CN113801498A - Clean roasting modification method for vanadium-containing shale - Google Patents

Clean roasting modification method for vanadium-containing shale Download PDF

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Publication number
CN113801498A
CN113801498A CN202111193701.8A CN202111193701A CN113801498A CN 113801498 A CN113801498 A CN 113801498A CN 202111193701 A CN202111193701 A CN 202111193701A CN 113801498 A CN113801498 A CN 113801498A
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China
Prior art keywords
roasting
crushing
vanadium
ball milling
drying
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CN202111193701.8A
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Inventor
范川林
朱庆山
潘锋
葛宇
马素刚
刘家义
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043—Drying, calcination
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D13/00—Apparatus for preheating charges; Arrangements for preheating charges
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases
    • F27D17/004—Systems for reclaiming waste heat
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases
    • F27D17/008—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases cleaning gases

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention discloses a method for modifying vanadium-containing shale by clean roasting. The method mainly comprises the working procedures of raw material crushing, ball milling, drying, preheating and roasting, and specifically comprises the following steps: the method comprises the steps of crushing vanadium-containing shale raw ore, adding limestone or dolomite, performing ball milling treatment, drying, entering a cyclone preheater, performing heat exchange with roasting smoke to preheat, entering the preheated raw material into a roasting process, performing roasting modification to obtain modified shale, wherein sulfur oxides and nitrogen oxides of the roasting smoke meet emission standards, and therefore the smoke can be directly discharged after dust removal. The method is simple to operate, can realize roasting modification of the vanadium-containing shale and simultaneously carry out desulfurization and denitrification treatment, and saves subsequent special desulfurization and denitrification processes.

