CN113968610B - Method for preparing biological flocculant by using biological iron-calcium slag in biological heap leaching - Google Patents
Method for preparing biological flocculant by using biological iron-calcium slag in biological heap leaching Download PDFInfo
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Abstract
The invention discloses a method for preparing a biological flocculant by utilizing biological iron-calcium slag in biological heap leaching, which utilizes the biological iron-calcium slag generated in the hydrometallurgy biological heap leaching process of low-grade copper ores to leach and concentrate iron in the biological iron-calcium slag, and comprises the following three main steps: (1) pre-separating iron and calcium: mixing the biological iron-calcium slag and the raffinate in proportion to obtain iron-rich raffinate, and then adding limestone to neutralize to obtain biological iron-rich slag; (2) multistage countercurrent leaching: biological iron-rich slag is circularly leached in a countercurrent way in the system through two stages of leaching tanks connected in series; (3) and (3) colloid destabilization separation: and (3) subjecting the mixed solution to ultrasonic destabilization and high-temperature viscosity reduction, and then performing filter pressing to obtain the biological flocculant. The invention has low production cost, the concentration of iron in the leaching solution is more than 100g/L, and the leaching solution can be used as a biological flocculant, thereby solving the problem of the accumulation of biological iron and calcium slag of enterprises, reducing the environmental protection risk and pressure, and creating economic benefit for the enterprises at the same time.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy post-treatment, in particular to a method for synthesizing a bioflocculant by utilizing biological iron and calcium slag resources generated in a copper sulfide ore biological wet dump leaching system.
Background
Copper-containing minerals are at least 360 kinds in nature, and these copper minerals can be divided into copper sulfide minerals and copper oxide minerals. The copper minerals in China are mainly sulfide ores. In the identified reserves, the sulphide ore accounts for 97%, the oxide ore station 10%, and the mixed ore accounts for 3%.
The copper sulfide mineral grade is low, and the traditional copper smelting technology is not suitable. Therefore, the 'biological heap leaching-solvent extraction-electrodeposition' quickly becomes the preferred process of the low-grade secondary copper sulfide ore by virtue of the advantages of low cost, low energy consumption, simple operation, environmental friendliness and the like. The biological heap leaching is generally that on hillsides, plate lands, slopes and other grounds near mines, impervious materials such as concrete, asphalt and the like are paved, ores are crushed and piled, then bacterial-containing leaching liquid which is prepared in advance and is mostly ferrous oxide thiobacillus and thiobacillus thiooxidans at present is poured or sprayed on the surface of the ores from the top surface of the ore pile by a pump, and air is introduced through an air vent pipeline which is buried in advance at the bottom to create organisms
Necessary condition for leaching. After a period of time, the leaching liquor containing the useful metals accumulates at the bottom of the heap and is collectively fed into a collection tank, and then useful metals are recovered by appropriate methods according to the properties of the different metals. The bacteria-containing leaching solution after metal recovery can be recycled after pH adjustment.
The type of the heap leaching process can be divided according to various characteristics, and the heap leaching process can be divided into a raw ore heap or a waste rock heap according to the geometric shape of a heap leaching field, and is mainly used for heap leaching of low-grade waste rock with higher height; secondly, the On-Off heap leaching field can be disassembled, and the thin-layer heap leaching is mainly used for oxidized ores; thirdly, a permanent single-layer or multi-layer heap leaching field is used for low-grade sulphide ore with medium heap leaching height; a valley type heap leaching field, which is constructed in the valley according to the field topography.
The permanent heap leaching method has low cost and high leaching rate, but can cause that the pyrite in the lower old heap can not be oxidized and the iron and acid concentration in the leaching solution and the raffinate are continuously increased, thereby increasing the environmental protection neutralization cost. Meanwhile, high concentrations of iron and acid may cause microorganisms in the system to be difficult to survive and reproduce, resulting in an increasingly reduced leaching rate and leaching rate. In addition, the concentration of iron in the raffinate is generally 50-70 g/L, the raffinate cannot meet the standard of a biological flocculant, and meanwhile, the raffinate contains more impurities and is narrow in use area.
The method for controlling the concentration of iron and acid in the system in the prior production is to adopt an open circuit part of raffinate to carry out lime neutralization or the raffinate is neutralized by limestone and then returns to a storage yard for spraying. And the amount of slag can be increased continuously along with the time, thereby causing great environmental protection and social pressure. At present, no appropriate solution is provided for the biological iron-calcium slag, so that a new idea can be provided for solving the environmental protection risk by recycling the iron-calcium slag.
