CN113753894A - Preparation method of ferroferric oxide loaded active carbon - Google Patents

Preparation method of ferroferric oxide loaded active carbon Download PDF

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Publication number
CN113753894A
CN113753894A CN202111157287.5A CN202111157287A CN113753894A CN 113753894 A CN113753894 A CN 113753894A CN 202111157287 A CN202111157287 A CN 202111157287A CN 113753894 A CN113753894 A CN 113753894A
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carbonization
clean coal
furnace
activation
briquetting
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薛银花
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Shanxi Huaqing Environmental Protection Co Ltd
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Shanxi Huaqing Environmental Protection Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/336—Preparation characterised by gaseous activating agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide [Fe3O4]
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/21—Attrition-index or crushing strength of granulates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above

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  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to the technical field of composite carbon materials, in particular to a preparation method of ferroferric oxide loaded activated carbon. The preparation method provided by the invention comprises the following steps: sequentially carrying out flotation and washing on Xinjiang clean coal to obtain washed clean coal; and mixing the washed clean coal and the iron powder, and then sequentially carrying out briquetting, carbonization and activation to obtain the ferroferric oxide loaded activated carbon. The ferroferric oxide loaded active carbon prepared by the preparation method can be recycled.

Description

Preparation method of ferroferric oxide loaded active carbon
Technical Field
The invention relates to the technical field of composite carbon materials, in particular to a preparation method of ferroferric oxide loaded activated carbon.
Background
Fluorine is a trace element, water with fluorine content of 0.4-0.6 mg/L in drinking water is harmless to human bodies, and high-fluorine water with fluorine content of more than 1.5mg/L is harmful to human bodies after long-term drinking, so that dental fluorosis and fluorosis can be caused seriously. For areas with high fluorine content, the discharge of a large amount of industrial wastewater with high fluorine content is one of the main factors except for natural factors in individual areas.
At present, the main treatment methods of fluorine-containing wastewater are a chemical precipitation method and an adsorption method, and for the adsorption method, the adsorption method adopting activated carbon is a method which is widely applied at present. However, in most of the existing water plants, in order to save cost when activated carbon is used for adsorbing fluorine-containing compounds, part of quartz sand or substances similar to quartz sand is added at the bottom, so that the adsorption is difficult to recycle.
Disclosure of Invention
The invention aims to provide a preparation method of ferroferric oxide loaded activated carbon, and the ferroferric oxide loaded activated carbon prepared by the preparation method can be recycled.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of ferroferric oxide loaded active carbon, which comprises the following steps:
sequentially carrying out flotation and washing on Xinjiang clean coal to obtain washed clean coal;
and mixing the washed clean coal and the iron powder, and then sequentially carrying out briquetting, carbonization and activation to obtain the ferroferric oxide loaded activated carbon.
Preferably, the caking index of the Xinjiang clean coal is 10-15, the ash content is 1.0-2.0 wt%, and the volatile component is less than 38 wt%.
Preferably, the heavy liquid adopted by the flotation is a zinc chloride aqueous solution;
the mass ratio of zinc chloride to water in the zinc chloride aqueous solution is 1: 1.5.
Preferably, the caking index of the washed clean coal is 5-18, the ash content is 0.5-2.5 wt%, the volatile matter content is 30-40 wt%, and the water content is 5-9 wt%.
Preferably, the mass ratio of the water-washed clean coal to the iron powder is 124: 1.
Preferably, the pressure of the briquetting is 22-30 MPa, and the motor power of a briquetting machine adopted by the briquetting is 15-50 Hz.
Preferably, the carbonization comprises a first carbonization step, a second carbonization step and a third carbonization step which are sequentially carried out;
the temperature of the first carbonization is 200-300 ℃, the temperature of the second carbonization is 400-450 ℃, and the temperature of the third carbonization is 500-550 ℃.