Description

Clean roasting modification method for vanadium-containing shale
Technical Field
The invention relates to the fields of chemical industry and materials, in particular to a method for modifying vanadium-containing shale by clean roasting.
Background
Vanadium is an important rare metal element, is widely applied to a plurality of important fields of national economy such as steel, non-ferrous, chemical industry, energy storage, optics, electronics, environmental protection, medicine, atomic energy and the like, and is called as monosodium glutamate in modern industry. The vanadium resource in China is rich and mainly exists in vanadium titano-magnetite and stone coal. The distribution of the vanadium-containing shale in China is very wide, the total reserve is 618.8 hundred million tons, wherein the industrial reserve is found to be 39 hundred million tons, the reserve with the content of more than 0.5 percent is 7707.5 million tons, and the vanadium-containing shale is V in vanadium titano-magnetite in China2O5The storage capacity is 2.7 times, and the storage capacity of vanadium pentoxide in stone coal of 7 provinces such as Xiang, Hui province, Gangxi province and the like can reach 11797 ten thousand tons. Therefore, China pays great attention to the extraction and development of vanadium resources in the vanadium-containing shale, and develops various technologies for extracting vanadium from stone coal.
Research on vanadium extraction from vanadium-containing shale is carried out in the 60 th of the 20 th century, and industrial production is carried out in the 70 th of the century, wherein a technical route of a fire roasting-wet vanadium extraction process and a full-wet vanadium extraction process is generally adopted. The pyro-wet process is usually carried out by sodium roasting or calcic roasting, followed by leaching with acid. However, sulfur and nitrogen oxides are generated during the calcination process, and desulfurization and denitrification treatment are required. Chinese patent CN103270195B adopts a shaft furnace to roast stone coal vanadium ore, and roasting flue gas is desulfurized after dust removal. However, the technique does not involve denitration treatment. The Chinese patent CN103215440B is to add a coal catalyst, a sulfur-fixing agent and a desulfurizing agent into stone coal, and to roast the stone coal at the temperature of 700-. However, the method does not involve denitration treatment, and a catalyst for coal is added to the raw material, increasing the raw material treatment cost. Chinese patent CN112811660A uses a special denitration tower to denitrate the exhaust gas, but does not desulfurize the exhaust gas.
Therefore, in view of the presently disclosed desulfurization and denitrification technology for shale roasting process, there are two main problems: (1) the desulfurization and the denitration need to be separately treated, and the simultaneous removal of sulfur oxides and nitrogen oxides is not realized; (2) the desulfurization and denitrification basically still adopt a special desulfurization and denitrification device, and the in-situ removal of sulfur oxides and nitrogen oxides in the shale roasting process is not realized.
Therefore, by combining the characteristics of the roasting process of the vanadium-containing shale, the in-situ desulfurization and denitrification technology and system in the roasting reactor in the roasting process of the vanadium-containing shale are designed, the flue gas desulfurization and denitrification treatment at the rear end is not needed, the flue gas waste heat recovery is fully considered, and the effective utilization of the sensible heat of the flue gas is realized.
Disclosure of Invention
The invention provides a system and a method for clean roasting modification of vanadium-containing shale, aiming at the problems of desulfurization and denitrification in the roasting process of the existing vanadium-containing shale. The method has the advantages of simple operation, realization of in-situ desulfurization and denitrification in the roasting reactor, elimination of subsequent desulfurization and denitrification links, and realization of recycling of flue gas heat.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for cleaning, roasting and modifying vanadium-containing shale mainly comprises a crushing process 1, a ball milling process 2, a drying and crushing process 3, a preheating process 4, a roasting process 5 and a flue gas dust removal process 6, and specifically comprises the following steps:
1) feeding the raw materials into a crushing process 1 for crushing treatment;
2) mixing the powder obtained in the crushing step 1 with limestone or dolomite, and then sending the mixture into a ball milling step 2 for ball milling treatment to obtain uniformly mixed powder;
3) sending the mixed powder obtained in the ball milling step 2 to a drying and crushing step 3 for drying treatment to obtain dried mixed powder;
4) sending the dry mixed powder obtained in the drying and crushing step 3 into a preheating step 4, and carrying out heat exchange with hot flue gas in a roasting step 5 to preheat;
5) and (3) sending the preheated mixed powder in the preheating step 4 to a roasting step 5, adding a denitration agent, roasting in an air atmosphere to obtain modified shale, sending flue gas generated by roasting to the preheating step 4, then entering a flue gas dedusting step 6, and discharging after dedusting.
Preferably, the addition amount of the limestone or dolomite is 0.5-5.0% of the mass of the powder.
Preferably, the ball milling step 2 ball-mills the mixture to a particle size of 0.10-0.50 mm.
Preferably, in the roasting process 5, a multilayer fluidized bed is used as a roasting reactor, air is used as fluidizing gas, urea is used as a denitration agent, the addition amount is 0.5-5.0% of the mass of the raw materials, the roasting temperature is 800-1000 ℃, and the roasting time is 0.5-4.0 h.
Compared with the prior report technology, the invention has the following outstanding advantages:
(1) the characteristics of the stone coal raw material and the roasting modification conditions are fully utilized, and the desulfurizer is added into the raw material, so that the in-situ desulfurization of the vanadium-containing shale can be realized while the migration of vanadium elements is promoted, and the subsequent additional addition of a desulfurization device is avoided;
(2) by means of the composition characteristics and roasting condition characteristics of the stone coal raw material, a denitration agent is sprayed in an auxiliary mode in the roasting process, and in-situ denitration is achieved, so that a subsequent special denitration device is omitted;
(3) the sensible heat of the roasting modified flue gas is fully utilized, the roasting flue gas and the raw materials are subjected to heat exchange, and the raw materials are preheated, so that the utilization of the sensible heat in the flue gas is realized.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a schematic flow chart of a clean roasting modification method of vanadium-containing shale according to the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
Example 1