Disclosure of Invention
The invention aims to provide a method for synthesizing a bioflocculant, which at least comprises two leaching tanks connected in series, and realizes the resource recycling of a large amount of biological calcium iron slag generated by limestone neutralization raffinate in the process of low-grade copper ore biological heap leaching.
In order to achieve the purpose, the method for synthesizing the biological flocculant comprises the following specific operation steps:
(1) biological heap leaching: the method comprises the steps of crushing and stacking low-grade copper ores, spraying leaching solution containing thiobacillus ferrooxidans on the surface of ores, leaching for a long time, enabling the leaching solution to enter a liquid-rich pool, extracting and electrodepositing, and selling cathode copper as a product. And neutralizing the raffinate with limestone to obtain the biological calcium iron slag. The biological iron-calcium slag contains 50-70% of water, 3-5% of iron and 5-10% of calcium, and the iron-calcium ratio is 1: 3-1: 1.
(2) Pre-separating iron and calcium: adding the biological calcium ferrite slag and the raffinate into a stirrer according to the solid-liquid ratio of 1: 1-1: 3, rotating at the speed of 60-200 r/min, stirring for 60-180 min, and carrying out solid-liquid separation to obtain gypsum slag and iron-rich raffinate. Adding limestone into the iron-rich raffinate for neutralization to obtain the biological iron-rich slag. The biological iron-rich slag contains 50-70% of water, 10-15% of iron and 3-5% of calcium, and the mass ratio of iron to calcium is 2: 1-5: 1.
(3) And leaching pretreatment: drying and crushing the biological iron-rich slag, and then carrying out primary leaching.
(4) And first-stage leaching: the method comprises the steps of firstly filling biological iron-rich slag and dilute sulfuric acid into a primary leaching tank, wherein the mass concentration of the dilute sulfuric acid is 20-50%, the solid-to-liquid ratio is 0.2: 1-2: 1 (kilogram: liter), starting stirring, rotating speed is 60-300 r/min, stirring time is 60-180 min, settling for 5-10 min, carrying out filter pressing, introducing primary leaching liquid into a secondary leaching tank, continuously stirring, and uniformly and safely treating the primary leaching slag.
(5) And secondary leaching: and (3) after the primary leachate is introduced into a secondary leaching tank, supplementing biological iron-rich slag according to the solid-to-liquid ratio of 0.2: 1-2: 1 (kilogram: liter), simultaneously adding concentrated sulfuric acid according to the volume ratio of 5: 1-20: 1 of the primary leachate to concentrated sulfuric acid, stirring at the rotating speed of 60-300 r/min for 60-180 min, settling for 5-10 min, if solid-liquid separation is realized, the iron in the leachate does not reach the target concentration, entering a filter press for filter pressing, and carrying out continuous leaching on the secondary leachate in a manner of countercurrent to the primary leaching tank, wherein dilute sulfuric acid is not supplemented any longer in the countercurrent leaching, and the concentrated sulfuric acid replaces the dilute sulfuric acid. If the colloid is viscous, the subsequent colloid destabilization separation step is carried out.
(6) And (3) colloid destabilization separation: and (3) firstly carrying out ultrasonic treatment on the mixed liquor in the secondary leaching tank, wherein the ultrasonic power is 100W, the working frequency is 20 KHz-40 KHz, and the time is 40-90 minutes, then heating to 60-90 ℃, carrying out solid-liquid separation, carrying out three-stage filter pressing, and carrying out filter pressing to obtain a leaching liquor, namely a biological flocculant semi-finished product.
The synthesis method of the biological flocculant has the following technical characteristics:
1) the method is characterized in that the method utilizes the solubility of iron in concentrated sulfuric acid to carry out countercurrent leaching on iron in the biological iron-calcium slag and concentrate the leached iron to synthesize the biological flocculant, and is still the first time in the field of post-treatment of the biological iron-calcium slag generated in hydrometallurgy biological heap leaching of low-grade copper ores.
2) And the following need to be noted: the main purpose in the iron-calcium pre-separation is to improve the iron-calcium ratio in the slag and greatly reduce the leaching times in the subsequent steps. The acid added in the primary leaching process is dilute sulfuric acid, and the acid added in the secondary leaching and countercurrent leaching processes is concentrated sulfuric acid. Because the concentration of calcium ions and other impurities in the product can be reduced to the maximum extent by adding sulfuric acid, and concentrated sulfuric acid is used for ensuring the acidity in the system, and simultaneously reducing the volume of the leaching solution and improving the leaching efficiency.
