CN115679134A - Method for treating carbon-silicon mudstone type uranium ore - Google Patents
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Abstract
The invention belongs to the technical field of metallurgy, and particularly relates to a method for treating carbon-silicon mudstone type uranium ores. (1) ore preparation: finely crushing carbon-silicon mudstone type uranium ore; (2) oxidizing and roasting: roasting the finely crushed ore in a high-temperature furnace, and ensuring that sufficient air is introduced in the roasting process; (3) alkali mixing and granulating: after the temperature of the roasted material is reduced to 100 ℃, adding an alkali solution, and stirring to bond a plurality of ore particles together to form larger spherical particles; (4) column packing and curing: curing the ore which has residual heat after the alkali mixing granulation; (5) spray leaching: spraying with alkali solution; (6) fractional recovery of leachate: and directly precipitating and recycling uranium for the uranium leaching liquid with high concentration in the former stage, and recycling uranium for the uranium leaching liquid with low concentration in the later stage by adopting an ion exchange method. Uranium is extracted from complex carbo-silicalite type uranium ores through processes of oxidizing roasting, alkali mixing curing and column leaching.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for treating carbon-silicon mudstone type uranium ores.
Background
The carbon silicalite type uranium ore refers to uranium ore which takes marine limestone, dolomite, carbonaceous silicalite, carbonaceous mudstone and the like as ore-bearing main rocks, and uranium mainly exists in an adsorption form. The carbon-silicon mudstone type uranium ores are widely distributed in China and are one of four major types of important uranium deposits in China. Because the composition of the carbo-sillimanite type uranium ore is complex, the carbo-sillimanite type uranium ore is usually rich in carbon (organic matters and carbonates) and sulfides (pyrite and the like) besides silicalite and clay ore, the hydrometallurgy processing difficulty is high, and the production cost is high, so that a mature carbo-sillimanite development technology system is not formed yet.
The technology for extracting uranium from carbon-silicon mudstone type uranium ore is researched earlier in China, wu-Peishen and the like (uranium mining metallurgy, volume 3 of No. 2 in 1987) research the leaching performance of certain carbon-silicon mudstone type uranium ore rich in pyrite and organic matters, the leaching rate of uranium is low when the ore is leached by using a general acid method, the analysis shows that acid-insoluble humic acid is the main reason for the low leaching rate of uranium in the ore, and the reasonable scheme for improving the leaching residual acidity is provided. The nuclear industry Beijing chemical metallurgy research institute also carries out some research works successively aiming at carbon-silicon mudstone uranium ores with different properties, such as a certain carbon-silicon mudstone uranium ore in the Jiangxi province, the lithology of the ore is claystone and carbon slate, a large amount of clay minerals are contained, uranium is adsorbed by the carbon rocks or other substances in a uranyl ion state, a Pachk tank 4 sections are adopted for serial leaching, the residual acidity is 30g/L, the leaching temperature is 70-80 ℃, the leaching time is 4h, the leaching rate of the uranium reaches 88%, but under the high-temperature and high-acid leaching conditions, the dissolution of impurities in the ore is accelerated, and Al in the leaching solution is added 3+ 20-40 g/L, high pulp consistency, difficult solid-liquid separation, and increased uranium loss caused by the difficulty in cleaning uranium adsorbed on the particle surface. The method of roasting by adding salt, roasting by adding salt into the product of roasting by oxidation, soaking and percolating crude ore by multi-stage countercurrent flow improves the leaching rate of uranium to over 70 percent, but the methods have the defects of difficult control of the process, high reagent consumption, complex roasting process by adding salt and Cl - 、F - Corrosion, etc.
In addition, aiming at a certain refractory uranium ore in Mexico in which uranium and organic matters are symbiotic, millikou (nuclear raw material, 1979) proposes that the uranium leaching rate of the refractory ore is improved by an oxidizing roasting method, in a typical process, the ore is dried at 180 ℃ and then ground to-10 meshes, and the leaching rate of uranium can be effectively improved by mainly roasting to remove carbon, changing the properties of clay minerals, reducing the consumption of acid leaching reagents and improving the leaching rate of uranium.