Preferably, the first carbonization, the second carbonization and the third carbonization respectively and correspondingly pass the briquetting materials obtained by briquetting through the process of a furnace head, a furnace and a furnace tail of a carbonization furnace;
the transmission speed of the pressing material through the furnace head, the furnace and the furnace tail is independently 0.3-0.6 m/min;
the rotation speed of the carbonization furnace is 1-3 r/min.
Preferably, the activation comprises a preliminary activation and a deep activation which are sequentially carried out;
the preliminary activation is carried out in a water vapor atmosphere; the pressure of the preliminary activation is 101.385-101.435 kPa, the temperature is 850-980 ℃, and the time is 2-4 h.
Preferably, the deep activation is carried out in a mixed atmosphere of water vapor and flue gas; the flue gas comprises 2 vol% SO2，15vol％N2，2vol％O213 vol% CO, 28 vol% CO2And a hydrocarbon and 40 vol% nitrogen oxide;
the volume ratio of the water vapor to the flue gas is 1: (2-9);
the deep activation temperature is 800-1100 ℃, the time is 55-70 h, and the steam pressure is 1.0-3.0 MPa.
The invention provides a preparation method of ferroferric oxide loaded active carbon, which comprises the following steps: sequentially carrying out flotation and washing on Xinjiang clean coal to obtain washed clean coal; and mixing the washed clean coal and the iron powder, and then sequentially carrying out briquetting, carbonization and activation to obtain the ferroferric oxide loaded activated carbon. According to the invention, Xinjiang clean coal is used as a raw material to prepare the activated carbon, the characteristics that the Xinjiang clean coal is small in ash content and high in purity, and the Xinjiang clean coal is low in trace elements (antimony, arsenic and the like) compared with the large and same clean coal and Shaanxi clean coal are utilized to prepare the activated carbon with better performance, and through the sequential flotation, washing, briquetting, carbonization and activation, the prepared activated carbon has a well-developed mesopore structure, and the fluorine-containing compounds in water can be effectively removed. Meanwhile, the added iron powder can be oxidized into ferroferric oxide through activation, so that the magnetism of a final product is improved, the separation of the activated carbon is facilitated, and the reuse of the activated carbon is realized. According to the description of the embodiment, the ferroferric oxide loaded activated carbon prepared by the preparation method can be reused for more than or equal to 5 times. According to the description of the embodiment, the ratio of the ferroferric oxide supported activated carbon prepared by the preparation method of the inventionThe surface area is more than or equal to 1000m2The iodine adsorption value is more than or equal to 1000mg/g, the ash content is less than or equal to 10%, the strength is more than or equal to 90%, the bulk density is 450-550 g/L, the content of ferroferric oxide is more than or equal to 2-3%, and the particle size is 8-30 meshes.
Detailed Description
The invention provides a preparation method of ferroferric oxide loaded active carbon, which comprises the following steps:
sequentially carrying out flotation and washing on Xinjiang clean coal to obtain washed clean coal;
and mixing the washed clean coal and the iron powder, and then sequentially carrying out briquetting, carbonization and activation to obtain the ferroferric oxide loaded activated carbon.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
According to the invention, Xinjiang clean coal is subjected to flotation and washing in sequence to obtain washed clean coal.
In the invention, the caking index of the Xinjiang clean coal is preferably 10-15, the ash content is preferably 1.0-2.0 wt%, and the volatile component is preferably <38 wt%.
Before flotation, the Xinjiang clean coal is preferably subjected to stone removal treatment. The process of the stone removing treatment is not limited in any way, and the process known by the technical personnel in the field is adopted to ensure that the bulk density of the coal subjected to the stone removing treatment is preferably within the range of 650-850 g/L, and the bulk density of the coal subjected to the stone removing treatment is more preferably 700-750 g/L. In a specific embodiment of the present invention, the stoning process specifically employs a TQSF gravity classification stoner.
In the invention, the heavy liquid used for flotation is preferably zinc chloride aqueous solution; the mass ratio of zinc chloride to water in the zinc chloride aqueous solution is preferably 1: 1.5. The flotation process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art.
In the invention, the time for washing is preferably 0.5-2 h, and more preferably 1-2 h. The method for washing by water is not limited in any way, and the residual zinc chloride aqueous solution in the clean coal obtained by flotation can be completely removed by adopting a method well known to those skilled in the art.