3) And the two-stage leaching tanks are connected in series, so that the production rate is greatly improved, the problems of low production speed and low leaching solution concentration of a single leaching tank are solved, and the quality target of the bioflocculant is ensured by countercurrent leaching.
4) And because concentrated sulfuric acid is added in the production process, the temperature is sharply increased in the leaching process, so a leaching tank, a filter press and filter cloth which are high-temperature resistant and acid resistant are selected. The ultrasonic treatment in the colloid destabilization separation step is mainly used for removing the colloid stable state, and the temperature rise is to reduce the liquid viscosity so as to separate the solid from the liquid.
The invention discloses a method for synthesizing a bioflocculant, which provides a method for recycling biological iron and calcium slag generated in low-grade copper ore hydrometallurgy biological heap leaching, and has the following beneficial effects:
1) the iron-calcium ratio in the slag is improved through iron-calcium pre-separation, the leaching frequency in the subsequent steps is greatly reduced, compared with the method of directly adopting a leaching process, the production cost is obviously saved, and the subsequent consumption of sulfuric acid is reduced due to the fact that the content of calcium in the generated biological iron-rich slag is low. The concentrated sulfuric acid used in the secondary leaching and countercurrent process ensures the acidity and leaching concentration in the system and improves the leaching efficiency.
2) Ultrasonic power is 100W in the ultrasonic treatment, and operating frequency is 20KHz ~40KHz, and in this frequency range, the kinetic energy that the colloid particle was provided to the ultrasonic wave can promote the collision between the particle, changes the distance between the colloid particle, destroys the stability of colloid structure, accelerates solid-liquid separation.
3) The invention provides a solution for a large amount of biological iron-calcium slag generated in the biological heap leaching process, solves the problem of biological iron-calcium slag accumulation of the existing enterprises, reduces the environmental protection risk and pressure, synthesizes a biological flocculant, and creates economic benefit for the enterprises.
Drawings
FIG. 1 is a process flow diagram of a method for synthesizing a bioflocculant according to the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with the specific examples, which should not be construed as limiting the present invention.
Example 1
In the embodiment, the raw material is biological iron-calcium slag of a certain mining company in Fujian, the biological iron-calcium slag contains 5.4% of iron, 10.1% of calcium, 64.4% of water content, and the mass ratio of iron to calcium is 1: 1.87, and the leaching process and the leaching effect are as follows:
(1) pre-separating iron and calcium: stirring the biological calcium ferrite slag and the raffinate according to the solid-liquid ratio of 1: 1 (kilogram: liter), rotating speed of 60 r/min, stirring time of 120min, and carrying out solid-liquid separation to obtain gypsum slag and iron-rich raffinate. Adding limestone into the iron-rich raffinate for neutralization to obtain gypsum slag and biological iron-rich slag. The biological iron-rich slag contains 66 percent of water content, 10 percent of iron content and 4.5 percent of calcium content, and the mass ratio of iron to calcium is 2.2: 1.
(2) And leaching pretreatment: drying and crushing the biological iron-rich slag, and then carrying out primary leaching.
(3) And first-stage leaching: and (2) loading biological iron-rich slag and dilute sulfuric acid into the primary leaching tank, wherein the mass concentration of the dilute sulfuric acid is 20%, the solid-liquid ratio is 1: 1.5, the rotating speed is 120r/min, the stirring time is 120min, the mixture is settled for 10min and then is subjected to pressure filtration, the primary leaching solution is introduced into the secondary leaching tank to be continuously stirred, and the primary leaching slag is uniformly and safely treated.
(4) And secondary leaching: and (3) after the primary leaching solution is introduced into a secondary leaching tank, supplementing biological iron-rich slag according to the solid-to-liquid ratio of 1: 2 (kilogram: liter), simultaneously adding concentrated sulfuric acid according to the leaching solution and concentrated sulfuric acid ratio of 7: 1 (volume ratio), rotating at the speed of 120r/min, stirring for 120min, and settling for 10 min.
(5) And colloid destabilization separation: and (3) carrying out ultrasonic treatment on the mixed liquor in the secondary leaching tank, wherein the ultrasonic power is 100W, the working frequency is 20KHz, and the time is 50 minutes, then heating to 80 ℃, carrying out solid-liquid separation, carrying out three-stage filter pressing, and obtaining a leaching liquor after filter pressing, wherein the detected iron concentration reaches 108.5 g/L.
