CN110396593B - Method for high-temperature steam roasting-acid leaching dephosphorization of high-phosphorus iron concentrate - Google Patents
Method for high-temperature steam roasting-acid leaching dephosphorization of high-phosphorus iron concentrate Download PDFInfo
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Abstract
A high-temperature steam roasting-acid leaching dephosphorization method for high-phosphorus iron concentrate comprises the following steps: (1) grinding and screening the high-phosphorus iron concentrate to obtain high-phosphorus iron concentrate powder; (2) conveying to a first-stage cyclone separator through a screw feeder; starting an induced draft fan to form negative pressure; (3) the first-stage solid material formed by gas-solid separation enters a suspension roasting furnace; (4) high-temperature water vapor generated by combustion of a burner enters the suspension roasting furnace to heat the primary solid material; (5) the heated material enters a secondary cyclone separator, secondary gas-solid separation is carried out, and secondary solid material is formed and discharged; (6) and (4) adding the secondary solid material into a stirring leaching tank, stirring and leaching, and filtering and separating the leached material. The method is suitable for the high-phosphorus refractory iron ore which has extremely fine embedded granularity and complex symbiotic relationship and can not be treated by the conventional ore dressing method, so that the iron ore resource is fully utilized, and the high-phosphorus refractory iron ore reaches high indexes in the aspects of iron grade, iron recovery rate and dephosphorization rate of products.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a high-temperature steam roasting-acid leaching dephosphorization method for high-phosphorus iron concentrate.
Background
The high-phosphorus iron ore is one of important complex and refractory iron ore resources, and has the characteristics of high iron grade, large reserve and high phosphorus content, so that the high-phosphorus iron ore has important significance in solving the problem of high-efficiency utilization of the high-phosphorus iron ore; the storage amount of the high-phosphorus iron ore in China is up to 74.5 hundred million tons, and the high-phosphorus iron ore is mainly distributed in Yangtze river drainage basins and Yunnan provinces, such as the phosphorus-containing iron ore in Meishan, the Ningxiang iron ore in Hubei, and the like; the high-phosphorus iron ore belongs to weak magnetic iron ores and mainly comprises two main types of hydrothermal type hematite and siderite, wherein the occurrence state of phosphorus in the hydrothermal type iron ore mainly comprises apatite, and the occurrence state of phosphorus in the sedimentary type iron ore mainly exists in the form of granular collophanite.
At present, iron-extracting and phosphorus-reducing methods for high-phosphorus iron ores mainly comprise magnetic separation, flotation, acid leaching, microbial leaching and other modes, but iron concentrates obtained by different methods generally have high phosphorus content (P is more than 0.25 percent) and cannot be used as qualified raw materials for blast furnace ironmaking; even if qualified iron ore concentrate is obtained, the defects of high process cost, low iron recovery rate and the like exist; therefore, the technology and process for efficiently dephosphorizing the high-phosphorus iron concentrate still need to be developed.
Disclosure of Invention
Aiming at the problems in the high-phosphorus iron concentrate dephosphorization utilization method, the invention provides the high-temperature steam roasting-acid leaching dephosphorization method for the high-phosphorus iron concentrate, the high-temperature steam roasting is matched with acid leaching dephosphorization, the recovery rate of iron and the grade of concentrate iron products are improved, and the phosphorus content in the concentrate is reduced.
