CN109516502B - Method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cake - Google Patents
Method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cake Download PDFInfo
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- CN109516502B CN109516502B CN201710843182.2A CN201710843182A CN109516502B CN 109516502 B CN109516502 B CN 109516502B CN 201710843182 A CN201710843182 A CN 201710843182A CN 109516502 B CN109516502 B CN 109516502B
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- C01G47/00—Compounds of rhenium
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Abstract
The invention discloses a method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes, and belongs to the technical field of rare metal smelting, high-risk solid waste treatment and resource comprehensive recycling. The method comprises four steps of copper-rhenium enrichment, copper-rhenium separation, rhenate solution preparation and rhenate crystallization. The method provided by the invention avoids the defects of acidification leaching in the prior art, utilizes the advantages of the treatment capacity of the traditional roasting process, and simultaneously overcomes the disadvantage of adverse effect on the environment in the traditional process, and the obtained ammonium rhenate has the advantages of extremely high purity, good recovery effect, simplicity and high efficiency in operation, environmental friendliness and low maintenance cost, and has great practical significance for the treatment of solid wastes and the recovery of scarce resources.
Description
Technical Field
The invention belongs to the field of rare metal metallurgy and the field of solid hazardous waste recycling, and particularly relates to a method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes.
Background
Rhenium is a metal element, one of the high melting point metals, with a melting point lower than 3410 degrees celsius of the metal tungsten, and can be used to make electrical filaments, shells for satellites and rockets, shields for nuclear reactors, etc., and is used chemically as a catalyst. Rhenium is a truly rare element. It is less than all the rare earth elements in the crusta, and is only greater than the protactinium and radium elements. In addition, it does not form a fixed mineral, usually associated with other metals.
The rhenium and its alloy can be used to make pen point of running water and high-temp. thermocouple, and as catalyst in dehydrogenation of alcohols, synthesis of ammonia and preparation of sulfur trioxide from sulfur dioxide. The alloy containing 90% of tungsten, 1% of vanadium and 9% of rhenium can resist high temperature. Rhenium is dispersed and expensive. Rhenium is widely used in various departments of modern industry, mainly used as a catalyst in the petroleum industry and the automobile industry, a petroleum reforming catalyst, rhenium alloy for the electronic industry and the aerospace industry and the like. RheniumThe strength and plasticity of tungsten, molybdenum and chromium can be improved simultaneously, and the phenomenon is called 'rhenium effect'. The tungsten-rhenium and molybdenum-rhenium alloy has good high-temperature strength and plasticity, can be processed into plates, sheets, wires and rods, is used for high-temperature structural members, elastic elements, electronic elements and the like of aerospace, and can also be used for manufacturing heating elements, workpieces, bulbs, X-ray instruments and medical instruments. W-Re-ThO2The alloy can be used as a high-temperature heating workpiece, and the tungsten-rhenium and molybdenum-rhenium alloy contact has high thermal corrosion resistance and high-temperature conductivity, and can improve the service life and the working reliability of power supply equipment. Such as: platinum-rhenium alloys, platinum-tungsten-rhenium alloys, molybdenum-rhenium alloys, and the like.
So far, copper arsenic filter cakes are an important raw material source for extracting metal rhenium, wherein the preparation of high-purity ammonium rhenate is an integral link for preparing the metal rhenium. Few reports of large-scale industrialization of smoke dust desulfurization and dearsenification by microwave heating methods are available. Due to this, the microwave heating characteristics are not well understood and the application of microwave high-temperature heating equipment is not extensive.
The existing main method for preparing ammonium rhenate is to recover ammonium rhenate by an acid system high-pressure leaching process, and the method has the advantages of long process flow, low recovery efficiency, high production cost and high equipment requirement. A method for preparing ammonium rhenate from rhenium-rich slag as disclosed in patent application No. 201610291100.3, wherein low-concentration rhenium-rich slag in waste copper smelting acid is precipitated by using a precipitant and NaClO is used3-NaCl-H2SO4The rhenium-rich slag is leached by the system, the pH value is adjusted to neutralize and remove impurities from the leaching solution, most of bismuth and part of copper, arsenic and molybdenum are removed, then an organic phase is adopted for extraction and back extraction, and the extraction liquid is concentrated, cooled and crystallized to obtain ammonium rhenate crystals.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes, which avoids the defect of acidification leaching, and the obtained ammonium rhenate has extremely high purity and has the advantages of simplicity and high efficiency in operation and environmental protection.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes comprises the following steps:
step 1: adding the additive into the copper-arsenic filter cake raw material, fully and uniformly stirring, and then roasting at the temperature of 200-400 ℃ to realize the separation of arsenic and sulfur, thereby obtaining a copper-rich and rhenium-rich intermediate product;
step 2: crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to obtain powder, adding a chlorinating agent into the powder, granulating, and volatilizing rhenium at 600-;
and step 3: spraying the obtained rhenium volatile matter by using an alkaline solution to obtain a rhenate solution, and purifying and impurity-removing, ion-exchanging and classically precipitating the rhenate solution;
and 4, step 4: and (3) introducing ammonia gas to adjust the pH value of the rhenate solution to 8.0-10.0, concentrating, cooling, crystallizing and recrystallizing to obtain a high-purity ammonium rhenate product and obtain a product with high-grade copper.