After the water washing is completed, the invention also preferably comprises drying; in the invention, the drying pressure is preferably 96-100 kPa, more preferably 97-98 kPa; the drying temperature is preferably 200-450 ℃, and more preferably 300-400 ℃. The drying time is not limited in any way, and the product obtained after drying can be ensured to be in the water content range of 5-9 wt%. In the invention, the drying is preferably carried out by using steam of a waste heat boiler and a biomass boiler, and the pressure of the drying is preferably the steam pressure in the boiler. In a particular embodiment of the invention, the drying is carried out in a converter, which is a stainless steel converter with a diameter of 1.2m and a length of 15 m; pressure of the drying
In the invention, the caking index of the washed clean coal is preferably 5-18, and more preferably 10-15; the ash content is preferably 0.5-2.5 wt%, and more preferably 1.0-2.0 wt%; the volatile component is preferably 30-40 wt%, and more preferably 32-38 wt%; the water content is preferably 5 to 9 wt%, more preferably 5 to 7 wt%.
After the washed clean coal is obtained, the washed clean coal and the iron powder are mixed, and then are subjected to briquetting, carbonization and activation in sequence to obtain the ferroferric oxide loaded active carbon.
Before the water-washed clean coal and the iron powder are mixed, the water-washed clean coal is preferably milled into powder; the process of the invention for milling is not limited in any way, and the process known to those skilled in the art is adopted to ensure that the particle size of the milled washed clean coal is less than or equal to 45 mu m. In a particular embodiment of the invention, the milling is preferably carried out in a GRM vertical mill.
In the present invention, the particle size of the iron powder is preferably <1mm, and more preferably 44 to 150 um.
In the present invention, the purity of the iron powder is preferably not less than 90 wt%, more preferably not less than 95 wt%.
In the present invention, the mass ratio of the water-washed clean coal to the iron powder is preferably 124: 1.
The mixing process is not particularly limited in the present invention, and the mixing process may be well known to those skilled in the art.
In the invention, the pressure of the briquetting is preferably 22-30 MPa, and more preferably 25-28 MPa; the rotating speed power of the briquetting is preferably 15-50 Hz, and more preferably 18-20 Hz. In a particular embodiment of the invention, the briquetting is carried out in a dry roll briquetting machine.
In the present invention, the briquetting strength of the briquette obtained by the briquetting is preferably not less than 92%. The shape of the block is not particularly limited in the present invention. In a specific embodiment of the present invention, the crush blocks are ellipsoidal; the major axis radius of the ellipsoidal pressure block is 5-9 mm, and the minor axis radius is 2-6 mm.
In the present invention, the carbonization preferably comprises a first carbonization step, a second carbonization step and a third carbonization step which are sequentially performed; preferably, the first carbonization, the second carbonization and the third carbonization respectively correspond to the process of sequentially passing the briquetting material obtained by the briquetting through the furnace head, the furnace and the furnace tail of the carbonization furnace. In the invention, the temperature of the furnace end (namely the temperature of the first carbonization) is preferably 200-300 ℃, and more preferably 220-280 ℃; the temperature in the furnace (i.e. the temperature of the second carbonization step) is preferably 400-450 ℃, and more preferably 420-430 ℃; the temperature of the furnace tail (namely the temperature of the third carbonization step) is preferably 500-550 ℃, and more preferably 510-530 ℃. In the invention, the conveying speed of the briquetting material through the furnace head, the furnace and the furnace tail is preferably 0.3-0.6 m/min, and more preferably 0.4-0.5 m/min. In the invention, the rotation speed of the carbonization furnace is preferably 1-3 r/min. In the invention, the carbonization time is preferably 30-60 min, and more preferably 40-50 min; the carbonization time is preferably the time from the furnace head to the furnace tail of the carbonized material. In the invention, the flue gas generated during carbonization is preferably sent into an incinerator for high-temperature incineration through an air blower, the high-temperature flue gas after incineration is adjusted to a proper temperature through a heat exchanger and then enters the carbonization furnace to carbonize the briquette, and the carbonization pressure is preferably 96-100 kPa, and more preferably 97-98 kPa.
