A CN113023684A CN202110254773.2A CN202110254773A CN113023684A CN 113023684 A CN113023684 A CN 113023684A CN 202110254773 A CN202110254773 A CN 202110254773A CN 113023684 A CN113023684 A CN 113023684A
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
- C01B17/0473—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by reaction of sulfur dioxide or sulfur trioxide containing gases with reducing agents other than hydrogen sulfide
- C01B17/0491—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by reaction of sulfur dioxide or sulfur trioxide containing gases with reducing agents other than hydrogen sulfide with hydrogen or hydrogen-containing mixtures, e.g. synthesis gas
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Abstract
The invention discloses a system and a method for preparing sulfur by catalytic reduction of high-sulfur flue gas by using carbon/iron sulfide.A pyrite and a carbon source are mixed and ground according to a set proportion, and the obtained mixed material is added into a pyrolysis furnace for pyrolysis; adding the coal gas obtained by reforming the pyrolysis gas and a pyrolysis solid product catalyst into a reduction tower, and carrying out catalytic reduction on sulfur dioxide in the introduced high-sulfur flue gas; and (3) carrying out gas-solid separation on the flue gas subjected to catalytic reduction, and recovering the generated elemental sulfur. The pyrite and the coal or the biomass are mechanically mixed and ground according to a proportion, and are sent into a pyrolysis furnace for co-pyrolysis, and the obtained carbon/iron sulfide serves as a catalyst. CO generated by the reaction of high-quality coal gas, carbon and oxygen reformed by pyrolysis gas at high temperature and blast furnace gas generated in the smelting process of the inactivated catalyst can be used as reducing agents, and the reducing agents CO in the process are rich in source, do not need to be added with CO, and are relatively suitable for catalytic reduction of sulfur dioxide in high-sulfur flue gas.
Description
Technical Field
The invention belongs to the technical field of high-sulfur flue gas treatment, and particularly relates to a system and a method for preparing sulfur by catalytically reducing high-sulfur flue gas with carbon/iron sulfide.
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.
For a long time, the energy consumption structure of China always takes coal as the main material, and SO generated by coal burning in the electric power industry, the metallurgical industry and the like2Seriously harms the health and ecological environment of residents, SO SO is generated in industrial production2The emission limits of (a) are becoming more stringent. At present, the limestone-gypsum method flue gas desulfurization method is most widely applied, and the product is desulfurized gypsum with lower utilization value. Part of (semi-) dry desulfurization products are strongly corrosive sulfuric acid, and the domestic market supplies the high-concentration SO with basic saturation2The discharge industry, such as sulfur-containing solid waste calcination, non-ferrous metal smelting industry and the like, faces transformation.
The sulfur is a solid substance, has the advantages of small capacity, no secondary pollution, small corrosivity, convenient storage and transportation and the like, and is a relatively ideal desulfurization product. Thus, catalytic reduction of SO2The method for preparing the sulfur is a promising desulfurization mode, can realize resource desulfurization, can relieve the current situation of sulfur resource shortage in China, and has important significance for social sustainable development.
Adding SO2The research on the catalytic reduction to elemental sulfur has mainly focused on the research on high-activity and high-selectivity catalysts. The used catalysts are mostly oxides and sulfides of transition metals and rare earth metals, and the problems of complicated process, high cost, oxidation and inactivation of the catalysts under the oxygen-containing condition and the like generally exist.
Disclosure of Invention
Aiming at the problems, the invention provides a system and a method for preparing sulfur by using carbon/iron sulfide to catalytically reduce high-sulfur flue gas.
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 system for preparing sulfur by using high-sulfur flue gas through catalytic reduction of carbon/iron sulfide, which comprises a mixing and grinding device, a pyrolysis furnace, a reforming furnace and a reduction tower, wherein,
the mixed grinding device is respectively connected with the pyrite and the carbon source and is used for mixing and grinding the pyrite and the carbon source;
the pyrolysis furnace is connected with an outlet of the mixing and grinding device and is used for pyrolyzing the mixed and ground materials;
the inlet of the reforming furnace is connected with the gas outlet of the pyrolysis furnace;
and a solid inlet of the reduction tower is connected with a solid outlet of the pyrolysis furnace, and a gas inlet of the reduction tower is respectively connected with a gas outlet of the reforming furnace and the high-sulfur flue gas source.
