Method for preparing ultrapure iron concentrate by deep processing of commercial grade magnetite concentrate
Technical Field
The invention belongs to the technical field of magnetite beneficiation, and particularly relates to a method for preparing ultrapure iron concentrate from high-quality commercial grade magnetite.
Background
With the continuous development of national economy, the demand of products such as permanent magnet materials, reduced iron and the like is increasing day by day, and the quality requirement of the products is higher and higher. At present, the raw materials for preparing permanent magnet materials (ferrite) and reduced iron powder are mainly iron oxide red and iron scale, and because the iron oxide red and the iron scale have small yield, high price and unstable quality, a new cheap raw material substitute is sought, and an important research subject to be solved is urgently needed.
The ultra-pure iron ore concentrate is the first choice raw material for many permanent magnetic ferrite pre-sintering material production units due to fine granularity, high quality and wide source. The ultra-pure iron concentrate generally requires TFe grade of more than 71.5 percent and SiO2The content of impurities (acid insoluble substances) is less than 0.3 percent, is an important raw material source of the novel iron-based mineral material, and can be used for producing powder metallurgy, magnetic materials, ultra-pure iron, clean steel base materials and the like.
Although iron ore resources are abundant in China, the resources suitable for processing ultra-pure iron ore concentrates are very limited and are mainly distributed in a few areas of Liaoning, Anhui, Shanxi, Fujian, Sichuan, Shandong and the like. The "beneficiation process of ultrapure iron ore concentrate and effective way for development and utilization" published in metal mine 1997, 12 th period summarizes three process flows for preparing ultrapure iron ore concentrate by beneficiation: (1) a magnetic-floating combined process, namely feeding, grinding, classifying by a cyclone, overflowing low intensity magnetic separation and magnetic fine cation reverse flotation; (2) a single magnetic separation process; (3) the stage grinding and magnetic-gravity combined process. "research on mineral separation experiment for preparing ultrapure iron ore concentrate from iron ore concentrate powder" published in 2009, metal mine, No. 5, contained 67.70% of TFeS and SiO24.88 percent of common iron ore concentrate is used as a raw material, and ore grinding, low-intensity magnetic separation, magnetic gravity separation and reverse flotation are adoptedThe process can produce TFe72.02% and SiO20.27% of ultra pure iron concentrate. "test for preparing ultrapure iron concentrate by magnetic separation column", published in 2018, 7, of the modern mining industry, a process flow of classification, grinding, weak magnetic rough separation and magnetic separation column fine separation is adopted by taking a common iron concentrate with an iron grade of 66.12% in Shandong as a raw material to obtain an iron grade of 71.64%, a recovery rate of 81.87% and SiO20.23% of ultra pure iron ore concentrate. However, the iron grade of the concentrate in the ultra-pure iron concentrate produced by the above method is still not ideal in general, especially in the case of SiO2The content and the content of acid insoluble substances are still high.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing ultrapure iron concentrate by deep processing of commercial grade magnetite concentrate, and TFe in the prepared ultrapure iron concentrate>72.1%、SiO2The content is less than or equal to 0.20 percent and the content of acid insoluble substances is less than or equal to 0.17 percent.
In order to realize the aim, the invention provides a method for preparing ultrapure iron concentrate by deep processing of commercial grade magnetite concentrate, which uses TFe at 66.5-68.5% and SiO2Commercial grade magnetite concentrate with the content of 4.0-6.8 percent is taken as a raw material, and the following process is adopted:
(1) first-stage grinding-grading operation: feeding commercial grade magnetite concentrate into a ball mill for grinding and grading by a spiral classifier, wherein the overflow granularity of the spiral classifier is-0.076 mm and accounts for 90-95%, and the grinding volume concentration of the ball mill is controlled to be 25-30%;
(2) one-section low-intensity magnetic separation operation: carrying out low-intensity magnetic separation on the overflow of the spiral classifier obtained in the step (1) to obtain a section of low-intensity magnetic separation concentrate, and discharging a section of low-intensity magnetic separation tailings; the low-intensity magnetic separation adopts a permanent magnet drum magnetic separator, and the magnetic field intensity is 135.00-165.00 kA/m.