In the present invention, the carbonization furnace is preferably an external heat chamber carbonization furnace; the furnace end of the carbonization furnace is generally heated by hot gas generated after high-temperature incineration of carbonization tail gas, volatile substances in the pressing block materials can be decomposed into coal gas, tar and the like through carbonization, a preliminary pore-forming effect is achieved, and a channel is provided for subsequent activation and reaming.
In the invention, the carbonization is carried out step by step, so that the quality of the carbonized material is more stable.
In the invention, the volatile content of the carbonized material obtained after carbonization is preferably 15-35 wt%, and more preferably 15-20 wt%.
In the present invention, the activation preferably includes preliminary activation and deep activation which are performed in this order; the preliminary activation is preferably carried out in a water vapor atmosphere; the pressure of the primary activation is preferably 101.385-101.435 kPa; the temperature is preferably 850-980 ℃, more preferably 880-950 ℃, and most preferably 900-920 ℃; the time is preferably 2 to 4 hours, and more preferably 3.0 to 3.5 hours. In the invention, the preliminary activation is carried out in a water vapor atmosphere to ensure the stable quality of the activated material; the preliminary activation control within the above condition range has the effect of adjusting the pores of the activated carbon, improving the quality thereof and stabilizing the performance thereof.
In the present invention, the deep activation is preferably performed in a mixed atmosphere of water vapor and flue gas; the flue gas preferably comprises 2 vol% SO2，15vol％N2，2vol％O2，13vol％CO，28vol％CO2And a hydrocarbon and 40 vol% nitrogen oxide; the volume ratio of the water vapor to the flue gas is preferably 1: (2-9), more preferably 1: (3-4). In the invention, the deep activation temperature is preferably 800-1100 ℃, and more preferably 880-1000 ℃; the time is preferably 50-70 h, and more preferably 60-70 h; the steam pressure is preferably 1.0 to 3.0MPa, and more preferably 2.0 to 2.5 MPa. In the invention, the deep activation is carried out in the mixed atmosphere of water vapor and smoke so as to ensure the stable quality of the activated material; the deep activation controlled in the above condition range has the effects of adjusting the pores of the activated carbon, improving the quality of the activated carbon and ensuring that the activated carbon has the same pore size and high porosityThe performance is more stable.
After the activation is finished, the invention also preferably comprises the steps of sequentially crushing and cleaning the activated material obtained by the activation; the crushing process is not limited in any way, and the process known by the technical personnel in the field is adopted to ensure that the crushed materials with the particle size of 8-30 meshes can be obtained. In the present invention, the cleaning preferably includes dust reduction and dust removal performed in this order; the process of ash and dust removal is not limited in any way, and can be carried out by adopting a process well known to those skilled in the art.