In a second aspect, the invention provides a method for preparing sulfur by using carbon/iron sulfide to catalytically reduce high-sulfur flue gas, which comprises the following steps:
mixing and grinding the pyrite and the carbon source according to a set proportion, and adding the obtained mixed material into a pyrolysis furnace for pyrolysis;
adding the coal gas obtained by reforming the pyrolysis gas and a pyrolysis solid product catalyst into a reduction tower, and carrying out catalytic reduction on sulfur dioxide in the introduced high-sulfur flue gas;
and (3) carrying out gas-solid separation on the flue gas subjected to catalytic reduction, and recovering the generated elemental sulfur.
Compared with the prior art, one or more technical schemes of the invention have the following beneficial effects:
the pyrite and the coal or the biomass are mechanically mixed and ground according to a proportion, and are sent into a pyrolysis furnace for co-pyrolysis, and the obtained carbon/iron sulfide serves as a catalyst. CO generated by the reaction of high-quality coal gas, carbon and oxygen reformed by pyrolysis gas at high temperature and blast furnace gas generated in the smelting process of the inactivated catalyst can be used as reducing agents, and the reducing agents CO in the process are rich in source, do not need to be added with CO, and are relatively suitable for catalytic reduction of sulfur dioxide in high-sulfur flue gas.
The carbon/iron sulfide is used as a catalyst, the pyrolysis gas reformed gas is used as a reducing agent, the catalytic reduction is carried out on the sulfur dioxide in the high-sulfur flue gas, and SO is2High conversion rate and low cost.
The catalyst preparation does not need complex loading and prevulcanization processes, only needs mechanical mixing and pyrolysis of the pyrite and the coal/biomass according to a proportion, and has simple and easily obtained raw materials, thereby saving the process time and the cost to a great extent.
Because a small amount of oxygen contained in the flue gas can react with the carbon in the carbon/iron sulfide to generate CO, most of the oxygen is consumed, and the oxidative inactivation of the catalyst under the oxygen-containing condition can be further avoided. By adopting the mode, the resource desulfurization of the flue gas is realized, high-value blast furnace raw materials can be produced, the resource utilization rate is high, the process operation is simple, and the cost is low.
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.
FIG. 1 is a schematic structural diagram of a system for preparing sulfur by reducing high-sulfur/high-sulfur oxygen-containing flue gas by carbon/iron sulfide catalysis CO according to an embodiment of the invention;
FIG. 2 is SO for the catalyst of example 1 of the present invention2A trend graph of conversion rate with reaction temperature;
FIG. 3 is SO for the catalyst of comparative example 1 of the present invention2The conversion rate is plotted against the reaction temperature.
The method comprises the following steps of 1, a pyrolysis furnace, 2, a reforming furnace, 3, a regeneration tower, 4, a kiln, 5, a metal smelting furnace, 6, a reduction tower, 7, a gas-solid separator, 8 and a blast furnace.
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 system for preparing sulfur by using high-sulfur flue gas through catalytic reduction of carbon/iron sulfide, which comprises a mixing and grinding device, a pyrolysis furnace, a reforming furnace and a reduction tower, wherein,
the mixed grinding device is respectively connected with the pyrite and the carbon source and is used for mixing and grinding the pyrite and the carbon source;
the pyrolysis furnace is connected with an outlet of the mixing and grinding device and is used for pyrolyzing the mixed and ground materials;
the inlet of the reforming furnace is connected with the gas outlet of the pyrolysis furnace;
and a solid inlet of the reduction tower is connected with a solid outlet of the pyrolysis furnace, and a gas inlet of the reduction tower is respectively connected with a gas outlet of the reforming furnace and the high-sulfur flue gas source.
In some embodiments, the gas-solid separator is connected with the gas outlet of the reduction tower.
In some embodiments, the system further comprises a blast furnace, and the blast furnace is connected with the solid outlet of the reduction tower.
The catalyst which is ineffective after catalytic reduction in the reduction tower can be used as a high-quality iron-making material to be added into a blast furnace for iron making, and the resource utilization of catalyst waste can be better realized.
Further, a gas outlet of the blast furnace is connected with a gas inlet of the reduction tower.
Blast furnace gas generated in the blast furnace ironmaking process contains high-concentration reducing gas, and can be used as a reducing agent for catalytic reduction of sulfur dioxide in flue gas.
In a second aspect, the invention provides a method for preparing sulfur by using carbon/iron sulfide to catalytically reduce high-sulfur flue gas, which comprises the following steps:
mixing and grinding the pyrite and the carbon source according to a set proportion, and adding the obtained mixed material into a pyrolysis furnace for pyrolysis;
adding the coal gas obtained by reforming the pyrolysis gas and a pyrolysis solid product catalyst into a reduction tower, and carrying out catalytic reduction on sulfur dioxide in the introduced high-sulfur flue gas;
and (3) carrying out gas-solid separation on the flue gas subjected to catalytic reduction, and recovering the generated elemental sulfur.