FIG. 1 is a schematic flow diagram of a system and a method for modifying vanadium-containing shale by clean roasting according to the present invention. Referring to the figure 1, the method for cleaning, roasting and modifying the vanadium-containing shale mainly comprises a crushing process 1, a ball milling process 2, a drying and crushing process 3, a preheating process 4, a roasting process 5 and a flue gas dust removal process 6, and specifically comprises the following steps:
1) feeding the raw materials into a crushing process 1 for crushing treatment;
2) mixing the powder obtained in the crushing step 1 with limestone or dolomite, and then sending the mixture into a ball milling step 2 for ball milling treatment to obtain uniformly mixed powder;
3) sending the mixed powder obtained in the ball milling step 2 to a drying and crushing step 3 for drying treatment to obtain dried mixed powder;
4) sending the dry mixed powder obtained in the drying and crushing step 3 into a preheating step 4, and carrying out heat exchange with hot flue gas in a roasting step 5 to preheat;
5) and (3) sending the preheated mixed powder in the preheating step 4 to a roasting step 5, adding a denitration agent, roasting in an air atmosphere to obtain modified shale, sending flue gas generated by roasting to the preheating step 4, then entering a dust removal step 6, and discharging after dust removal.
The preheating process adopts primary cyclone preheating and secondary cyclone preheating. The flue gas dust removal process adopts cyclone dust removal and cloth bag dust removal.
Example 2
In this embodiment, the method for modifying the vanadium-containing shale by clean roasting described in example 1 is adopted. After being crushed by a crusher, the vanadium-containing shale is mixed with limestone according to the mass ratio of 1: 0.005 evenly mixing, sending to a ball mill for ball milling treatment, ball milling the mixture until the content of particles with the particle diameter of 0.5mm is not less than 95%, sending the evenly mixed powder obtained by ball milling to a drying and crushing procedure 3 for drying and crushing treatment, drying and crushingThe treated raw materials are sent to a preheating process 4, heat exchange is carried out between the treated raw materials and hot flue gas generated in a roasting process 5 in a secondary cyclone preheater to preheat, the preheated raw materials are sent to the roasting process 5, urea solution with 5% of the mass of the raw materials is sprayed in the preheated raw materials, roasting is carried out in a fluidized bed for 4.0 hours at 800 ℃ in nitrogen atmosphere, and the contents of oxysulfide and nitric oxide in the flue gas are respectively 63mg/m after the flue gas is respectively sent to the preheating process 4 and a flue gas dust removal process 6 through detection3And 213mg/m3And the modified vanadium-containing shale is collected for later use after reaching the direct discharge standard.
Example 3
In this embodiment, the method for modifying the vanadium-containing shale by clean roasting described in example 1 is adopted. After being crushed by a crusher, the vanadium-containing shale is mixed with limestone according to the mass ratio of 1: 0.05, uniformly mixing, conveying to a ball mill for ball milling treatment, ball milling the mixture until the content of particles with the particle diameter of 0.25mm is not less than 95%, conveying the uniformly mixed powder obtained by ball milling to a drying and crushing procedure 3, drying and crushing, conveying the raw material subjected to drying and crushing treatment to a preheating procedure 4, performing heat exchange with hot flue gas generated by a roasting procedure 5 in a secondary cyclone preheater to preheat, conveying the preheated raw material to a roasting procedure 5, spraying urea solution with the mass of 2.5% of the raw material, roasting in a fluidized bed at 900 ℃ for 2.0 hours in nitrogen atmosphere, respectively passing the flue gas through the preheating procedure 4 and a flue gas dedusting procedure 6, and detecting that the contents of oxysulfide and nitric oxide are 71mg/m respectively3And 226mg/m3And the modified vanadium-containing shale is collected for later use after reaching the direct discharge standard.
Example 4
In this embodiment, the method for modifying the vanadium-containing shale by clean roasting described in example 1 is adopted. After being crushed by a crusher, the vanadium-containing shale is mixed with limestone according to the mass ratio of 1: 0.03, uniformly mixing, conveying to a ball mill for ball milling treatment, ball milling the mixture until the content of particles with the particle diameter of 0.3mm is not less than 95%, conveying uniformly mixed powder obtained by ball milling to a drying and crushing process 3, drying and crushing, conveying the raw materials subjected to drying and crushing treatment to a preheating process 4, and mixing with the raw materials generated in a roasting process 5 in a secondary cyclone preheaterPreheating hot flue gas by heat exchange, delivering the preheated raw material to a roasting process 5, spraying urea solution with 3.5% of the raw material mass, roasting in a fluidized bed at 1000 deg.C under nitrogen atmosphere for 0.5h, and detecting that the contents of sulfur oxide and nitrogen oxide are 66mg/m respectively after the flue gas passes through a preheating process 4 and a flue gas dust removal process 6 respectively3And 214mg/m3And the modified vanadium-containing shale is collected for later use after reaching the direct discharge standard.
Example 5
In this embodiment, the method for modifying the vanadium-containing shale by clean roasting described in example 1 is adopted. After being crushed by a crusher, the vanadium-containing shale is mixed with limestone according to the mass ratio of 1: 0.01, uniformly mixing, sending the mixture to a ball mill for ball milling treatment, ball milling the mixture until the content of particles with the particle diameter of 0.2mm is not less than 95%, sending the uniformly mixed powder obtained by ball milling to a drying and crushing process 3, drying and crushing, sending the raw material subjected to drying and crushing treatment to a preheating process 4, carrying out heat exchange with hot flue gas generated by a roasting process 5 in a secondary cyclone preheater to preheat, sending the preheated raw material to a roasting process 5, spraying urea solution with the mass of 3.5% of the raw material, roasting the raw material in a fluidized bed at 850 ℃ for 3.5 hours in nitrogen atmosphere, respectively carrying out preheating process 4 and flue gas dedusting process 6 on the flue gas, and detecting that the contents of oxysulfide and nitric oxide are 73mg/m respectively3And 217mg/m3And the modified vanadium-containing shale is collected for later use after reaching the direct discharge standard.
The method can be realized by upper and lower limit values and interval values of intervals of process parameters (such as temperature, time and the like), and embodiments are not listed.
Conventional technical knowledge in the art can be used for the details which are not described in the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (4)