The method of the invention is carried out according to the following steps:
(1) grinding the high-phosphorus iron concentrate until the part with the particle size of-0.074 mm accounts for more than or equal to 65 percent of the total mass, and screening the part with the particle size of less than or equal to 0.8mm to be used as high-phosphorus iron concentrate powder;
(2) putting the high-phosphorus iron concentrate powder material into a storage bin, and conveying the high-phosphorus iron concentrate powder material into a primary cyclone separator through a screw feeder; the discharge hole of the primary cyclone separator is communicated with the feed inlet at the lower part of the suspension roasting furnace, and the top of the suspension roasting furnace is communicated with the feed inlet of the secondary cyclone separator through an upper channel; the air outlet of the secondary cyclone separator is communicated with the feed inlet of the primary cyclone separator, the air outlet of the primary cyclone separator is communicated with the feed inlet of the dust removing equipment, and the air outlet of the dust removing equipment is communicated with the induced draft fan; starting an induced draft fan, and forming negative pressure in the primary cyclone separator, the suspension roasting furnace and the secondary cyclone separator;
(3) under the action of negative pressure, carrying out gas-solid separation on the high-phosphorus iron ore concentrate powder in a primary cyclone separator to form a primary solid material; the first-stage solid material enters the bottom of the suspension roasting furnace;
(4) a burner is arranged at the bottom of the suspension roasting furnace; introducing gas and combustion-supporting air into the combustor, and combusting by the combustor to generate high-temperature water vapor; high-temperature steam enters the suspension roasting furnace from the bottom of the suspension roasting furnace to heat the primary solid material;
(5) the heated material enters a secondary cyclone separator from an upper passage, and after secondary gas-solid separation is carried out in the secondary cyclone separator, the formed secondary solid material is discharged from a discharge hole of the secondary cyclone separator under the action of gravity;
(6) a discharge port of the secondary cyclone separator is opposite to the stirring leaching tank, and a sulfuric acid solution is placed in the stirring leaching tank; and (3) feeding the secondary solid material into a stirring leaching tank through a discharge port for stirring leaching, filtering and separating the generated leaching material, washing the solid phase with water and drying to obtain the dephosphorization iron concentrate.
The high-phosphorus iron concentrate contains 0.5-1.5% of P by mass percent, and the iron grade is 55-63%.
The fuel gas is natural gas, liquefied petroleum gas or coal gas.
In the method, the volume flow ratio of the fuel gas introduced into the combustor to the combustion-supporting air is 1: 12-1: 15, and H in the high-temperature steam is2The volume percentage of O is more than or equal to 10 percent.
In the method, the volume mass flow ratio of the high-temperature steam to the primary solid material in unit time is 4-6 m3/kg。
In the method, the temperature in the suspension roasting furnace is 1050-1200 ℃, and the residence time of the primary solid material in the suspension roasting furnace is 15-30 s.
In the method, after gas-solid separation is carried out in the primary cyclone separator, the generated primary tail gas enters the dust removal equipment, and is discharged by the induced draft fan after dust removal.
In the method, after secondary gas-solid separation is carried out in the secondary cyclone separator, the generated secondary tail gas enters the primary cyclone separator.
In the method, the initial concentration of the sulfuric acid solution is 0.05-0.3 mol/L, the liquid-solid ratio of the sulfuric acid solution to the secondary solid material is 4-6L/kg when agitation leaching is carried out, the temperature of the agitation leaching is 10-35 ℃, and the time is 15-30 min.
In the method, the stirring speed during stirring leaching is 15-30 r/min.
The iron grade of the dephosphorized iron concentrate is 63-65%, and the P content is less than or equal to 0.1% by mass percent.
In the method, the recovery rate of the iron is more than or equal to 92 percent. .
The principle of the invention is as follows: the phosphorus in the high-phosphorus iron concentrate exists mainly in the form of apatite, which is a generic name of calcium-containing phosphate minerals and can be specifically divided into fluorapatite and chlorophosphite ashAnd hydroxyapatite whose chemical composition may be abbreviated as Ca10(PO4)6(F,Cl,OH)2(ii) a The apatite is mainly fluorapatite Ca10(PO4)6F2(ii) a Burning hydrogen-containing components (such as methane, ethane, propane, hydrogen, etc.) such as natural gas, liquefied petroleum gas, coal gas, etc. in a burner to generate high-temperature water vapor (H)2O), mixing with fluorapatite Ca in a suspension roasting furnace10(PO4)6F2And the following reactions occur:
Ca10(PO4)6F2+2H2O＝Ca10(PO4)6(OH)2+2HF
and
Ca10(PO4)6(OH)2＝3Ca3(PO4)2+CaO+H2O；
the fluorapatite is converted into hydroxyapatite Ca with poor thermal stability under the action of high-temperature water vapor10(PO4)6(OH)2The hydroxyapatite is continuously decomposed at high temperature to generate tricalcium phosphate Ca which is easy to leach3(PO4)2And the internal structure of the ore particles is in a loose and porous state, so that the effect of acid leaching dephosphorization of the high-phosphorus iron concentrate is enhanced.
