Clean production process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore

文档序号:502901 发布日期:2021-05-28 浏览:33次 中文

阅读说明:本技术 一种从离子吸附型钼铼矿中回收钼铼的清洁生产工艺 (Clean production process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore ) 是由 张博 李占元 杨光 柳林 于 2021-01-04 设计创作,主要内容包括:本发明涉及一种从离子吸附型钼铼矿中回收钼铼的清洁生产工艺,包括以下步骤:将离子吸附型钼铼矿破碎后加入反应釜中,采用浸取剂溶液对离子吸附型钼铼矿进行第一次浸出,然后再采用浸取剂和助浸剂的混合溶液对离子吸附型钼铼矿进行第二次浸出,最后将两次得到的浸出液混合后回收其中的钼和铼。本发明第一次浸出采用浸取剂溶液使矿石中易于回收的钼离子和铼离子浸出进入溶液,第二次浸出使用浸取剂和助浸剂的混合溶液使矿石中难以回收的钼离子和铼离子浸出进入溶液,从而提高了钼和铼的浸出率,同时减少了浸取剂和助浸剂的用量。该方法具有成本低、环保性好、工艺简单的特点。该工艺中铼回收率大于70%,钼回收率大于80%。(The invention relates to a clean production process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore, which comprises the following steps: crushing the ion adsorption type molybdenum-rhenium ore, adding the crushed ion adsorption type molybdenum-rhenium ore into a reaction kettle, carrying out primary leaching on the ion adsorption type molybdenum-rhenium ore by adopting a leaching agent solution, then carrying out secondary leaching on the ion adsorption type molybdenum-rhenium ore by adopting a mixed solution of a leaching agent and a leaching assistant agent, and finally mixing leaching solutions obtained in the two times and recovering molybdenum and rhenium. According to the invention, the leaching agent solution is adopted in the first leaching to leach the molybdenum ions and the rhenium ions which are easy to recover in the ore into the solution, and the mixed solution of the leaching agent and the leaching aid is adopted in the second leaching to leach the molybdenum ions and the rhenium ions which are difficult to recover in the ore into the solution, so that the leaching rate of molybdenum and rhenium is improved, and the dosage of the leaching agent and the leaching aid is reduced. The method has the characteristics of low cost, good environmental protection and simple process. The recovery rate of rhenium and molybdenum in the process is more than 70% and 80%.)

1. A clean production process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore is characterized by comprising the following steps:

(1) crushing the ion adsorption type molybdenum-rhenium ore to a particle size range of 0.045-0.25 mm;

(2) adding the ion adsorption type molybdenum-rhenium ore crushed in the step (1) into a reaction kettle with 2-4 baffle plates, then adding a leaching agent solution for primary leaching, carrying out solid-liquid separation, and collecting to obtain a primary leaching solution;

(3) and (3) performing secondary leaching on the ion adsorption type molybdenum-rhenium ore treated in the step (2) by adopting a mixed solution of a leaching agent and an auxiliary leaching agent, performing solid-liquid separation, collecting to obtain a secondary leaching solution, combining the primary leaching solution and the secondary leaching solution, and recovering molybdenum and rhenium.

2. The process according to claim 1, wherein in the step (2), the leaching agent is at least one of sodium hydroxide and potassium hydroxide, and the concentration of the leaching agent in the leaching agent solution is 2-6 mol/L.

3. The process according to claim 1, wherein in the step (2), the liquid-solid ratio of the leaching agent solution to the crushed ion adsorption type molybdenum-rhenium ore is 2-12L: 1 kg.

4. The process as claimed in claim 1, wherein in the step (2), the leaching temperature is 30-80 ℃ and the leaching time is 0.5-3 h.

5. The process of claim 1, wherein in step (3), the leaching agent is at least one of sodium hydroxide and potassium hydroxide; the leaching aid is an oxidant capable of oxidizing low-valence molybdenum and rhenium into high-valence molybdenum and rhenium, and a reagent with stronger ion adsorption type molybdenum ion and rhenium ion replacement capability.