(3) Concentrating and dehydrating the first-stage low-intensity magnetic concentrate: concentrating and dehydrating the first-stage low-intensity magnetic separation concentrate obtained in the step (2), and controlling the mass concentration of the concentrated underflow ore pulp to be 55-65%;
(4) two-stage ore grinding-grading operation: feeding the concentrated underflow obtained in the step (3) into a second-stage ore grinding-grading operation, wherein the second-stage ore grinding adopts a vertical stirring mill, the grading adopts a cyclone, the grading overflow granularity of the cyclone is controlled to be-0.038 mm and accounts for 88-95%, and the ore grinding volume concentration of the vertical stirring mill is controlled to be 26-35%;
(5) two-stage low-intensity magnetic separation rough concentration, demagnetization and two-stage low-intensity magnetic separation fine concentration operation: carrying out secondary low-intensity magnetic separation roughing on the grading overflow obtained in the step (4) to obtain secondary low-intensity magnetic separation roughing concentrate, and discharging secondary low-intensity magnetic separation roughing tailings; demagnetizing the second-stage low-intensity magnetic separation rough concentration ore, feeding the second-stage low-intensity magnetic separation fine concentration ore to obtain second-stage low-intensity magnetic separation fine concentration ore, and discharging second-stage low-intensity magnetic separation fine concentration tailings;
the two-stage low-intensity magnetic separation rough separation and the two-stage low-intensity magnetic separation fine separation both adopt permanent magnet drum magnetic separators; the magnetic field intensity of the two-stage low-intensity magnetic separation rough concentration is 150.00-165.00 kA/m, and the magnetic field intensity of the two-stage low-intensity magnetic separation fine concentration is 101.00-130.00 kA/m;
controlling TFe of the two-stage low intensity magnetic separation concentration concentrate by cooperatively adjusting the process conditions of the steps (1), (2), (3), (4) and (5)>71.2%、SiO2The content is less than or equal to 0.7 percent;
(6) performing two-stage low-intensity magnetic separation and concentration concentrate demagnetizing-concentrating operation: demagnetizing the two-stage low intensity magnetic separation concentrated concentrate obtained in the step (5), and concentrating, wherein the mass concentration of the concentrated underflow pulp is controlled to be 32-40%;
(7) reverse flotation operation: feeding the concentrated underflow obtained in the step (6) into reverse flotation operation, wherein the reverse flotation operation adopts a primary roughing and a secondary fine separation open-circuit process, and a collecting agent adopted in the reverse flotation operation is prepared by heating and modifying dodecylamine and glacial acetic acid solution according to a mass ratio of 4: 0.9-4: 1.1; the medicament system is as follows: the dosage of the collecting agent for rough concentration is 55-65 g/t, the dosage of the collecting agent for fine concentration is 23-32 g/t, and the dosage of the collecting agent for fine concentration is 15-22 g/t; the reverse flotation operation finally obtains the flotation tank bottom TFe>72.0%、SiO2The content is less than or equal to 0.20 percent, the content of acid insoluble substances is less than or equal to 0.17 percent of ultrapure iron ore concentrate, and the flotation foam is TFe70.7 percent of high-purity iron ore concentrate;
further, the collecting agent adopted in the reverse flotation operation in the step (7) is prepared by mixing laurylamine and glacial acetic acid solution according to the mass ratio of 4: 1 and heating with hot water at 90-100 ℃ for modification.
Compared with the prior art, the method for preparing the ultrapure iron concentrate by the deep processing of the commercial grade magnetite concentrate has the following advantages:
(1) the grinding is flexible and variable by combining ball milling and vertical stirring milling, the grinding granularity of the ball milling is close to that of most commercial-grade iron ore concentrates, whether ball milling equipment needs to be added or not can be considered in the process of process improvement, the grinding granularity of the vertical stirring milling is uniform and easy to control, the occupied area is small, and the grinding is efficient and energy-saving.
(2) The two-stage magnetic separation and the two-stage magnetic separation are respectively subjected to demagnetizing treatment before and after the two-stage magnetic separation and concentration, so that the influence of magnetic groups on the magnetic separation and flotation processes is avoided, and the separation index is favorably improved.
(3) The flotation reagent system is simple, the collecting agent is prepared by mixing, heating and modifying dodecylamine and glacial acetic acid solution according to the mass ratio of 4: 1, the source of raw materials is wide, the dosage is small, the selectivity is good, and the method is very environment-friendly.
(4) The mineral processing process is simple, stable and reliable, and has strong applicability. According to the selection grade and the selection difficulty degree of commercial grade magnetite concentrate, the TFe grade in the obtained ultrapure iron concentrate is as high as 72.10-72.19 percent, and SiO2The content is 0.18-0.20 percent, and the content of acid insoluble substances is 0.15-0.17 percent. Meanwhile, high-purity iron ore concentrate with TFe grade of 70.86-71.12% can be obtained.
Drawings
FIG. 1 is a schematic process flow diagram of a method for producing ultrapure iron concentrate by further processing commercial grade magnetite concentrate according to the present invention;
fig. 2 is a mass flow chart of a method for preparing ultrapure iron concentrate by deep processing of commercial grade magnetite concentrate according to the present invention.
Detailed Description
For the purpose of describing the present invention, the following description will be made in detail with reference to the accompanying drawings and examples for the preparation of ultrapure iron concentrate by further processing of commercial grade magnetite concentrate according to the present invention.