Compared with the prior art, the invention has the outstanding characteristics that:
1. the method takes the high-phosphorus iron concentrate as a raw material, and is particularly suitable for high-phosphorus refractory iron ores which have extremely fine embedded granularity and complex symbiotic relationship and cannot be treated by a conventional ore dressing method, so that iron ore resources are fully utilized;
2. qualified iron ore concentrate with the iron grade of more than or equal to 63 percent, the iron recovery rate of more than or equal to 92 percent and the phosphorus content of less than or equal to 0.1 percent can be produced;
3. the process equipment is mature in each stage, the adaptability to the high-phosphorus iron concentrate obtained by the common ore dressing method is strong, and the high-phosphorus iron concentrate reaches high indexes in the aspects of iron grade, iron recovery rate and dephosphorization rate of products.
Drawings
FIG. 1 is a schematic structural diagram of a high-temperature steam roasting-acid leaching dephosphorization apparatus for high-phosphorus iron concentrate in an embodiment of the present invention;
in the figure, the device comprises a bin 1, a bin 2, a screw feeder 3, a primary cyclone separator 4, a dust removing device 5, an induced draft fan 6, a burner 7, a suspension roasting furnace 8, an upper channel 9, a secondary cyclone separator 10 and a stirring and leaching tank.
Detailed Description
The following examples are only to illustrate the present invention.
In the embodiment of the invention, the washing is carried out until the washing liquor is neutral, the drying temperature is 120 +/-5 ℃, and the drying is carried out until the mass percentage of water is less than or equal to 0.1%.
Compared with the traditional mode, the dephosphorization rate and the iron recovery rate of the embodiment of the invention are respectively improved by 10-20% and 5-20%, and the dosage and roasting time of natural gas are adjusted according to the species characteristics of different iron ore powders, so that the best strengthening effect can be achieved.
In the embodiment of the invention, the iron grade TFe of the high-phosphorus iron concentrate is 47-51 percent, and the high-phosphorus iron concentrate comprises 7-15 percent of FeO and SiO by mass percentage29～16％，Al2O34.6～5％，CaO 2～5％，MgO 0.4～0.7％，P 0.5～1.5％，S≤0.05％，MnO20.4～1.1％，TiO20.2～0.4％。
The structure of the device for roasting, acid leaching and dephosphorizing high-temperature steam of high-phosphorus iron concentrate in the embodiment of the invention is shown in figure 1, and the device comprises a storage bin 1, a screw feeder 2, a primary cyclone separator 3, a suspension roasting furnace 7, a secondary cyclone separator 9 and a stirring and leaching tank 10; an outlet of the bin 1 is communicated with an inlet 2 of the screw feeder, an outlet of the screw feeder 2 is communicated with a feed inlet of a primary cyclone separator 3, a discharge outlet of the primary cyclone separator 3 is communicated with a feed inlet at the lower part of a suspension roasting furnace 7, the top of the suspension roasting furnace 7 is communicated with a feed inlet of a secondary cyclone separator 9 through an upper channel 8, and a discharge outlet of the secondary cyclone separator 9 is opposite to a stirring leaching tank 10; wherein, the bottom of the suspension roaster 7 is provided with a burner 6, the gas outlet of the secondary cyclone separator 9 is communicated with the feed inlet of the primary cyclone separator 3, the gas outlet of the primary cyclone separator 3 is communicated with the feed inlet of the dust removing device 4, and the gas outlet of the dust removing device 4 is communicated with the induced draft fan 5.