The following examples are provided to describe the preparation method of the ferroferric oxide-supported activated carbon provided by the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Removing stones from the Xinjiang clean coal (the parameters are 10 caking index, 1.0 wt% ash and 36.5 wt% volatile matter) by a TQSF gravity grading stone remover to obtain the Xinjiang clean coal with bulk density of 730 g/L;
after 80kg of Xinjiang clean coal with bulk density of 730g/L is subjected to flotation by using 31.2kg of zinc chloride solution (the weight ratio of zinc chloride to water is 1:1.5), washing with water for 0.8h to remove the zinc chloride solution, and drying in a stainless steel converter with the diameter of 1.2m and the length of 15m in a drying atmosphere of drying by using steam of a waste heat boiler and a biomass boiler at the pressure of 97kPa until the washed clean coal with water (the bonding index is 10, the ash content is 1.2 wt%, the volatile content is 34.8 wt%, and the water content is 6 wt%);
placing the water-washed clean coal into a GRM vertical mill for milling until the milled particle size is less than or equal to 45 mu m, uniformly mixing 8kg of the milled water-washed clean coal with 0.0645kg of iron powder with the particle size of 42 mu m (the purity is more than or equal to 95 wt%) in the conveying process, feeding the mixture into a dry-method roller-type briquetting machine for briquetting, wherein the pressure of the briquetting is 25MPa, the rotating speed and the power of the briquetting are 18Hz, and obtaining a briquetting material (an ellipsoidal briquetting material, the major axis radius is 5mm, the minor axis radius is 2mm, and the briquetting strength is 92%);
conveying the pressing block material to an external heating chamber carbonization furnace, wherein the temperature of a furnace head of the external heating chamber carbonization furnace is 260 ℃, the temperature in the furnace is 430 ℃, and the temperature of a furnace tail is 520 ℃; the carbonization time is 38min, the conveying speed of the pressing block is 0.4m/min, the rotation speed of the carbonization furnace is 2r/min, the carbonization atmosphere is hot gas obtained by burning carbonized tail gas at high temperature, the pressure is 97kPa, and a carbonized material (the volatile content is 32 wt%) is obtained;
firstly, preliminarily activating the carbonized material in a water vapor atmosphere with the pressure of 101.389kPa, wherein the preliminary activation temperature is 930 ℃ and the time is 3 h; then, the steam and the flue gas (containing 2 vol% of SO) are carried out at the pressure of 2.2MPa and the volume ratio of 1:3.52，15vol％N22 vol% of O213 vol% CO, 28 vol% CO2And hydrocarbon and 40 vol% of oxynitride), the deep activation is carried out at 950 ℃ for 52 hours, and after the activated material with 8-30 meshes is obtained by crushing, ash reduction and dust removal are carried out in sequence, so as to obtain the ferroferric oxide loaded activated carbon.
Example 2
Removing stones from the Xinjiang clean coal (the parameters are 12 caking index, 1.3 wt% ash and 36.8 wt% volatile matter) by a TQSF gravity grading stone remover to obtain the Xinjiang clean coal with the bulk density of 740 g/L;
after 10kg of Xinjiang clean coal with the bulk density of 740g/L is subjected to flotation by using 3.9kg of zinc chloride solution (the weight ratio of zinc chloride to water is 1:1.5), washing with water for 0.8h to remove the zinc chloride solution, and drying in a stainless steel converter with the diameter of 1.2m and the length of 15m in the drying atmosphere of drying by using steam of a waste heat boiler and a biomass boiler at the pressure of 98kPa until washed clean coal with water (the bonding index is 10, the ash content is 1.42 wt%, the volatile content is 35.8 wt%, and the water content is 6.3 wt%);
placing the washed clean coal in a GRM vertical mill for milling until the milled particle size is less than or equal to 45 microns, uniformly mixing 10kg of the milled clean coal with 0.0806kg of iron powder (the purity is more than or equal to 95%) with the particle size of 42 microns in the conveying process, feeding the mixture into a dry-method roller type briquetting machine for briquetting, wherein the pressure of the briquetting is 25Mpa, the rotating speed power of the briquetting is 19Hz, and obtaining a briquetting material (an ellipsoidal briquetting material, the major axis radius is 5mm, the minor axis radius is 2mm, and the briquetting strength is 92.7%);
conveying the pressing block material to an external heating chamber carbonization furnace, wherein the temperature of a furnace head of the external heating chamber carbonization furnace is 268 ℃, the temperature of the furnace is 425 ℃, and the temperature of a furnace tail is 525 ℃; the carbonization time is 40min, the conveying speed of the pressing block is 0.4m/min, the rotation speed of the carbonization furnace is 2r/min, the carbonization atmosphere is hot gas obtained by burning the carbonized tail gas at high temperature, and the pressure is 98.2kPa, so that a carbonized material (the volatile content is 31.8 wt%) is obtained;
firstly, preliminarily activating the carbonized material in a water vapor atmosphere with the pressure of 101.402kPa, wherein the preliminary activation temperature is 948 ℃, and the time is 3.5 h; then, the steam and the flue gas (containing 2 vol% of SO) are carried out at the pressure of 2.3MPa and the volume ratio of 1:3.32，15vol％N22 vol% of O213 vol% CO, 28 vol% CO2And hydrocarbon and 40 vol% of oxynitride), the deep activation is carried out at 980 ℃ for 63h, the activated material is crushed to obtain 8-30 meshes of activated material, and then ash reduction and dust removal are carried out in sequence to obtain the ferroferric oxide loaded activated carbon.