In recent years, domestic researchers have conducted research work on bioleaching of low-grade carbon-silicon mudstone type uranium resources containing organic matters and sulfides, for example, in patent CN105714115B, "a method for leaching uranium by using bacteria in carbon-silicon mudstone type uranium ores", the method proposes that the bacteria leaching is performed by using mineral leaching bacteria subjected to breeding and domestication, and compared with a conventional chemical leaching method, the method can shorten leaching time, improve uranium leaching rate, facilitate effective recovery of the low-grade carbon-silicon mudstone uranium resources, and enlarge uranium resource utilization rate. However, the bacterial leaching process cannot treat ores with high carbonate content, and a special bacterial oxidation tank is required for bacterial culture, so that industrial production is not easy to carry out. Based on the analysis of the existing research, the main difficulties existing in the development of carbon-silicon mudstone type uranium resources are as follows: 1) The organic matter content in the ore is high, and the leaching of uranium is adversely affected; 2) Sulfide and uranium in the ore coexist, and the sulfide needs to be efficiently decomposed; 3) Because of containing clay minerals, the solid-liquid separation of the agitation leached ore pulp is very difficult; 4) Aiming at the carbon-silicon-argillite type uranium ores with high carbonate content, the acid consumption is high when the uranium ores are leached by adopting an acid method, the leaching rate of uranium is low when the uranium ores are leached by adopting a conventional alkali method, and no research report related to efficient treatment of the uranium ores exists at present.
Disclosure of Invention
The invention aims to provide a method for processing carbo-silicalite type uranium ores, which is used for extracting uranium from complex carbo-silicalite type uranium ores through processes of oxidizing roasting, alkali mixing curing and column leaching.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for processing carbon-silicon mudstone type uranium ore,
(1) Preparing ores: finely crushing the carbo-silicalite type uranium ore;
(2) Oxidizing roasting: roasting the finely crushed ore in a high-temperature furnace, and ensuring that sufficient air is introduced in the roasting process;
(3) Alkali mixing and granulation: after the temperature of the roasted material is reduced to 100 ℃, adding an alkali solution, and stirring to bond a plurality of ore particles together to form larger spherical particles;
(4) Column filling and curing: curing the ore which has the residual heat after the alkali mixing and granulation;
(5) Spray leaching: spraying with an alkali solution;
(6) And (3) recycling the leaching solution in parts: directly precipitating and recycling uranium for the uranium leaching solution with high concentration in the former stage, and recycling uranium for the uranium leaching solution with low concentration in the later stage by adopting an ion exchange method;
the alkali is a mixture of sodium carbonate and sodium bicarbonate, and the mass ratio of the sodium carbonate to the sodium bicarbonate is 2.
The granularity of the fine ore in the step (1) is-1 mm to-5 mm.
The roasting temperature in the step (2) is 400-500 ℃.
The roasting time in the step (2) is 1-4 h.
The mass concentration of the alkali solution in the step (3) is 50-400 g/L.
The liquid-solid ratio of the alkali solution in the step (3) is 0.1-0.2L/kg.
The granularity of the spherical particles in the step (3) is-3 mm to-10 mm.
In the step (4), the ore which is mixed with the alkali and granulated and has residual heat is put into a column leaching device for curing, and the curing time is 3-7 days.
The mass concentration of the alkali solution in the step (5) is 0-10 g/L, and the spraying time is 5-30 d.
In the step (5), clear water or a circulating solution is adopted to prepare an alkali solution for spraying.
The beneficial effects obtained by the invention are as follows:
the invention provides a method for extracting uranium from carbon-containing and sulfur-containing carbo-silicalite type uranium ores. The method comprises the steps of firstly carrying out fine crushing treatment on ores, then adopting air oxidation roasting to remove organic matters, decompose sulfides and change the lattice composition of clay minerals, then reinforcing the alkaline leaching process through alkali mixing and curing, finally adopting a column leaching process to directly obtain clear liquid, and adopting direct precipitation and an ion exchange method to carry out fractional recovery on leachate. The method of the invention thoroughly solves the problem of the influence of organic matters and sulfides on uranium leaching, reduces reagent consumption in the alkaline leaching process, is not limited by the carbonate content in the ore, can efficiently process the complex carbo-silicalite type uranium ore, is easy to operate automatically and is easy to realize industrial production.