Preferably, the additive is soluble sodium salt and soluble ammonium salt, the soluble sodium salt is any one or mixture of more of sodium chloride, sodium nitrate, sodium sulfate, sodium sulfite, sodium carbonate, sodium bicarbonate and sodium bisulfate, the soluble ammonium salt is any one or mixture of more of ammonium sulfate, ammonium chloride and ammonium nitrate,
preferably, the addition amount of the additive is 2.0-30.0% of the mass fraction of the copper arsenic filter cake raw material, and more preferably, the addition amount of the additive is 20.0% of the mass fraction of the copper arsenic filter cake raw material.
Preferably, the temperature of the calcination is 200-400 deg.C, and more preferably, the temperature of the calcination is 300 deg.C.
Preferably, the particle size of the powder is controlled to be 20-200 mesh, more preferably, the particle size of the powder is controlled to be 100 mesh.
Preferably, the chlorinating agent is a chlorine-containing salt comprising one or a mixture of more of potassium chloride, sodium chloride, calcium chloride, lead chloride, sodium chlorate and potassium chlorate, the adding proportion of the chlorinating agent is 10.0-50.0% of the mass fraction of the powder, and more preferably, the adding proportion of the chlorinating agent is 40.0% of the mass fraction of the powder
Preferably, the alkaline solution is any one or a mixture of sodium hydroxide, potassium hydroxide and sodium bicarbonate.
Preferably, the purification and impurity removal is carried out by adopting magnesium salt to precipitate trace arsenic impurities.
Preferably, the ion exchange is carried out using a large pore size resin having a volumetric exchange flow rate of 1.0 to 3.0m3/h。
Preferably, the classical precipitation method comprises adding 5.0-20.0% ammonium chloride or ammonia water at 60-80 deg.C, standing, adjusting pH to 7.0-8.0 by adding hydrochloric acid, naturally settling, and filtering with cloth bag.
Preferably, the concentration temperature is 80-105 ℃, and the cooling crystallization temperature is below 0 ℃.
The invention has the beneficial effects that:
the method for extracting ammonium rhenate from the high-risk solid waste copper-arsenic filter cake has the characteristics of industrial, clean and large-batch treatment of high-risk solid wastes and efficient recycling of scarce resources, and has good industrial application value and prospect. The process avoids the defects of acidification leaching, utilizes the advantages of the treatment capacity of the traditional roasting process, overcomes the disadvantage of adverse effect on the environment in the traditional process, and has the advantages of high purity of the obtained ammonium rhenate, good recovery effect, simple and efficient operation, environmental friendliness, low maintenance cost and great practical significance on the treatment of solid wastes and the recovery of scarce resources.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one skilled in the art from the embodiments given herein are intended to be within the scope of the invention.
Example 1
Adding sodium bisulfate with the mass fraction of 2.0 percent into the copper arsenic filter cake raw material, fully and uniformly stirring, and then roasting the material at the temperature of below 200 ℃ to realize the separation of arsenic and sulfur; crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to obtain powder, controlling the granularity of the powder to be 20 meshes, adding potassium chloride with the mass fraction of 15.0% into the powder, granulating, and volatilizing rhenium at 600 ℃; spraying the obtained rhenium volatile matter by using a sodium hydroxide solution to obtain a sodium rhenate solution, adding a magnesium chloride solution with the mass fraction of 3.0% into the sodium rhenate solution to perform purification and impurity removal, wherein the purification and impurity removal are to precipitate trace arsenic and other impurities by using a magnesium salt, and D312 large-aperture resin is used at the particle size of 1.5m3Ion exchange is carried out at the exchange flow rate of/h, ammonia water is added for standing, then hydrochloric acid is used for adjusting the pH value to 8.0, and natural precipitation is carried out; and (3) introducing ammonia gas to adjust the pH value to 9.0, concentrating at 90 ℃, cooling and crystallizing at-4 ℃, and recrystallizing to obtain a high-purity ammonium rhenate product and a product with high-grade copper.