Example 3
Removing stones from the Xinjiang clean coal (the parameters are index 13, ash content is 1.5 wt% and volatile matter is 37.3 wt%) by a TQSF gravity grading stone remover to obtain the Xinjiang clean coal with bulk density of 750 g/L;
after 15kg of Xinjiang clean coal with the bulk density of 750g/L is subjected to flotation by using 5.85kg of zinc chloride solution (the weight ratio of zinc chloride to water is 1:1.5), washing with water for 0.8h to remove the zinc chloride solution, and drying in a stainless steel converter with the diameter of 1.2m and the length of 15m in the drying atmosphere of drying by using steam of a waste heat boiler and a biomass boiler under the pressure of 98kPa until the washed clean coal with water (the bonding index is 10, the ash content is 1.58 wt%, the volatile matter is 36.2 wt%, and the water content is 7.3%);
placing the washed clean coal in a GRM vertical mill, grinding until the grain size of the ground clean coal is less than or equal to 45 mu m, uniformly mixing 15kg of the ground washed clean coal with 0.120kg of iron powder (the purity is more than or equal to 95%) with the grain size of 42 mu m in the conveying process, feeding the mixture into a dry-method roll-type briquetting machine, and briquetting, wherein the pressure of the briquetting is 27MPa, the rotating speed power of the briquetting is 20Hz, so that a briquetting material (an ellipsoidal briquetting material, the radius of a long shaft is 5mm, the radius of a short shaft is 2mm, and the strength of the briquetting is 94%) is obtained;
conveying the pressing block material to an external heating chamber carbonization furnace, wherein the temperature of a furnace head of the external heating chamber carbonization furnace is 275 ℃, the temperature in the furnace is 430 ℃, and the temperature of a furnace tail is 530 ℃; the carbonization time is 40min, the conveying speed of the pressing block is 0.4m/min, the rotation speed of the carbonization furnace is 2r/min, the carbonization atmosphere is hot gas obtained by burning the carbonized tail gas at high temperature, the pressure is 98.8kPa, and the carbonized material (the volatile content is 30.5 wt%) is obtained;
firstly, preliminarily activating the carbonized material in a water vapor atmosphere with the pressure of 101.435kPa, wherein the preliminary activation temperature is 980 ℃ and the time is 3.5 h; then steam and flue gas (containing 2 vol% of SO) at the pressure of 2.4MPa and the volume ratio of 1:3.52，15vol％N2，2vol％O2，13vol％CO，28vol％CO2And hydrocarbon and 40 vol% oxynitride), the deep activation is carried out at 990 ℃ for 65 hours, the activated material with 8-30 meshes is obtained by crushing, and then ash reduction and dust removal are carried out in sequence to obtain the ferroferric oxide loaded activated carbon.