1. The method mainly comprises a crushing process (1), a ball milling process (2), a drying and crushing process (3), a preheating process (4), a roasting process (5) and a flue gas dedusting process (6), and specifically comprises the following steps:
1) feeding the raw material into a crushing process (1) for crushing treatment;
2) mixing the powder obtained in the crushing step (1) with limestone or dolomite, and then sending the mixture into a ball milling step (2) for ball milling treatment to obtain uniformly mixed powder;
3) sending the mixed powder obtained in the ball milling procedure (2) to a drying and crushing procedure (3) for drying treatment to obtain dried mixed powder;
4) sending the dried mixed powder obtained in the drying and crushing step (3) into a preheating step (4), and carrying out heat exchange with hot flue gas in a roasting step (5) to preheat;
5) and (3) sending the preheated mixed powder in the preheating step (4) to a roasting step (5), adding a denitration agent, roasting in an air atmosphere to obtain modified shale, sending flue gas generated by roasting to the preheating step (4), then entering a flue gas dedusting step (6), and discharging after dedusting.
2. The method for modifying the shale containing vanadium through clean roasting according to claim 1, wherein the addition amount of limestone or dolomite is 0.5-5.0% of the mass of the powder.
3. The method for cleaning, roasting and modifying the shale containing vanadium according to claim 1, wherein the ball milling step (2) is carried out to ball mill the mixed material to 0.10-0.50 mm.
4. The method for cleaning, roasting and modifying the shale containing vanadium according to claim 1, wherein the roasting process (5) adopts a multilayer fluidized bed as a roasting reactor, air as fluidizing gas and urea as a denitration agent, the addition amount of the denitration agent is 0.5-5.0% of the mass of the raw materials, the roasting temperature is 800-1000 ℃, and the roasting time is 0.5-4.0 h.
CN202111193701.8A 2021-10-13 2021-10-13 Clean roasting modification method for vanadium-containing shale Pending CN113801498A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101053749A (en) * 2007-05-30 2007-10-17 武汉钢铁(集团)公司 Method for removing nitrogen oxide in sintering flue gas
CN101503762A (en) * 2009-03-20 2009-08-12 湖南大学 Desulphurization and vanadium extraction technique for calcinated vanadium ore
CN103215440A (en) * 2013-05-17 2013-07-24 尹小林 Desulfuration roasting method of vanadium-extraction stone coal
CN111298620A (en) * 2020-02-27 2020-06-19 中国科学院过程工程研究所 Belt type pellet roasting flue gas desulfurization and denitrification system and method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101053749A (en) * 2007-05-30 2007-10-17 武汉钢铁(集团)公司 Method for removing nitrogen oxide in sintering flue gas
CN101503762A (en) * 2009-03-20 2009-08-12 湖南大学 Desulphurization and vanadium extraction technique for calcinated vanadium ore
CN103215440A (en) * 2013-05-17 2013-07-24 尹小林 Desulfuration roasting method of vanadium-extraction stone coal
CN111298620A (en) * 2020-02-27 2020-06-19 中国科学院过程工程研究所 Belt type pellet roasting flue gas desulfurization and denitrification system and method

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