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Method for preparing ammonium perrhenate

A technology of ammonium perrhenate and ammonium salt, applied in the direction of improving process efficiency, can solve problems such as affecting industrial utilization, low product quality, waste of resources, etc., and achieve high quality, comprehensive recovery and utilization, and widely available raw materials. Effect

Active Publication Date: 2015-05-20
洛阳双罗铼材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the production of ammonium perrhenate by evaporation and crystallization, the molybdenum impurities mixed in the rhenium-rich recovery solution are also precipitated in the form of ammonium molybdate crystals (Zhang Qixiu, edited by Zhao Qinsheng, "Tungsten and Molybdenum Metallurgy", September 2005, No. 206- 210 pages), because the evaporation and crystallization properties of ammonium molybdate are the same as those of ammonium perrhenate, it is difficult to remove ammonium molybdate in ammonium perrhenate product even if it is crystallized multiple times, and the ammonium perrhenate product obtained in the third step is inevitable The ground is mixed with ammonium molybdate impurities, resulting in low product grade, difficult to reach more than 90%, affecting industrial utilization
[0014] At present, my country processes 140,000 to 160,000 tons of molybdenum concentrates every year only through oxidation roasting, and continuously produces poor rhenium stock solutions such as molybdenum roasting flue gas eluate and soot leachate, plus enterprises that carry out wet leaching and electro-oxidation leaching The oxidized leaching solution and electro-oxidizing solution produced produce millions of tons of poor rhenium stock solution every year. Due to the low content of rhenium in the poor rhenium stock solution, it is usually at 10ˉ 2 On the order of g / L, most of them are discarded as sewage by manufacturers, resulting in a waste of resources

Method used

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  • Method for preparing ammonium perrhenate
  • Method for preparing ammonium perrhenate
  • Method for preparing ammonium perrhenate

Examples

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Effect test

Embodiment 1

[0048] Ammonium perrhenate is prepared by using molybdenite oxidation leaching solution as raw material, enriched by solvent extraction, concentrated under reduced pressure, thermally decomposed and dissolved and crystallized. The preparation process is as follows figure 1 shown.

[0049] Rhenium-depleted stock solution: molybdenite oxidation leaching solution, which is obtained by high pressure oxygen leaching of molybdenite. The composition of the leaching solution is 0.116 g / L and Mo is 23.4 g / L. In industrial practice, since rhenium is a kind of scattered metal, its content in the earth's crust is about 1×10ˉ 7 %, it is very rare in nature, and its content is low in rhenium-containing ores. The content of rhenium in the poor rhenium stock solution produced after pyrolysis or wet decomposition is low, and the rhenium-containing liquid with rhenium content less than 0.01g / L is equivalent to Each ton of the solution contains less than 10 grams of rhenium, which is of li...

Embodiment 2

[0074] The rhenium compound ammonium perrhenate is prepared by using molybdenite roasting flue gas eluate and smoke leaching liquid as raw materials, ion exchange resin adsorption enrichment, vacuum concentration, thermal decomposition and dissolution crystallization. The preparation process is as follows image 3 shown.

[0075] Rhenium-depleted stock solution: molybdenite roasting flue gas eluate and soot leaching liquid, the molybdenite roasting temperature is 600°C, the roasting method is fluidized roasting, and the rhenium content in the molybdenite roasting flue gas eluent is 1.4g / L, the molybdenum content is 16g / L.

[0076] Prepare ammonium perrhenate, concrete steps are as follows:

[0077] Step 1: Concentrate under reduced pressure to prepare concentrated crystals

[0078] This example uses ion exchange resin adsorption and ammonium salt desorption to collect NH 4 ReO 4 The rhenium-rich recovery solution is concentrated under reduced pressure at 95°C to obtain co...

Embodiment 3

[0101] In this embodiment, the molybdenite electro-oxidizing solution is used as raw material, and the rhenium compound ammonium perrhenate is prepared by extracting and enriching with an organic solvent, concentrating under reduced pressure, thermally decomposing, and dissolving and crystallizing.

[0102] Rhenium-depleted stock solution: molybdenite electrooxidation solution. The molybdenum concentrate slurry made by mixing molybdenum concentrate with 10% NaCl is electrolyzed. During the solution electrolysis, the anode generates oxidant ClO - , the molybdenum concentrate particles are oxidized by the electrochemical oxidant and dissolved in the solution, the composition of the electro-oxidant solution: rhenium 0.038g / L, molybdenum 15 g / L.

[0103] Prepare ammonium perrhenate, concrete steps are as follows:

[0104] Step 1: Concentrate under reduced pressure to prepare concentrated crystals

[0105] In this example, quaternary ammonium salt extraction and perchloric acid s...

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Abstract

The invention relates to the technical field of rhenium recycling and in particular relates to a method for preparing ammonium perrhenate. The ammonium perrhenate is prepared by purifying rhenium-enriched recovery liquid obtained by enrichment of poor-rhenium stock solution, and the rhenium-enriched recovery liquid is subjected to vacuum concentration, heating decomposition and dissolution-crystallization so as to prepare ammonium perrhenate. The method comprises the following steps: step 1, performing vacuum concentration to prepare a concentrated crystal; step 2, performing heating decomposition to collect rhenium heptoxide solids; step 3, performing dissolution-crystallization to prepare ammonium perrhenate; and step 4, recycling molybdenum and rhenium. According to the method disclosed by the invention, molybdenum and rhenium can be effectively separated from each other, and high-grade ammonium perrhenate can be prepared; and moreover, the poor-rhenium stock solution serves as a raw material, the raw materials are wide and readily available, and integrated resource recycling is realized.

Description

technical field [0001] The invention relates to the technical field of rhenium recycling, in particular to one A method for preparing ammonium perrhenate. Background technique [0002] Rhenium has corrosion resistance, wear resistance and good ductility. It is a very important industrial raw material and has a wide range of uses. It can be used as a catalyst, solid propulsion heat-sensitive element, aircraft engine turbine blade, electron tube structural material and superconductor, etc. It is an important intermediate for the preparation of rhenium. The body is rhenium heptoxide and ammonium perrhenate. [0003] The crustal abundance of rhenium is too low, less than 10 -7 %, and associated with molybdenite and porphyry copper ore, more than 80% of rhenium products in the world are recovered from molybdenite processing. Since rhenium mainly exists in molybdenite in the form of isomorphism, the ionic radius of rhenium and molybdenum is similar, both are about 0.06nm, and t...

Claims

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Application Information

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IPC IPC(8): C22B61/00C22B34/34C22B3/22
CPCY02P10/20
Inventor 赵维根楚慧慧范家富潘硕实
Owner 洛阳双罗铼材料科技有限公司
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