In some embodiments, the char source is coal or biomass.
Furthermore, the content of the pyrite is 5 to 50 percent.
Furthermore, the grain diameter of the pyrite after being mixed and ground with the carbon source is 60-80 meshes.
In some embodiments, the temperature for mixing and pyrolyzing the pyrite and the carbon source is 500-800 ℃, and the pyrolysis time is 30-60 min.
C and O in the catalyst2Reaction to produce CO, 2C + O2→ 2CO, not only to avoid the oxidative deactivation of the catalyst, but also to provide CO necessary for the reaction, promoting SO2Reduction of (2). High-quality coal gas obtained after pyrolysis gas reforming, CO generated by reaction of carbon and oxygen at high temperature and blast furnace gas generated in the smelting process of the deactivated catalyst can be used as reducing agents, and the reducing agents CO in the process are rich in source and do not need to be added with CO.
Feeding the catalyst to a reduction column, N2Introducing reducing agent CO and high-sulfur/high-sulfur oxygen-containing flue gas preheated by waste heat after the catalyst reaches a preset temperature for shielding gas, and closing shielding gas N2The deactivated catalyst is iron-rich material and may be used as blast furnace iron-smelting material.
The process for producing sulfur by using carbon/iron sulfide to catalytically reduce high-sulfur/high-sulfur oxygen-containing flue gas is mainly characterized by reducing SO by CO2The reaction, following the COS intermediate mechanism: MSx + CO → COS + MSX-1，2COS+SO2→2CO2+3/2S2，S+MSX-1→MSXAccording to the proportion 2:1 ratio of CO to SO2And (4) flow rate.
In some embodiments, the high sulfur flue gas source is a desulfurized coke regeneration flue gas source, a sulfur-containing solid waste calcination flue gas source, or/and a metal smelting flue gas source.
In some embodiments, the method further comprises the step of blast furnace ironmaking using the deactivated catalyst in the reduction tower as a raw material.
Further, the method also comprises the step of introducing coal gas generated by blast furnace ironmaking into a reduction tower as a reduction gas to reduce sulfur dioxide in the flue gas.
Example 1
As shown in fig. 1, a system for preparing sulfur by catalytic reduction of high-sulfur flue gas by using carbon/iron sulfide comprises a mixing and grinding device, a pyrolysis furnace 1, a reforming furnace 2 and a reduction tower 6, wherein,
the mixed grinding device is respectively connected with the pyrite and the carbon source and is used for mixing and grinding the pyrite and the carbon source;
the pyrolysis furnace 1 is connected with an outlet of the mixing and grinding device and is used for pyrolyzing the mixed and ground materials;
the inlet of the reforming furnace 2 is connected with the gas outlet of the pyrolysis furnace 1;
and a solid inlet of the reduction tower 6 is connected with a solid outlet of the pyrolysis furnace 1, and a gas inlet of the reduction tower 6 is respectively connected with a gas outlet of the reforming furnace 2 and a high-sulfur flue gas source.
The gas-solid separator 7 is connected with a gas outlet of the reduction tower 6, the blast furnace 8 is connected with a solid outlet of the reduction tower 6, and a gas outlet of the blast furnace 8 is connected with a gas inlet of the reduction tower 6.
Firstly, mixing and grinding pyrite and coal mechanically according to the proportion of 5:1 into 60-80 meshes of CO2/N2Heating to 600 deg.C in atmosphere, and pyrolyzing for 40min to obtain carbon/iron sulfide catalyst with specific surface area of 280m2/g。
Then 5g of catalyst were charged into a reduction column, N2For shielding gas, after the temperature of the catalyst reaches 500 ℃, introducing reducing agent CO and high-sulfur flue gas preheated by waste heat (space velocity of 6000 h)-1Flow 300ml/min, SO215000ppm CO 30000ppm) while turning off the shielding gas N2And carrying out catalytic reduction on sulfur dioxide in the flue gas.
SO of catalyst2The conversion rate increased with the increase of the reaction temperature, and SO was measured at 500 deg.C, 600 deg.C, 700 deg.C and 800 deg.C as shown in FIG. 22The conversions were 21%, 56%, 95% and 99.8%, respectively.
The flue gas after catalytic reduction flows out of the reduction tower, and sulfur is recovered after gas-solid separation by a gas-solid separator. The deactivated catalyst in the reduction tower is an iron-rich material and can be used as a blast furnace iron-making raw material, and blast furnace gas generated in the process is returned to the reduction tower to be used as a reducing agent.