Example 2
In the embodiment, the raw material is biological iron-calcium slag of a mining company in Jiangxi, the biological iron-calcium slag contains 3.7% of iron, 10.8% of calcium, 68.1% of water content, and the mass ratio of iron to calcium is 1: 2.91, and the leaching process and the leaching effect are as follows:
(1) pre-separating iron and calcium: stirring the biological calcium ferrite slag and the raffinate according to the solid-liquid ratio of 1: 1 (kilogram: liter), rotating speed of 80r/min, stirring time of 160min, and carrying out solid-liquid separation to obtain gypsum slag and iron-rich raffinate. Adding limestone into the iron-rich raffinate for neutralization to obtain gypsum slag and biological iron-rich slag. The biological iron-rich slag contains 61% of water, 8.1% of iron and 6.8% of calcium, and the mass ratio of iron to calcium is 1.19: 1.
(2) And leaching pretreatment: drying and crushing the biological iron-rich slag, and then adding the crushed biological iron-rich slag into a leaching tank 1.
(3) And first-stage leaching: and (3) loading biological iron-rich slag and dilute sulfuric acid into the primary leaching tank, wherein the mass concentration of the dilute sulfuric acid is 30%, the solid-liquid ratio is 1: 1.2 (kilogram: liter), the rotating speed is 120r/min, the stirring time is 120min, the mixture is settled for 10min and then is subjected to pressure filtration, the primary leaching solution is introduced into the secondary leaching tank to be continuously stirred, and the primary leaching slag is uniformly and safely treated.
(4) And secondary leaching: and (3) after the primary leaching solution is introduced into a secondary leaching tank, supplementing biological iron-rich slag according to the solid-to-liquid ratio of 1: 1.5 (kilogram: liter), simultaneously adding concentrated sulfuric acid according to the volume ratio of the leaching solution to concentrated sulfuric acid of 8: 1, rotating at the speed of 120r/min, stirring for 120min, settling for 10min, obviously separating solid from liquid, carrying out filter pressing, safely treating the secondary leaching slag and the primary leaching slag, and detecting that the iron concentration of the secondary leaching solution is 70.06 g/L. And (3) the quality target of the biological flocculant is not met, and the secondary leachate is reversely pumped into the primary leaching tank for continuous leaching.
(5) And countercurrent leaching: and after the second-stage leaching solution returns to the first-stage leaching tank, supplementing biological iron-rich slag in the first-stage leaching tank according to the solid-to-liquid ratio of 1: 1 (kilogram: liter), simultaneously adding concentrated sulfuric acid in the leaching solution to concentrated sulfuric acid ratio of 10: 1 (volume ratio), rotating at the speed of 180r/min, stirring for 180min, after settling for 10min, introducing the mixture into a filter press 1, introducing the leaching solution into the second-stage leaching tank, supplementing biological iron-rich slag in the second-stage leaching tank according to the solid-to-liquid ratio of 1: 2 (kilogram: liter), simultaneously adding concentrated sulfuric acid in the leaching solution to concentrated sulfuric acid ratio of 20: 1 (volume ratio), rotating at the speed of 100r/min, and after settling for 5min, introducing into a colloid destabilization separation step.
(6) And colloid destabilization separation: and (3) carrying out ultrasonic treatment on the mixed liquor in the secondary leaching tank, wherein the ultrasonic power is 120W, the working frequency is 35KHz, and the time is 90 minutes, then heating to 90 ℃, carrying out solid-liquid separation, carrying out three-stage filter pressing, and carrying out filter pressing to obtain a leaching liquor, wherein the detected iron concentration reaches 112.1 g/L.