6. The process of claim 5, wherein the oxidizing agent is at least one of hydrogen peroxide, sodium peroxide, and potassium permanganate, and the more metathesis-competent agent is at least one of ammonium chloride, sodium chloride, and ammonium sulfate.

7. The process according to claim 1, wherein in the step (3), the concentration of the leaching agent in the mixed solution is 2-6 mol/L, and the concentration of the leaching aid in the mixed solution is 0.1-0.5 mol/L.

8. The process according to claim 1, wherein in the step (3), the liquid-solid ratio of the mixed solution to the ion adsorption type molybdenum-rhenium ore treated in the step (2) is 1-6L: 1 kg.

9. The process of claim 1, wherein in the step (3), the leaching temperature is 30-80 ℃ and the leaching time is 0.5-3 h.

10. The process as claimed in claims 1 to 9, wherein in steps (2) and (3), the first leaching and the second leaching are stirred by axial flow paddles at a rotating speed of 30-150 rpm.

Technical Field

The invention relates to a clean production process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore, belonging to the field of comprehensive utilization of mineral resources.

Background

Molybdenum and rhenium are important strategic resources, and the molybdenum has the characteristics of high melting point, high strength, corrosion resistance and the like, so that the molybdenum is widely applied to the fields of steel industry, nonferrous metallurgy, petrochemical industry and the like, wherein the molybdenum consumed by the steel industry accounts for about 70-80% of the total consumption of the molybdenum, and is used for manufacturing various structural alloy steels, stainless steels, tool steels and high-speed steels; rhenium has excellent creep resistance and catalytic performance and is widely applied to the fields of aerospace, petrochemical industry and the like, wherein about 80 percent of rhenium is used for manufacturing single crystal blades of an aircraft engine, and about 20 percent of rhenium is used for producing petroleum hydrogenation catalysts.

The content of molybdenum in nature is very low, and the abundance of molybdenum in the earth crust is 1.1 multiplied by 10-6More than 20 molybdenum ores are known, wherein the most abundant and industrially valuable ore is molybdenite, which accounts for about 98% of the molybdenum production at home and abroad; rhenium has no independent mineral in nature, and the abundance of rhenium in the crust is only 0.7X 10-9Predominantly present in the form of isomorphs in the porphyry molybdenite, which is usually recovered as a by-product in the molybdenum concentrate smelting process. Molybdenum grade in molybdenum-rhenium ore found in Wuliqiong plateau in Guizhou is 0.1% -0.4%, rhenium grade is 20-40 g/t, and the molybdenum-rhenium ore reaches industrial grade, but after the ore is subjected to detailed mineral structure research, the ore is found to have no obvious molybdenum-containing mineral, the main phase structure of the mineral is quartz and clay mineral, and the distribution of rhenium and molybdenum has positive correlation with the clay mineral. Finally, the molybdenum-rhenium ore of Wulicheng plateau in Guizhou is proved that a small amount of rhenium is enriched from seawater in the deposition process of mudstone, the geological action occurs in the later period, the molybdenite existing on the periphery is melted by hydrothermal solution and decomposed into molybdenum and rhenium ions which are absorbed and enriched by clay minerals in the mudstone, and the novel ion-absorption type molybdenum-rhenium ore is formed.

The molybdenum yield and consumption of China are at the top of the world, but with the continuous development of molybdenum ore resources, high-quality resources are increasingly deficient, and the molybdenum ore resources which are poor, fine, miscellaneous and the like and are difficult to utilize become main raw materials for extracting molybdenum. Therefore, an economically feasible development method for the novel ion adsorption type molybdenum-rhenium ore is found, and the method has important significance for guaranteeing supply of strategic metal resources in China.

Molybdenum and rhenium are extracted from rhenium-containing molybdenum concentrate, molybdenum sulfide and rhenium sulfide in minerals are oxidized into high-valence molybdenum oxide and rhenium oxide, and then the high-valence molybdenum oxide and rhenium oxide are prepared into ammonium molybdate and ammonium rhenate through leaching, impurity removal, extraction and other processes, and the rhenium-containing molybdenum concentrate is mainly oxidized by an oxidizing roasting method and a pressure oxidation method, wherein the main advantages and disadvantages are shown in table 1.