The TFe grade of a certain commercial grade magnetite concentrate in China is 66.83 percent, and the main impurity SiO is2、Al2O3CaO and MgO contents of 6.18%, 0.68%, 0.28% and 0.22% respectively,the content of other impurity elements is low.
As shown in fig. 1 and shown in fig. 2, the method for preparing ultrapure iron concentrate by deep processing of commercial grade magnetite concentrate of the present invention adopts the following steps:
(1) first-stage grinding-grading operation: the commercial grade magnetite concentrate is fed into a ball mill for grinding and grading by a spiral classifier, the overflow granularity of the spiral classifier is-0.076 mm and accounts for 95 percent, and the grinding volume concentration of the ball mill is controlled to be 28 percent;
(2) one-section low-intensity magnetic separation operation: carrying out low-intensity magnetic separation on the overflow of the spiral classifier obtained in the step (1) to obtain a section of low-intensity magnetic separation concentrate with TFe grade of 68.95%, and discharging a section of low-intensity magnetic separation tailings with TFe grade of 12.44%; the low-intensity magnetic separation adopts a permanent magnetic drum magnetic separator, and the magnetic field intensity is 159.24 kA/m;
(3) concentrating and dehydrating the first-stage low-intensity magnetic concentrate: concentrating and dehydrating the obtained first-stage low-intensity magnetic separation concentrate, and controlling the mass concentration of the concentrated underflow ore pulp to be 58%;
(4) two-stage ore grinding-grading operation: feeding the concentrated underflow obtained in the step (3) into a second-stage ore grinding-grading operation, wherein the second-stage ore grinding adopts a vertical stirring mill, the grading adopts a cyclone, the grading overflow particle size of the cyclone is controlled to be-0.038 mm and accounts for 90%, and the ore grinding volume concentration of the vertical stirring mill is controlled to be 31%;
(5) two-stage low-intensity magnetic separation rough concentration, demagnetization and two-stage low-intensity magnetic separation fine concentration operation: carrying out secondary low-intensity magnetic separation roughing on the grading overflow obtained in the step (4) to obtain secondary low-intensity magnetic separation roughing concentrate with TFe grade of 71.14%, and discharging secondary low-intensity magnetic separation roughing tailings with TFe grade of 12.92%; demagnetizing the second-stage low-intensity magnetic separation rough concentration ore, feeding the second-stage low-intensity magnetic separation fine concentration ore to obtain a second-stage low-intensity magnetic separation fine concentration ore with the TFe grade of 71.41%, and discharging second-stage low-intensity magnetic separation fine concentration tailings with the TFe grade of 28.81%; the two-stage low-intensity magnetic separation concentration tailings can be used as iron ore raw materials of a concentrating mill, and can also be directly incorporated into total tailings.
The two-stage low-intensity magnetic separation rough separation and the two-stage low-intensity magnetic separation fine separation both adopt permanent magnet drum magnetic separators; the magnetic field intensity of the two-stage low-intensity magnetic separation rough concentration is 159.24kA/m, and the magnetic field intensity of the two-stage low-intensity magnetic separation fine concentration is 127.39 kA/m;
(6) performing two-stage low-intensity magnetic separation and concentration concentrate demagnetizing-concentrating operation: demagnetizing the two-stage low intensity magnetic separation concentrated concentrate obtained in the step (5), and concentrating, wherein the mass concentration of the concentrated underflow pulp is controlled at 36.5%;
(7) reverse flotation operation: feeding the concentrated underflow obtained in the step (6) into reverse flotation operation, wherein the reverse flotation operation adopts a primary roughing and a secondary fine concentration open-circuit process, and a collecting agent adopted in the reverse flotation operation is prepared by heating and modifying dodecylamine and glacial acetic acid solution according to the mass ratio of 4: 1; the medicament system is as follows: the using amount of the rough concentration collecting agent is 60g/t, the using amount of the collecting agent in the first concentration is 30g/t, and the using amount of the collecting agent in the second concentration is 20 g/t; the reverse flotation operation finally obtains the flotation tank bottom TFe>72.10%、SiO2The content of the ultra-pure iron concentrate is 0.17 percent, and the flotation froth is TFe70.86 percent high-purity iron concentrate.
Research shows that the collector is prepared by mixing and heating dodecylamine and glacial acetic acid solution according to the mass ratio of 4: 1 and modifying, and the collector has an obvious using effect. If only dodecylamine is used as a collector, only TFe 71.5% -71.8% and SiO can be obtained2The ultra-pure iron ore concentrate with the content of 0.22 to 0.25 percent and the acid insoluble substance of 0.20 to 0.23 percent can not obtain TFe>72.0%、SiO2The content is less than or equal to 0.20 percent, and the content of acid insoluble substances is less than or equal to 0.17 percent.