The test result shows that: the purity of ammonium rhenate obtained after the high-risk solid waste copper arsenic filter cake is treated reaches 99.2%, and the recovery rate is 98.8%.
Example 2
Adding ammonium sulfate with the mass fraction of 15.0% into the copper-arsenic filter cake raw material, fully and uniformly stirring, and roasting the material at the temperature of below 400 ℃ to realize the separation of arsenic and sulfur; crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to 200 meshes, adding potassium chloride with the mass fraction of 50.0% into powder, granulating, and volatilizing rhenium at 800 ℃; spraying the obtained rhenium volatile substance with potassium hydroxide solution to obtain sodium rhenate solution, adding magnesium chloride solution with mass fraction of 5.0% to the sodium rhenate solution to purify and remove trace impurities such as arsenic, and purifying with D316 macroporous resin at 3.0m3Ion exchange is carried out at the exchange flow rate of/h, ammonia water is added for standing, then hydrochloric acid is used for adjusting the pH value to 8.0, and natural precipitation is carried out; adjusting pH to 10.0 by introducing ammonia gas, concentrating at 105 deg.C, cooling at-1 deg.C for crystallization, and recrystallizing to obtain high-purity ammonium rhenate productA product with high-grade copper is obtained.
The test result shows that: the purity of ammonium rhenate obtained after the high-risk solid waste copper arsenic filter cake is treated reaches 99.8%, and the recovery rate is 99.2%.
Example 3
Adding sodium carbonate with the mass fraction of 30.0% into the copper-arsenic filter cake raw material, fully and uniformly stirring, and roasting the material at the temperature of below 300 ℃ to realize the separation of arsenic and sulfur; crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to 100 meshes, adding sodium chloride with the mass fraction of 8.0% and calcium chloride with the mass fraction of 10.0% into the powder, granulating, and volatilizing rhenium at 1200 ℃; spraying the obtained rhenium volatile substance with sodium bicarbonate solution to obtain sodium rhenate solution, adding 10.0 wt% magnesium chloride solution to the sodium rhenate solution to purify and remove trace arsenic and other impurities, and purifying with D310 macroporous resin at 1.0m3Ion exchange is carried out at the exchange flow rate of/h, ammonia water is added for standing, then hydrochloric acid is used for adjusting the pH value to 7.0, and natural precipitation is carried out; and (3) introducing ammonia gas to adjust the pH value to 9.0, concentrating at 80 ℃, cooling and crystallizing at-5 ℃, and recrystallizing to obtain a high-purity ammonium rhenate product and a product with high-grade copper.
The test result shows that: the purity of ammonium rhenate obtained after the high-risk solid waste copper arsenic filter cake is treated reaches 99.5%, and the recovery rate is 99.0%.
Example 4
Adding sodium sulfite with the mass fraction of 20.0 percent into the copper-arsenic filter cake raw material, fully and uniformly stirring, and roasting the material at the temperature of below 200 ℃ to realize the separation of arsenic and sulfur; crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to 100 meshes, adding 40.0 mass percent of sodium chlorate into the powder, granulating, and volatilizing rhenium at 800 ℃; spraying the obtained rhenium volatile matter by using a potassium hydroxide solution to obtain a sodium rhenate solution, adding a magnesium chloride solution with the mass fraction of 5.0% to the sodium rhenate solution to purify and remove impurities, and adopting D316 macroporous resin at 3.0m3Ion exchange is carried out at the exchange flow rate of/h, ammonia water is added for standing, then hydrochloric acid is used for adjusting the pH value to 7.5, and natural sedimentation is carried outPrecipitating; and (3) introducing ammonia gas to adjust the pH value to 8.5, concentrating at 105 ℃, cooling and crystallizing at-5 ℃, and recrystallizing to obtain a high-purity ammonium rhenate product and a product with high-grade copper.
The test result shows that: the purity of ammonium rhenate obtained after the high-risk solid waste copper arsenic filter cake is treated reaches 99.4%, and the recovery rate is 99.1%.