Table 1 main oxidation process of rhenium-containing molybdenum concentrate

The oxidation roasting method oxidizes molybdenum sulfide in molybdenum concentrate into molybdenum oxide calcine through oxidation roasting, the used oxidant is usually air or oxygen-enriched air, the oxidation roasting method has the characteristics of low cost, high production efficiency and the like, and the oxidation roasting method is a main molybdenum concentrate oxidation process in the world at present, and more than 80% of molybdenum oxide calcine is produced by the oxidation roasting process. The equipment used in the oxidation roasting method mainly comprises a multi-hearth furnace and a rotary kiln, the roasting temperature is generally controlled at 500-650 ℃, but molybdenum and rhenium in the ion adsorption type rare earth ore mainly exist in clay minerals in an ion adsorption mode, and Re2O7Sublimation at 273 ℃ MoO3Obviously sublime at 650 ℃, if the process is adopted to treat the ion adsorption type molybdenum-rhenium ore, the recovery rate of molybdenum and rhenium cannot be ensured, a spraying device is required to be arranged at the rear end to recover the volatilized molybdenum and rhenium, and the process is complex; on the other hand, the oxidizing-roasting method mainly provides heat through the oxidation reaction of sulfur in molybdenite, but the ion-adsorption-type molybdenum-rhenium ore has a very low sulfur content, and it is difficult to generate sufficient heat to maintain the oxidation reaction, and it is necessary to supplement the heat by an external heat source, which is costly, and therefore, the oxidizing-roasting method is not suitable for treating the ion-adsorption-type molybdenum-rhenium ore.

The pressure oxidation method is mainly characterized in that under the conditions of high temperature and high pressure, molybdenum sulfide and rhenium sulfide are oxidized into molybdenum oxide and rhenium oxide by using a proper oxidant in a solution, then impurities are removed, extraction and precipitation are carried out for recovery, the temperature is usually controlled to be 200-300 ℃ in the production process, and the pressure is usually controlled to be 1-5 MPa. For the ion adsorption type molybdenum-rhenium ore, molybdenum and rhenium exist in an ion adsorption form, and the pressure oxidation method can ensure higher recovery rates of molybdenum and rhenium, but the process is carried out under the conditions of high temperature and high pressure, has higher requirements on the safety of production, simultaneously, the used reagent has stronger corrosivity, needs to be produced in special high-temperature-resistant, high-pressure-resistant and corrosion-resistant equipment, and has higher production cost, so the pressure oxidation method is not suitable for treating the ion adsorption type molybdenum-rhenium ore.

In conclusion, as a novel molybdenum-rhenium ore, a treatment method with reasonable technical economy is not available at present. Therefore, the development of a high-efficiency clean recovery process of molybdenum and rhenium for the ion adsorption type molybdenum-rhenium ore is urgent.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a clean production process for recovering molybdenum and rhenium from the ion adsorption type molybdenum-rhenium ore, so as to realize the comprehensive recovery of molybdenum and rhenium in the ion adsorption type molybdenum-rhenium ore.

In order to achieve the purpose, the invention adopts the technical scheme that: a clean production process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) crushing the ion adsorption type molybdenum-rhenium ore to a particle size range of 0.045-0.25 mm;

(2) adding the ion adsorption type molybdenum-rhenium ore crushed in the step (1) into a reaction kettle with 2-4 baffle plates, then adding a leaching agent solution for primary leaching, carrying out solid-liquid separation, and collecting to obtain a primary leaching solution;

(3) and (3) performing secondary leaching on the ion adsorption type molybdenum-rhenium ore treated in the step (2) by adopting a mixed solution of a leaching agent and an auxiliary leaching agent, performing solid-liquid separation, collecting to obtain a secondary leaching solution, combining the primary leaching solution and the secondary leaching solution, and recovering molybdenum and rhenium.