Claims (7)
1. A method for preparing a biological flocculant by utilizing biological iron-calcium slag in biological heap leaching is characterized by comprising the following specific steps:
(1) biological heap leaching: crushing and stacking low-grade copper ores, spraying and leaching solution containing thiobacillus ferrooxidans, allowing the leaching solution to enter a pregnant solution tank, extracting and electrodepositing to obtain copper at a cathode, and neutralizing raffinate with limestone to obtain biological iron-calcium slag;
(2) pre-separation of iron and calcium: stirring and reacting the biological iron-calcium slag and the raffinate, wherein the solid-liquid ratio of the biological iron-calcium slag to the raffinate is 1: 1-1: 3, and the unit of the solid-liquid ratio is kilogram: rising, stirring for 60-180 min, performing solid-liquid separation to obtain gypsum slag and an iron-rich raffinate, adding limestone into the iron-rich raffinate to neutralize to obtain biological iron-rich slag, wherein the water content of the biological iron-rich slag is 50-70%, the iron mass content is 10-15%, the calcium mass content is 3-5%, and the iron-calcium mass ratio is 2: 1-5: 1;
(3) leaching pretreatment: drying and crushing the biological iron-rich slag, and then carrying out primary leaching;
(4) primary leaching: firstly, loading biological iron-rich slag and dilute sulfuric acid into a primary leaching tank, stirring and leaching, carrying out solid-liquid separation, and introducing a primary leaching solution into a secondary leaching tank for continuous stirring; the mass concentration of the dilute sulfuric acid is 20-50%, the solid-liquid ratio of the biological iron-rich slag to the dilute sulfuric acid is 0.2: 1-2: 1, and the unit of the solid-liquid ratio is kilogram: lifting;
(5) secondary leaching: and (2) after the primary leaching solution is introduced into a secondary leaching tank, supplementing biological iron-rich slag and concentrated sulfuric acid, adding concentrated sulfuric acid according to the volume ratio of the primary leaching solution to the concentrated sulfuric acid of 5: 1-20: 1, and supplementing the biological iron-rich slag according to the solid-liquid ratio of 0.2: 1-2: 1, wherein the unit of the solid-liquid ratio is kilogram: lifting; stirring and settling, if solid-liquid separation can be carried out, indicating that the iron in the leaching solution does not reach the target concentration, entering a filter press for filter pressing, carrying out continuous leaching on the secondary leaching solution in a primary leaching tank in a counter-current manner, and replacing dilute sulfuric acid with concentrated sulfuric acid during counter-current leaching; if the colloid is viscous, entering a colloid destabilization separation step;
(6) and (3) colloid destabilization separation: and (3) firstly carrying out ultrasonic treatment on the mixed liquor in the secondary leaching tank, wherein the ultrasonic power in the ultrasonic treatment is 100-120W, the working frequency is 20 KHz-40 KHz, and the time is 40-90 minutes, then heating and settling, carrying out solid-liquid separation, and carrying out filter pressing to obtain a leaching liquor, namely a biological flocculant semi-finished product, wherein the iron concentration in the leaching liquor is more than 100 g/L.
2. The method for preparing the bioflocculant by using the biological iron and calcium slag in the biological heap leaching according to claim 1, wherein the biological iron and calcium slag in the step (1) has a water content of 50-70%, a mass iron content of 3% -5%, a mass calcium content of 5-10%, and an iron and calcium mass ratio of 1: 3-1: 1.
3. The method for preparing the bioflocculant by using the biological iron and calcium slag in the biological heap leaching according to claim 1, wherein the stirring reaction in the step (2) is performed at a rotating speed of 60-200 r/min.
4. The method for preparing the bioflocculant by using the biological iron and calcium slag in the biological heap leaching according to claim 1, wherein the acid added in the first time in the step (4) is dilute sulfuric acid, the mass concentration of the dilute sulfuric acid is 20% -50%, the solid-to-liquid ratio of the biological iron-rich slag to the dilute sulfuric acid is 0.2: 1-1: 1, and the unit of the solid-to-liquid ratio is kilogram: and (5) rising.
5. The method for preparing the bioflocculant by using the biological iron and calcium slag in the biological heap leaching according to claim 1, wherein the biological iron-rich slag and the concentrated sulfuric acid are supplemented after the primary leaching solution in the step (5) is introduced into the secondary leaching tank, the concentrated sulfuric acid is added according to the volume ratio of the primary leaching solution to the concentrated sulfuric acid being 5: 1-10: 1, and the biological iron-rich slag is supplemented according to the solid-liquid ratio being 0.2: 1-1: 1, wherein the unit of the solid-liquid ratio is kilogram: and (5) rising.
6. The method for preparing the bioflocculant by using the biological iron and calcium slag in the biological heap leaching according to claim 1, wherein the rotating speed in the step (5) is 60-300 r/min, and the stirring time is 60-180 min.
7. The method for preparing the bioflocculant by using the biological iron and calcium slag in the biological heap leaching according to claim 1, wherein after the ultrasonic treatment in the step (6), the temperature is firstly raised to 60-90 ℃ so as to reduce the liquid viscosity, and then three-stage pressure filtration is performed.
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| US5873927A (en) * | 1997-05-16 | 1999-02-23 | Echo Bay Mines, Limited | Integrated, tank/heap biooxidation process |
| CN101049978A (en) * | 2007-04-30 | 2007-10-10 | 南开大学 | Method for preparing polymerized iron chloride by using cinder of sulfur iron ore |
| CN101475246A (en) * | 2008-01-04 | 2009-07-08 | 上海爱启生态科技有限公司 | Preparation of efficient polybasic acid iron salt flocculant |
| CN101618929A (en) * | 2008-11-04 | 2010-01-06 | 刘文治 | Method of treating alkaline sludge containing heavy metal as resources |
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