Comparative example 1
The difference from example 1 is that: replacement of pyrite in example 1 with FeS2The mass ratio of coal to pyrite was 5.2:1, and the rest was the same as in example 1.
The specific surface area of the catalyst was 255m2/g。
Then 5g of catalyst were charged into a reduction column, N2For shielding gas, after the temperature of the catalyst reaches 500 ℃, introducing reducing agent CO and high-sulfur flue gas preheated by waste heat (space velocity of 6000 h)-1Flow 300ml/min, SO215000ppm CO 30000ppm) while turning off the shielding gas N2And carrying out catalytic reduction on sulfur dioxide in the flue gas.
As shown in FIG. 3, SO was obtained at 500 deg.C, 600 deg.C, 700 deg.C and 800 deg.C2The conversions were 19%, 45%, 81% and 94%, respectively.
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 system for preparing sulfur by using carbon/iron sulfide to catalytically reduce high-sulfur flue gas is characterized in that: comprises a mixing and grinding device, a pyrolysis furnace, a reforming furnace and a reduction tower, wherein,
the mixed grinding device is respectively connected with the pyrite and the carbon source and is used for mixing and grinding the pyrite and the carbon source;
the pyrolysis furnace is connected with an outlet of the mixing and grinding device and is used for pyrolyzing the mixed and ground materials;
the inlet of the reforming furnace is connected with the gas outlet of the pyrolysis furnace;
and a solid inlet of the reduction tower is connected with a solid outlet of the pyrolysis furnace, and a gas inlet of the reduction tower is respectively connected with a gas outlet of the reforming furnace and the high-sulfur flue gas source.
2. The system for preparing sulfur by catalytic reduction of high sulfur flue gas by carbon/iron sulfide as claimed in claim 1, wherein: the gas-solid separator is connected with a gas outlet of the reduction tower.
3. The system for preparing sulfur by catalytic reduction of high sulfur flue gas by carbon/iron sulfide as claimed in claim 1, wherein: the blast furnace is connected with a solid outlet of the reduction tower;
further, a gas outlet of the blast furnace is connected with a gas inlet of the reduction tower.
4. A method for preparing sulfur by using carbon/iron sulfide to catalytically reduce high-sulfur flue gas is characterized by comprising the following steps: the method comprises the following steps:
mixing and grinding the pyrite and the carbon source according to a set proportion, and adding the obtained mixed material into a pyrolysis furnace for pyrolysis;
adding the coal gas obtained by reforming the pyrolysis gas and a pyrolysis solid product catalyst into a reduction tower, and carrying out catalytic reduction on sulfur dioxide in the introduced high-sulfur flue gas;
and (3) carrying out gas-solid separation on the flue gas subjected to catalytic reduction, and recovering the generated elemental sulfur.
5. The method for preparing sulfur by the catalytic reduction of high-sulfur flue gas by carbon/iron sulfide as claimed in claim 4, wherein: the carbon source is coal or biomass.
6. The method for preparing sulfur by the catalytic reduction of high-sulfur flue gas by carbon/iron sulfide as claimed in claim 4, wherein: 5 to 50 percent of pyrite;
furthermore, the grain diameter of the mixed and ground pyrite and the carbon source is 60-100 meshes.
7. The method for preparing sulfur by the catalytic reduction of high-sulfur flue gas by carbon/iron sulfide as claimed in claim 4, wherein: the temperature for mixing and pyrolyzing the pyrite and the carbon source is 500-800 ℃, and the pyrolysis time is 30-60 min.
8. The method for preparing sulfur by the catalytic reduction of high-sulfur flue gas by carbon/iron sulfide as claimed in claim 4, wherein: the high-sulfur flue gas source is a desulfurized coke regenerated flue gas source, a sulfur-containing solid waste calcined flue gas source or/and a metal smelting flue gas source.
9. The method for preparing sulfur by the catalytic reduction of high-sulfur flue gas by carbon/iron sulfide as claimed in claim 4, wherein: the method also comprises a step of blast furnace iron making by taking the deactivated catalyst in the reduction tower as a raw material.
10. The method for preparing sulfur by the catalytic reduction of high sulfur flue gas by carbon/iron sulfide as claimed in claim 9, wherein: and the method also comprises the step of introducing coal gas generated by blast furnace ironmaking into a reduction tower as a reduction gas to reduce sulfur dioxide in the flue gas.
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| GB428979A (en) * | 1934-06-12 | 1935-05-22 | Axel Rudolf Lindblad | Improvements in the production of sulphur |
| US20010000475A1 (en) * | 1998-01-14 | 2001-04-26 | Yun Jin | Sulfide catalysts for reducing SO2 to elemental sulfur |
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