In the embodiment of the invention, the stirring speed during stirring leaching is 15-30 r/min.
Example 1
The adopted high-phosphorus iron ore concentrate is certain domestic high-phosphorus iron ore, the iron grade is 50.65%, iron and phosphorus are partially symbiotic, and the high-phosphorus iron ore concentrate contains 0.83% of P, 14.35% of FeO and SiO according to mass percentage29.48％，Al2O34.78％，CaO 2.15％，MgO 0.48％，P0.83％，S 0.042％，MnO21.03％，TiO20.38％；
The method adopts a device of high-temperature steam roasting-acid leaching dephosphorization of high-phosphorus iron concentrate, and comprises the following steps:
grinding the high-phosphorus iron concentrate until the part with the particle size of-0.074 mm accounts for 70 percent of the total mass, and screening the part with the particle size of less than or equal to 0.8mm to be used as high-phosphorus iron concentrate powder;
putting the high-phosphorus iron concentrate powder material into a storage bin, and conveying the high-phosphorus iron concentrate powder material into a primary cyclone separator through a screw feeder; at the moment, a draught fan, a primary cyclone separator, a suspension roasting furnace and a secondary cyclone separator are started to form negative pressure;
under the action of negative pressure, carrying out gas-solid separation on the high-phosphorus iron ore concentrate powder in a primary cyclone separator to form a primary solid material; the first-stage solid material enters the bottom of the suspension roasting furnace; after gas-solid separation is carried out in the primary cyclone separator, the generated primary tail gas enters dust removal equipment, and is discharged by a draught fan after dust removal;
introducing gas and air into the combustor, and combusting by the combustor to generate high-temperature water vapor; high-temperature steam enters the suspension roasting furnace from the bottom of the suspension roasting furnace to heat the primary solid material; the fuel gas is natural gas; the volume flow ratio of fuel gas to air is 1:12, and H in high-temperature steam218% by volume of O; the volume mass flow ratio of the high-temperature water vapor to the first-grade solid material in unit time is 5.8m3Per kg; the temperature in the suspension roasting furnace is 1050 ℃, and the retention time of the primary solid material in the suspension roasting furnace is 28 s;
the heated material enters a secondary cyclone separator from an upper passage, and after secondary gas-solid separation is carried out in the secondary cyclone separator, the formed secondary solid material is discharged from a discharge hole of the secondary cyclone separator under the action of gravity and enters a stirring leaching tank; after secondary gas-solid separation is carried out in the secondary cyclone separator, the generated secondary tail gas enters the primary cyclone separator;
a sulfuric acid solution is placed in the stirring leaching tank; the secondary solid material enters a stirring leaching tank for stirring leaching, wherein the initial concentration of a sulfuric acid solution is 0.1mol/L, the liquid-solid ratio of the sulfuric acid solution to the secondary solid material is 6L/kg when the stirring leaching is carried out, the stirring leaching temperature is 28 ℃, and the time is 20 min; filtering and separating the generated leached materials, washing and drying the solid phase to obtain a dephosphorization iron concentrate, wherein the iron grade is 64.36 percent, and the P content is 0.09 percent by mass percent; the recovery of iron was 93.89%. .