The technical scheme of the invention is that by utilizing the characteristic that molybdenum and rhenium are adsorbed on clay minerals, after the ion adsorption type molybdenum-rhenium ore is crushed and ground, leaching agent solution is adopted to leach the ion adsorption type molybdenum-rhenium ore for the first time, so that molybdenum ions and rhenium ions which are easy to recover in the ore are leached into the solution; and then, leaching the ore for the second time by adopting a mixed solution of a leaching agent and a leaching aid, so that molybdenum ions and rhenium ions which are difficult to recover in the ore are leached into the solution. The leaching aid comprises high-valence molybdenum ions and rhenium ions which are easy to dissolve in solution and are oxidized from low-valence molybdenum ions and rhenium ions in ores, and a reagent with stronger replacement capacity for ion adsorption type molybdenum ions and rhenium ions, so that the leaching efficiency is improved; on the other hand, the consumption of impurity ions to the leaching aid in the first leaching process is avoided through two leaching operations, and the recovery rate of molybdenum and rhenium is improved. Compared with the conventional molybdenum ore treatment process, the method does not need a fire roasting treatment process and high-temperature-resistant, high-pressure-resistant and corrosion-resistant high-pressure leaching equipment, greatly shortens the process flow and saves the cost.

In a preferable embodiment of the process of the invention, in the step (2), the leaching agent is at least one of sodium hydroxide and potassium hydroxide, and the concentration of the leaching agent in the leaching agent solution is 2-6 mol/L.

In the step (2), the liquid-solid ratio of the leaching agent solution to the crushed ion adsorption type molybdenum-rhenium ore is 2-12L: 1 kg.

As a preferred embodiment of the process, in the step (2), the leaching temperature is 30-80 ℃, and the leaching time is 0.5-3 h.

In a preferred embodiment of the process of the present invention, in the step (3), the leaching agent is at least one of sodium hydroxide and potassium hydroxide; the leaching aid is an oxidant capable of oxidizing low-valence molybdenum and rhenium into high-valence molybdenum and rhenium, and a reagent with stronger ion adsorption type molybdenum ion and rhenium ion replacement capability.

Preferably, the oxidizing agent is at least one of hydrogen peroxide, sodium peroxide and potassium permanganate, and the agent with stronger replacement ability is at least one of ammonium chloride, sodium chloride and ammonium sulfate.

In the preferable embodiment of the process of the invention, in the step (3), the concentration of the leaching agent in the mixed solution is 2-6 mol/L, and the concentration of the leaching aid in the mixed solution is 0.1-0.5 mol/L.

In a preferred embodiment of the process of the present invention, in the step (3), the liquid-solid ratio of the mixed solution to the ion adsorption type molybdenum-rhenium ore treated in the step (2) is 1-6L: 1 kg.

As a preferred embodiment of the process, in the step (3), the leaching temperature is 30-80 ℃, and the leaching time is 0.5-3 h.

In the steps (2) and (3), the first leaching and the second leaching are stirred by an axial flow propeller at the rotating speed of 30-150 rpm.

Compared with the prior art, the invention has the beneficial effects that:

(1) the method has the advantages of low cost, capability of recovering molybdenum and rhenium in ores by adopting an in-situ leaching mode near a stope, saving long-distance transportation cost, no need of large-scale equipment, low capital construction cost and production cost, and suitability for large-scale industrial application.

(2) The process is simple, the recovery of molybdenum and rhenium in the ion adsorption type molybdenum-rhenium ore can be realized by crushing and leaching the ore, and the process is simple and easy to control.

(3) The method has the advantages that the method is good in environmental protection, all the used reagents are conventional reagents, the recovery rate of molybdenum and rhenium is improved by leaching twice, the consumption of leaching agents and leaching aids is reduced, and the method is environment-friendly.

(4) The invention has the advantages that the recycling efficiency is high, the clay mineral and the alkaline solution react to easily generate viscous slurry solution, the baffle plate is arranged in the reaction kettle, the axial flow paddle is adopted for stirring, the clay mineral can be fully dispersed in the alkaline solution, excessive argillization is avoided, the leaching efficiency of molybdenum and rhenium is improved, and meanwhile, the lower rotating speed is beneficial to energy conservation and consumption reduction.

Detailed Description

To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.

Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.

Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products obtained by a known method.

The used raw material is ion adsorption type molybdenum-rhenium ore produced in certain places in Guizhou, wherein the molybdenum content is 980g/t, and the rhenium content is 28 g/t.