Test example 1
According to the GB/T7702.20-2008 standard, the specific surface area (m) of the ferroferric oxide loaded activated carbon in the embodiment 1-3 is tested2/g)；
According to the GB/T7702.7-2008 standard, testing the iodine adsorption value (mg/g) of the ferroferric oxide loaded activated carbon in the embodiment 1-3;
testing ash content (wt%) of the ferroferric oxide loaded activated carbon according to GB/T7702.15-2008;
testing the strength (%) of the ferroferric oxide loaded activated carbon in the embodiment 1-3 according to the GB/T7702.3-2008 standard;
testing the bulk density (g/L) of the ferroferric oxide loaded activated carbon in examples 1-3 according to the GB/T7702.4-2008 standard;
testing the particle size of the ferroferric oxide loaded activated carbon in the embodiment 1-3 according to the GB/T7702.2-2008 standard;
testing the iron content (wt%) of the ferroferric oxide loaded activated carbon in the embodiment 1-3 according to the standard GB/T12496.19-2015;
the test results are shown in table 1:
TABLE 1 Performance parameters of the ferroferric oxide loaded activated carbon described in examples 1-3 of the present application
Examples Example 1 Example 2 Example 3
Specific surface area (m)2/g) 1050 1045 1047
Iodine adsorption number (mg/g) 1045 1037 1041
Ash content (wt%) 9.76 8.95 9.12
Strength (%) 95 94 95
Bulk Density (g/L) 489 495 497
Iron content (wt%) 2.4 2.3 2.2
Test example 2
The magnetic particle-loaded carbon material and the commercial 8X 30-mesh common activated carbon are regenerated after being used, and the obtained data indexes are shown in the table 2:
TABLE 2 data index of regenerated carbon material loaded with magnetic particles and commercial 8X30 mesh-like common activated carbon after use
Figure BDA0003289107910000101
Remarking: in the regeneration condition after use, the regeneration is carried out at 500-600 ℃ for 90 minutes.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of ferroferric oxide loaded activated carbon is characterized by comprising the following steps:
sequentially carrying out flotation and washing on Xinjiang clean coal to obtain washed clean coal;
and mixing the washed clean coal and the iron powder, and then sequentially carrying out briquetting, carbonization and activation to obtain the ferroferric oxide loaded activated carbon.
2. The preparation method according to claim 1, wherein the Xinjiang clean coal has a caking index of 10-15, an ash content of 1.0-2.0 wt%, and a volatile content of <38 wt%.
3. The method according to claim 1, wherein the heavy liquid used for the flotation is an aqueous solution of zinc chloride;
the mass ratio of zinc chloride to water in the zinc chloride aqueous solution is 1: 1.5.
4. The method according to claim 1, wherein the washed clean coal has a caking index of 5 to 18, an ash content of 0.5 to 2.5 wt%, a volatile matter content of 30 to 40 wt%, and a water content of 5 to 9 wt%.
5. The preparation method according to claim 1, wherein the mass ratio of the water-washed clean coal to the iron powder is 124: 1.
6. The preparation method of claim 1, wherein the pressure of the briquetting is 22-30 MPa, and the motor power of a briquetting machine used for the briquetting is 15-50 Hz.
7. The production method according to claim 1, wherein the carbonization comprises a first carbonization, a second carbonization, and a third carbonization, which are performed in this order;
the temperature of the first carbonization is 200-300 ℃, the temperature of the second carbonization is 400-450 ℃, and the temperature of the third carbonization is 500-550 ℃.
8. The preparation method according to claim 7, wherein the first carbonization, the second carbonization and the third carbonization respectively correspond to a process of sequentially passing a briquette material obtained by briquetting through a furnace head, a furnace and a furnace tail of a carbonization furnace;
the transmission speed of the pressing material through the furnace head, the furnace and the furnace tail is independently 0.3-0.6 m/min;
the rotation speed of the carbonization furnace is 1-3 r/min.
9. The production method according to claim 1, wherein the activation includes preliminary activation and deep activation which are performed in this order;
the preliminary activation is carried out in a water vapor atmosphere; the pressure of the preliminary activation is 101.385-101.435 kPa, the temperature is 850-980 ℃, and the time is 2-4 h.
10. The method of claim 9, wherein the deep activation is performed in a mixed atmosphere of water vapor and flue gas; the flue gas comprises 2 vol% SO2，15vol％N2，2vol％O2，13vol％CO，28vol％CO2And a hydrocarbon and 40 vol% nitrogen oxide;
the volume ratio of the water vapor to the flue gas is 1: (2-9);
the deep activation temperature is 800-1100 ℃, the time is 55-70 h, and the steam pressure is 1.0-3.0 MPa.
CN202111157287.5A 2021-09-30 2021-09-30 Preparation method of ferroferric oxide loaded active carbon Pending CN113753894A (en)

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Application publication date: 20211207