Example 2
The adopted high-phosphorus iron ore concentrate is high-phosphorus iron ore in China, iron and phosphorus are partially symbiotic, the iron grade is 47.35 percent, and the high-phosphorus iron ore concentrate contains 0.9 percent of P, 7.81 percent of FeO and SiO according to the mass percentage215.80％，Al2O34.67％，CaO 4.63％，MgO 0.49％，P0.90％，S 0.03％，MnO20.41％，TiO20.20％。
The method is the same as example 1, except that:
(1) grinding the high-phosphorus iron concentrate until the part with the particle size of-0.074 mm accounts for 80 percent of the total mass;
(2) the fuel gas is liquefied petroleum gas; the volume flow ratio of fuel gas to air is 1:15, and H in high-temperature steam220% by volume of O; the volume mass flow ratio of the high-temperature water vapor to the first-grade solid material in unit time is 4.3m3Per kg; the temperature in the suspension roasting furnace is 1100 ℃, and the retention time of the primary solid material in the suspension roasting furnace is 17 s;
(3) the initial concentration of the sulfuric acid solution is 0.08mol/L during agitation leaching, the liquid-solid ratio of the sulfuric acid solution to the secondary solid material is 4L/kg during agitation leaching, the temperature of the agitation leaching is 20 ℃, and the time is 30 min;
(4) the iron grade of the dephosphorization iron concentrate is 63.99 percent, and the P content is 0.08 percent by mass percent; the recovery of iron was 94.24%.
Example 3
The adopted high-phosphorus iron ore concentrate is high-phosphorus iron ore in China, iron and phosphorus are partially symbiotic, the iron grade is 49.35 percent, and the high-phosphorus iron ore concentrate contains 0.79 percent of P, 12.19 percent of FeO and SiO according to the mass percentage210.50％，Al2O35.00％，CaO 2.48％，MgO 0.64％，P0.79％，S 0.05％，MnO20.64％，TiO20.36％。
The method is the same as example 1, except that:
(1) grinding the high-phosphorus iron concentrate until the part with the particle size of-0.074 mm accounts for 75 percent of the total mass;
(2) the fuel gas is coal gas; the volume flow ratio of fuel gas to air is 1:13, H in high-temperature steam219% by volume of O; the volume mass flow ratio of the high-temperature water vapor to the first-grade solid material in unit time is 5.5m3Per kg; the temperature in the suspension roasting furnace is 1200 ℃, and the retention time of the primary solid material in the suspension roasting furnace is 22 s;
(3) the initial concentration of the sulfuric acid solution is 0.15mol/L during agitation leaching, the liquid-solid ratio of the sulfuric acid solution to the secondary solid material is 5L/kg during agitation leaching, the temperature of the agitation leaching is 25 ℃, and the time is 25 min;
(4) the iron grade of the dephosphorization iron concentrate is 63.56 percent, and the P content is 0.06 percent by mass; the recovery of iron was 92.59%.
Claims (8)
1. A high-temperature steam roasting-acid leaching dephosphorization method for high-phosphorus iron concentrate is characterized by comprising the following steps of:
(1) grinding the high-phosphorus iron concentrate until the part with the particle size of-0.074 mm accounts for more than or equal to 65 percent of the total mass, and screening the part with the particle size of less than or equal to 0.8mm to be used as high-phosphorus iron concentrate powder;
(2) putting the high-phosphorus iron concentrate powder material into a storage bin, and conveying the high-phosphorus iron concentrate powder material into a primary cyclone separator through a screw feeder; the discharge hole of the primary cyclone separator is communicated with the feed inlet at the lower part of the suspension roasting furnace, and the top of the suspension roasting furnace is communicated with the feed inlet of the secondary cyclone separator through an upper channel; the air outlet of the secondary cyclone separator is communicated with the feed inlet of the primary cyclone separator, the air outlet of the primary cyclone separator is communicated with the feed inlet of the dust removing equipment, and the air outlet of the dust removing equipment is communicated with the induced draft fan; starting an induced draft fan, and forming negative pressure in the primary cyclone separator, the suspension roasting furnace and the secondary cyclone separator;
(3) under the action of negative pressure, carrying out gas-solid separation on the high-phosphorus iron ore concentrate powder in a primary cyclone separator to form a primary solid material; the first-stage solid material enters the bottom of the suspension roasting furnace;
(4) a burner is arranged at the bottom of the suspension roasting furnace; introducing gas and combustion-supporting air into the combustor, and combusting by the combustor to generate high-temperature water vapor; high-temperature steam enters the suspension roasting furnace from the bottom of the suspension roasting furnace to heat the primary solid material; the volume flow ratio of fuel gas introduced into the combustor to combustion air is 1: 12-1: 15, and H in high-temperature steam2The volume percentage of O is 10-20%; the volume mass flow ratio of the high-temperature steam to the first-stage solid material in unit time is 4-6 m3/kg；
(5) The heated material enters a secondary cyclone separator from an upper passage, and after secondary gas-solid separation is carried out in the secondary cyclone separator, the formed secondary solid material is discharged from a discharge hole of the secondary cyclone separator under the action of gravity;
(6) a discharge port of the secondary cyclone separator is opposite to the stirring leaching tank, and a sulfuric acid solution is placed in the stirring leaching tank; and (3) feeding the secondary solid material into a stirring leaching tank through a discharge port for stirring leaching, filtering and separating the generated leaching material, washing the solid phase with water and drying to obtain the dephosphorization iron concentrate.