Example 1

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.12mm, and adding 2kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 3 baffle plates, simultaneously adding 1.5kg of sodium hydroxide, heating to 60 ℃ for primary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 2.09mg/L and the molybdenum concentration of 92.91 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 6L of tap water, 900g of sodium hydroxide, 80g of hydrogen peroxide and 240g of ammonium sulfate, heating to 60 ℃, starting secondary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining secondary leaching liquid with the rhenium concentration of 3.49mg/L and the molybdenum concentration of 121.67 mg/L. The recovery of rhenium amounted to 74.83% and the recovery of molybdenum amounted to 84.65% during leaching.

Example 2

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.12mm, and adding 2kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 3 baffle plates, simultaneously adding 1.5kg of potassium hydroxide, heating to 60 ℃ for primary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 2.06mg/L and the molybdenum concentration of 86.34 mg/L;

(3) and (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 6L of tap water, 900g of potassium hydroxide, 240g of potassium permanganate and 100g of sodium chloride, heating to 60 ℃, starting secondary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining secondary leaching liquid with the rhenium concentration of 3.30mg/L and the molybdenum concentration of 122.59 mg/L. The recovery of rhenium amounted to 72.06% and the recovery of molybdenum amounted to 81.58% during leaching.

Example 3

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.12mm, and adding 2kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 3 baffle plates, simultaneously adding 1.5kg of sodium hydroxide, heating to 60 ℃ for primary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 2.18mg/L and the molybdenum concentration of 97.41 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 6L of tap water, 900g of sodium hydroxide, 100g of hydrogen peroxide and 360g of ammonium sulfate, heating to 60 ℃, starting secondary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining secondary leaching liquid with the rhenium concentration of 3.76mg/L and the molybdenum concentration of 122.47 mg/L. The recovery of rhenium amounted to 79.31% and the recovery of molybdenum amounted to 87.19% during leaching.

Example 4

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.12mm, and adding 2kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 15L of tap water into a reaction kettle with 3 baffle plates, simultaneously adding 1.5kg of sodium hydroxide, heating to 60 ℃ for primary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 1.39mg/L and the molybdenum concentration of 55.29 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 10L of tap water, 900g of sodium hydroxide, 80g of hydrogen peroxide and 240g of ammonium sulfate, heating to 60 ℃, starting secondary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining secondary leaching liquid with the rhenium concentration of 2.08mg/L and the molybdenum concentration of 82.93 mg/L. The recovery of rhenium amounted to 77.56% and the recovery of molybdenum amounted to 86.35% during leaching.

Example 5

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.12mm, and adding 2kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 3 baffle plates, simultaneously adding 1.5kg of sodium hydroxide, heating to 80 ℃ for primary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 2.03mg/L and the molybdenum concentration of 90.88 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 6L of tap water, 900g of sodium hydroxide, 80g of hydrogen peroxide and 240g of ammonium sulfate, heating to 80 ℃, starting secondary leaching, wherein the leaching time is 2h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining secondary leaching liquid with the rhenium concentration of 3.81mg/L and the molybdenum concentration of 129.03 mg/L. The recovery of rhenium amounted to 77.03% and the recovery of molybdenum amounted to 85.87% during leaching.

Example 6

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.12mm, and adding 2kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 3 baffle plates, simultaneously adding 1.5kg of sodium hydroxide, heating to 60 ℃ for primary leaching, wherein the leaching time is 3h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 1.98mg/L and the molybdenum concentration of 85.86 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 6L of tap water, 900g of sodium hydroxide, 80g of hydrogen peroxide and 240g of ammonium sulfate, heating to 60 ℃, starting secondary leaching, wherein the leaching time is 3h, the rotating speed of an axial flow paddle is 80rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining secondary leaching liquid with the rhenium concentration of 3.72mg/L and the molybdenum concentration of 132.09 mg/L. The recovery of rhenium amounted to 75.19% and the recovery of molybdenum amounted to 84.24% during leaching.