(1) Organic matters and sulfides in the ores are removed through an oxidizing roasting process, the lattice composition of the clay minerals is destroyed, and the adverse effect of the organic matters, the sulfides and the clay minerals on uranium leaching is effectively solved.
(2) Compared with the stirring leaching process, the process can be carried out under the condition of coarser ore granularity without ore grinding, and clear liquid can be directly obtained through column leaching, so that the problem of difficulty in solid-liquid separation of uranium ore leaching ore pulp of the type is solved.
(3) Compared with the conventional column leaching, the alkali-mixing curing process is adopted, the leaching process is strengthened, the leaching period is shortened, the initial uranium concentration of the leaching solution is high, the leaching solution can be directly precipitated, and the subsequent uranium recovery efficiency is improved.
(4) The fine mud is granulated in the alkali mixing process, so that the permeability of the ore heap is greatly improved, and the influence of clay and argillaceous minerals on the permeability of the ore heap is avoided.
(5) The leaching process does not require heating, and the residual alkali can be recycled.
(6) The process has high treatment efficiency, is not limited by the content of carbonate in the ore, is easy to operate automatically and is easy for industrial production.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The method for treating the carbon-silicon mudstone type uranium ore comprises the following steps:
(1) Preparing ores: and (3) finely crushing the uranium ore of the carbo-silicalite type.
(2) Oxidizing and roasting: roasting the finely crushed ore in a high-temperature furnace at a certain temperature for a certain time, and ensuring that sufficient air is introduced in the roasting process.
(3) Alkali mixing and granulation: after the temperature of the roasted material is reduced to about 100 ℃, adding an alkali solution with a certain liquid-solid ratio, and stirring to bond a plurality of ore particles together to form larger spherical particles.
(4) Column filling and curing: and (3) putting the ore with residual heat after the alkali mixing and granulation into a column leaching device for curing.
(5) Spray leaching: preparing aqueous alkali with a certain concentration by adopting clear water or circulating solution for spraying.
(6) And (3) recycling the leaching solution in parts: and directly precipitating and recycling uranium for the uranium leaching liquid with high concentration in the former stage, and recycling uranium for the uranium leaching liquid with low concentration in the later stage by adopting an ion exchange method.
The specific method for recycling uranium in step (6) may be a technique mature in the art, and is not described herein again.
In the invention, except for special description, the related proportion and percentage are mass ratio, the related alkali is a mixture of sodium carbonate and sodium bicarbonate, and the ratio of the two is 2.
In some embodiments, the mineral fines in step (1) have a particle size of from-1 mm to-5 mm.
In some embodiments, the calcination temperature in step (2) is 400 to 500 ℃, preferably 450 ℃.
In some embodiments, the calcination time in step (2) is from 1 to 4 hours.
In some embodiments, the mass concentration of the alkali solution in the step (3) is 50 to 400g/L.
In some embodiments, the liquid-to-solid ratio of the alkaline solution in step (3) is 0.1 to 0.2L/kg.
In some embodiments, the spherical particles in step (3) have a particle size of from-3 mm to-10 mm.
In some embodiments, the maturation time in step (4) is between 3 and 7 days.
In some embodiments, the mass concentration of the alkali solution in the step (5) is 0 to 10g/L.
In some embodiments, the spraying time in step (5) is from 5 to 30 days.
Example 1
The Guibei carbon-sillimanite type uranium ore consists of three lithologies of sandstone, mudstone and dolomite, and is rich in organic matters (C) Is provided with Content 4.8%) and pyrite (FeS) 2 5.4% of carbonate content, high carbonate Content (CO) 2 16.5 percent of clay, 7.8 percent of uranium grade, and 0.120 percent of uranium grade.
The method for processing the uranium ore comprises the following process steps:
(1) Ore fine crushing: crushing large uranium ores firstly, and then finely crushing the crushed large uranium ores to be-3 mm.
(2) Oxidizing and roasting: 5kg of the ore after the fine crushing in the step (1) is taken and roasted in a customized tubular furnace at 480 ℃ for 3h (wherein the temperature rise time is 0.5 h), and sufficient air is introduced in the roasting process.