2. The method of high temperature steam roasting-acid leaching dephosphorization of high-phosphorus iron concentrate according to claim 1, wherein the high-phosphorus iron concentrate contains 0.5-1.5% by mass of P and has an iron grade of 55-63%.
3. The method for dephosphorization of high-phosphorus iron concentrate by high-temperature steam roasting-acid leaching according to claim 1, wherein said fuel gas is natural gas, liquefied petroleum gas or coal gas.
4. The high-temperature steam roasting-acid leaching dephosphorization method for the high-phosphorus iron concentrate according to claim 1, wherein in the step (4), the temperature in the suspension roasting furnace is 1050-1200 ℃, and the retention time of the primary solid material in the suspension roasting furnace is 15-30 s.
5. The method for dephosphorization by high-temperature steam roasting-acid leaching of high-phosphorus iron concentrate according to claim 1, characterized in that in the step (6), the initial concentration of the sulfuric acid solution is 0.05-0.3 mol/L, the liquid-solid ratio of the sulfuric acid solution to the secondary solid material is 4-6L/kg when agitation leaching is carried out, the temperature of the agitation leaching is 10-35 ℃, and the time is 15-30 min.
6. The method for dephosphorization by high-temperature steam roasting-acid leaching of high-phosphorus iron concentrate according to claim 1, wherein in the step (6), the stirring speed during the stirring leaching is 15-30 r/min.
7. The method for high-temperature steam roasting-acid leaching dephosphorization of high-phosphorus iron concentrate according to claim 1, wherein the iron grade of the dephosphorization iron concentrate is 63-65%, and the phosphorus content is less than or equal to 0.1% by mass percentage.
8. The method for dephosphorization of high-phosphorus iron concentrate by high-temperature steam roasting-acid leaching according to claim 1, characterized in that the recovery rate of iron is more than or equal to 92%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1283222A (en) * | 1997-12-26 | 2001-02-07 | 日本钢管株式会社 | Refining method of molten iron and reduction smelting method for producing molten iron |
| CN102230075A (en) * | 2011-06-20 | 2011-11-02 | 江苏大学 | Dephosphorizing process of molybdenum nickel ore |
| CN108707746A (en) * | 2018-06-27 | 2018-10-26 | 东北大学 | The method that two-stage roasting-magnetic separation-leaching high-phosphor oolitic hematite carries iron drop phosphorus |
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| JPS63270427A (en) * | 1987-04-24 | 1988-11-08 | Chiyoda Chem Eng & Constr Co Ltd | Method for removing deposited solid matter containing gallium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1283222A (en) * | 1997-12-26 | 2001-02-07 | 日本钢管株式会社 | Refining method of molten iron and reduction smelting method for producing molten iron |
| CN102230075A (en) * | 2011-06-20 | 2011-11-02 | 江苏大学 | Dephosphorizing process of molybdenum nickel ore |
| CN108707746A (en) * | 2018-06-27 | 2018-10-26 | 东北大学 | The method that two-stage roasting-magnetic separation-leaching high-phosphor oolitic hematite carries iron drop phosphorus |
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