Example 5
Adding sodium bisulfate with the mass fraction of 35.0% into the copper arsenic filter cake raw material, fully and uniformly stirring, and roasting the material at the temperature of below 350 ℃ to realize the separation of arsenic and sulfur; crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to 150 meshes, adding sodium chloride with the mass fraction of 8.0% and calcium chloride with the mass fraction of 10.0% into the powder, granulating, and volatilizing rhenium at 900 ℃; spraying the obtained rhenium volatile substance with sodium bicarbonate solution to obtain sodium rhenate solution, adding 10.0 wt% magnesium chloride solution to the sodium rhenate solution to purify and remove trace arsenic and other impurities, and purifying with D310 macroporous resin at 1.0m3Ion exchange is carried out at the exchange flow rate of/h, ammonia water is added for standing, then hydrochloric acid is used for adjusting the pH value to 7.6, and natural precipitation is carried out; and (3) introducing ammonia gas to adjust the pH value to 9.5, concentrating at 80 ℃, cooling and crystallizing at-6 ℃, and recrystallizing to obtain a high-purity ammonium rhenate product and a product with high-grade copper.
The test result shows that: the purity of ammonium rhenate obtained after the high-risk solid waste copper arsenic filter cake is treated reaches 99.2%, and the recovery rate is 99.6%.
Although the present invention has been described with reference to the specific embodiments, it should be understood that the scope of the present invention is not limited thereto, and those skilled in the art will appreciate that various modifications and variations can be made without inventive changes by those skilled in the art based on the technical solutions of the present invention.
Claims (7)
1. A method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes is characterized by comprising the following steps:
step 1: adding the additive into the copper-arsenic filter cake raw material, fully and uniformly stirring, and then roasting at the temperature of 200-400 ℃ to realize the separation of arsenic and sulfur, thereby obtaining a copper-rich and rhenium-rich intermediate product;
the additive is soluble sodium salt and soluble ammonium salt, the soluble sodium salt is any one or a mixture of more of sodium chloride, sodium nitrate, sodium sulfate, sodium sulfite, sodium carbonate, sodium bicarbonate and sodium bisulfate, the soluble ammonium salt is any one or a mixture of more of ammonium sulfate, ammonium chloride and ammonium nitrate, and the addition amount of the additive is 2.0-30.0% of the mass fraction of the copper-arsenic filter cake raw material;
step 2: crushing and grinding the obtained copper-rich and rhenium-rich intermediate product to obtain powder, adding a chlorinating agent into the powder, granulating, and volatilizing rhenium at 600-;
the chlorinating agent is chlorine-containing salts and comprises one or a mixture of more of potassium chloride, sodium chloride, calcium chloride, lead chloride, sodium chlorate and potassium chlorate, and the addition proportion of the chlorinating agent is 10.0-50.0% of the mass fraction of the powder;
and step 3: spraying the obtained rhenium volatile matter by using an alkaline solution to obtain a rhenate solution, and purifying and impurity-removing, ion-exchanging and classically precipitating the rhenate solution;
and 4, step 4: and (3) introducing ammonia gas to adjust the pH value of the rhenate solution to 8.0-10.0, concentrating, cooling, crystallizing and recrystallizing to obtain a high-purity ammonium rhenate product and obtain a product with high-grade copper.
2. The method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes according to claim 1, wherein the particle size of the powder is controlled to be 20-200 meshes.
3. The method for extracting ammonium rhenate from the high-risk solid waste copper-arsenic filter cakes according to claim 1, wherein the alkaline solution is any one or a mixture of sodium hydroxide, potassium hydroxide and sodium bicarbonate.
4. The method for extracting ammonium rhenate from the high-risk solid waste copper-arsenic filter cake according to claim 1, wherein the purification and impurity removal is to precipitate trace arsenic impurities by using magnesium salts.
5. The method for extracting ammonium rhenate from the high-risk solid waste copper-arsenic filter cake according to claim 1, wherein the ion exchange adopts a large-aperture resin, and the volume exchange flow rate of the large-aperture resin is 1.0-3.0m & lt 3 & gt/h.
6. The method for extracting ammonium rhenate from the high-risk solid waste copper-arsenic filter cake according to claim 1, wherein the classic precipitation method comprises the steps of adding ammonium chloride or ammonia water with the mass concentration of 5.0-20.0% at the temperature of 60-80 ℃, standing, adjusting the pH value to 7.0-8.0 by adding hydrochloric acid, and performing cloth bag filtration after natural precipitation.
7. The method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes according to claim 1, wherein the concentration temperature is 80-105 ℃, and the cooling crystallization temperature is below 0 ℃.
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Effective date of registration: 20220525 Address after: 572732 No. 1, Hainan (Changjiang) clean energy high tech Industrial Park, Haiwei Town, Changjiang Li Autonomous County, Hainan Province Patentee after: Hainan Walker New Material Technology Co.,Ltd. Address before: 412007 503, building C, R & D center, China Power Valley Independent Innovation Park, Xianyue Ring Road, Tianyuan District, Zhuzhou City, Hunan Province Patentee before: HUNAN TRAILBLAZER ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. |