(3) Alkali mixing and granulation: and (3) taking out the roasted material in the step (2), cooling to about 100 ℃, adding 300g/L of alkali solution according to the liquid-solid ratio of 0.2L/kg, mixing, uniformly infiltrating the solution and the ore, and granulating.
(4) Column filling and curing: and (3) putting the ore which is mixed with the alkali and granulated and has the residual heat into a column leaching device for curing, wherein the inner diameter of a column is 5cm, the height of the column is 2m, the upper part and the lower part of the column are sealed, and curing is carried out for 5 days at normal temperature.
(5) Spray leaching: after the maturation is finished, the mixture is firstly sprayed with clear water for 5 days, and then sprayed with a leaching agent (with the alkali concentration of about 5 g/L) prepared from tail liquid for 20 days, wherein the spraying is 500mL each day, and the spraying ratio is 2: 1.
(6) And (3) uranium recovery: the average value of the uranium concentration of the leachate before 4d is sprayed is 6.87g/L, the uranium is recovered by direct precipitation after impurity removal, the uranium concentration of the leachate is gradually reduced from the 5 th day, the uranium is recovered by an ion exchange method, and the adsorption tail liquid is returned to prepare the leaching agent.
The final effect is as follows: compared with the conventional alkaline leaching and stirring process, after the process is adopted, the alkaline consumption is reduced to 4.2 percent from 8.5 percent, the consumption of potassium permanganate is reduced to 0 percent from 1 percent, the uranium grade of the tailings is reduced to 0.012 percent from 0.025 percent, and the uranium leaching rate is increased to 90.0 percent from 79.2 percent.
Example 2
Carbon of northwestThe uranium ore is mainly divided into limestone type, silicalite type and slate type, and is rich in organic matter (C) Is provided with Content 5.7%) and pyrite (FeS) 2 3.4 percent of carbonate content and higher (CO) 2 Content 7.5%), but belongs to low-grade uranium ore (uranium grade 0.078%).
The method for processing the uranium ore comprises the following process steps:
(1) Ore fine crushing: the uranium ore is finely crushed to-5 mm.
(2) Oxidizing and roasting: 4kg of the ore after the fine crushing in the step (1) is taken and roasted in a customized tubular furnace at 450 ℃ for 2h (wherein the temperature rise time is 0.5 h), and sufficient air is ensured to be introduced in the roasting process.
(3) Alkali mixing and granulation: and (3) taking out the roasted material in the step (2), cooling to about 100 ℃, adding 200g/L of alkali solution according to the liquid-solid ratio of 0.15L/kg, mixing, uniformly infiltrating the solution and the ore, and granulating.
(4) Column filling and curing: and (3) putting the ore which is mixed with the alkali and granulated and has the residual heat into a column leaching device for curing, wherein the inner diameter of a column is 5cm, the height of the column is 2m, the upper part and the lower part of the column are sealed, and curing is carried out for 3d at normal temperature.
(5) Spray leaching: after the maturation is finished, the mixture is firstly sprayed with clear water for 5 days, and then sprayed with a leaching agent (with the alkali concentration of about 5 g/L) prepared from tail liquid for 25 days, wherein the spraying is 400mL each day, and the spraying ratio is 2: 1.
(6) And (3) uranium recovery: the average value of the uranium concentration of the leachate 3d before spraying is 5.75g/L, the uranium is recovered by direct precipitation after impurity removal, the uranium concentration of the leachate is gradually reduced from the 4d, the uranium is recovered by an ion exchange method, and the adsorption tail liquid is returned to prepare the leaching agent.
The final effect is as follows: compared with the conventional alkaline leaching stirring process, after the process disclosed by the invention is adopted, the alkaline consumption is reduced to 3.2% from 6.5%, the potassium permanganate using amount is reduced to 0 from 0.8%, the uranium grade of the tailings is reduced to 0.010% from 0.022%, and the uranium leaching rate is increased to 87.2% from 71.8%.
Example 3
Some carbon sillimanite type uranium ore in Hunan province, the ore-containing surrounding rock is mainly silicalite, and the carbonate content in the ore is low (CO) 2 Content 0.5%), richContaining organic substances (C) Is provided with Content 4.9%) and pyrite (content 4.8%), most of the uranium being present in the carbonaceous slime of the ore in an adsorbed state or in close symbiotic relationship with pyrite, the uranium grade being 0.107%, when the uranium ore is leached by the acid method, high spent acid leaching is required (spent acid is greater than 50 g/L), and the leachate has a high concentration of impurity ions.