Example 7

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.045mm, and adding 5kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 2 baffle plates, simultaneously adding 800g of sodium hydroxide, heating to 30 ℃ for primary leaching, wherein the leaching time is 3h, the rotating speed of an axial flow paddle is 150rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 4.43mg/L and the molybdenum concentration of 196.59 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 6L of tap water, 480g of sodium hydroxide, 21g of hydrogen peroxide and 80g of ammonium sulfate, heating to 30 ℃, starting secondary leaching, wherein the leaching time is 3h, the rotating speed of an axial flow paddle is 150rpm, and after the reaction is finished, carrying out vacuum filtration for solid-liquid separation to obtain secondary leaching liquid with the rhenium concentration of 9.05mg/L and the molybdenum concentration of 327.65 mg/L. The recovery of rhenium amounted to 70.52% and the recovery of molybdenum amounted to 80.24% during leaching.

Example 8

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding the ion adsorption type molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.25mm, and adding 0.83kg of the ion adsorption type molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle with 4 baffle plates, simultaneously adding 2.4kg of sodium hydroxide, heating to 80 ℃ for primary leaching, wherein the leaching time is 0.5h, the rotating speed of an axial flow paddle is 30rpm, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, and obtaining primary leaching liquid with the rhenium concentration of 0.96mg/L and the molybdenum concentration of 37.88 mg/L.

(3) And (3) continuously adding the ion adsorption type molybdenum-rhenium ore treated in the step (2) into a reaction kettle, simultaneously adding 5L of tap water, 1.2Kg of sodium hydroxide, 102g of hydrogen peroxide and 400g of ammonium sulfate, heating to 80 ℃ to start secondary leaching, wherein the leaching time is 0.5h, the rotating speed of an axial flow paddle is 30rpm, and after the reaction is finished, carrying out vacuum filtration for solid-liquid separation to obtain secondary leaching liquid with the rhenium concentration of 2.07mg/L and the molybdenum concentration of 72.79 mg/L. The recovery of rhenium amounted to 85.67% and the recovery of molybdenum amounted to 91.32% during leaching.

Comparative example 1

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding the molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.075mm, and adding 2kg of the molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle, simultaneously adding 1.5kg of sodium hydroxide, heating to 60 ℃ to start leaching, wherein the leaching time is 2h, after the reaction is finished, carrying out vacuum filtration for solid-liquid separation, wherein the rhenium concentration in the obtained leaching solution is 2.54mg/L, the rhenium recovery rate in the leaching process is 45.36%, the molybdenum concentration in the leaching solution is 100.61mg/L, the molybdenum recovery rate in the leaching process is 51.33%, and the rhenium and molybdenum recovery rates are lower in the leaching process without adding an auxiliary leaching agent.

Comparative example 2

A process for recovering molybdenum and rhenium from ion adsorption type molybdenum-rhenium ore comprises the following steps:

(1) grinding the molybdenum-rhenium ore in a vibration mill until the granularity is less than 0.075mm, and adding 2kg of the molybdenum-rhenium ore into a reaction kettle;

(2) adding 10L of tap water into a reaction kettle, simultaneously adding 1.5kg of sodium hydroxide, 100g of hydrogen peroxide and 400g of ammonium sulfate, heating to 60 ℃ to start leaching, wherein the leaching time is 2h, and after the reaction is finished, carrying out vacuum filtration to carry out solid-liquid separation to obtain primary leachate, wherein the rhenium concentration is 2.73mg/L and the molybdenum concentration is 112.84 mg/L.

(3) And (3) continuously adding the filter residue into a reaction kettle, simultaneously adding 6L of tap water, 900g of sodium hydroxide, 80g of hydrogen peroxide and 240g of ammonium sulfate, heating to 60 ℃ to start leaching, wherein the leaching time is 2h, and after the reaction is finished, carrying out vacuum filtration to carry out solid-liquid separation to obtain secondary leachate, wherein the rhenium concentration is 3.16mg/L, and the molybdenum concentration is 101.27 mg/L. The recovery rate of rhenium is 82.51% in total, the recovery rate of molybdenum is 88.57% in total, a mixed solution of a leaching agent and a leaching aid is adopted for the two leaching processes of the molybdenum-rhenium ore, and although the recovery rates of molybdenum and rhenium can be improved, the consumption of the reagent is large.

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

9页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:钨冶炼协同除硅的方法

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!