The method for processing the uranium ore comprises the following process steps:
(1) Ore fine crushing: the uranium ore is finely crushed to-3 mm.
(2) Oxidizing roasting: 5kg of the ore after the fine crushing in the step (1) is roasted in a customized tubular furnace at 500 ℃ for 2.5h (wherein the temperature rise time is 0.5 h), and sufficient air is introduced in the roasting process.
(3) Alkali mixing and granulation: and (3) taking out the roasted material in the step (2), cooling to about 100 ℃, adding 200g/L of alkali solution according to the liquid-solid ratio of 0.12L/kg, mixing, uniformly infiltrating the solution and the ore, and granulating.
(4) Column filling and curing: and (3) putting the ore which is mixed with the alkali and granulated and has the residual heat into a column leaching device for curing, wherein the inner diameter of a column is 5cm, the height of the column is 2m, the upper part and the lower part of the column are sealed, and curing is carried out for 7 days at normal temperature.
(5) Spray leaching: after the maturation is finished, the mixture is firstly sprayed with clear water for 5 days, and then sprayed with a leaching agent (with the alkali concentration of about 5 g/L) prepared from tail liquid for 25 days, wherein the spraying is 500mL every day, and the spraying ratio is 2: 1.
(6) And (3) uranium recovery: the average value of the uranium concentration of the leachate 3d before spraying is 7.75g/L, the uranium is recovered by direct precipitation after impurity removal, the uranium concentration of the leachate is gradually reduced from the 4d, the uranium is recovered by an ion exchange method, and the adsorption tail liquid is returned to prepare the leaching agent.
The final effect is as follows: compared with the conventional acid leaching and stirring process, the process can avoid leaching high residual acid, and the tailings have the uranium grade of 0.013% and the uranium leaching rate of 87.9%.
Claims (10)
1. A method for processing a carbon-silicon mudstone type uranium ore is characterized in that:
(1) Preparing ore: finely crushing carbon-silicon mudstone type uranium ore;
(2) Oxidizing and roasting: roasting the finely crushed ore in a high-temperature furnace, and ensuring that sufficient air is introduced in the roasting process;
(3) Alkali mixing and granulation: after the temperature of the roasted material is reduced to 100 ℃, adding an alkali solution, and stirring to enable a plurality of ore particles to be bonded together to form larger spherical particles;
(4) Column filling and curing: curing the ore which has residual heat after the alkali mixing granulation;
(5) Spray leaching: spraying with an alkali solution;
(6) And (3) recycling the leaching solution in parts: directly precipitating and recycling uranium for the uranium leaching solution with high concentration in the former stage, and recycling uranium for the uranium leaching solution with low concentration in the later stage by adopting an ion exchange method;
the alkali is a mixture of sodium carbonate and sodium bicarbonate, and the mass ratio of the sodium carbonate to the sodium bicarbonate is 2.
2. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, characterized in that: the granularity of the fine ore in the step (1) is-1 mm to-5 mm.
3. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, wherein: the roasting temperature in the step (2) is 400-500 ℃.
4. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, characterized in that: the roasting time in the step (2) is 1-4 h.
5. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, characterized in that: the mass concentration of the alkali solution in the step (3) is 50-400 g/L.
6. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, characterized in that: the liquid-solid ratio of the alkali solution in the step (3) is 0.1-0.2L/kg.
7. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, characterized in that: the granularity of the spherical particles in the step (3) is-3 mm to-10 mm.
8. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, wherein: in the step (4), the ore which is mixed with the alkali and granulated and has residual heat is put into a column leaching device for curing, and the curing time is 3-7 days.
9. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, characterized in that: in the step (5), the mass concentration of the alkali solution is 0-10 g/L, and the spraying time is 5-30 d.
10. The process for the treatment of uranium ores of the carbo-silico type according to claim 1, wherein: in the step (5), clear water or a circulating solution is adopted to prepare an alkali solution for spraying.
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