Purification process of copper smelting byproduct ammonium perrhenate

A by-product technology of ammonium perrhenate and ammonium perrhenate, applied in the preparation of rhenium compounds, rhenium compounds, inorganic chemistry, etc., can solve the problem of high ion content

Pending Publication Date: 2020-11-03

铜陵铜冠优创特种材料有限公司

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Problems solved by technology

[0004] The purpose of the present invention is to provide a purification process for ammonium perrhenate, a by-product of copper smelting, to solve th...

Method used

The purification process of copper smelting by-product ammonium perrhenate provided by the invention comprises six steps of dissolving, vacuum filtration, resin exchange, evaporative concentration, freeze crystallization and filter drying, by thick ammonium rhenate solution pH value The adjustment of dissolved concentration, dissolution temperature, crystallization time, crystallization temperature, stirring rate and selection of s...

Abstract

The invention discloses a purification process of a copper smelting byproduct ammonium perrhenate. The process comprises the following six steps: dissolving, vacuum filtration, resin exchange, evaporation concentration, freezing crystallization and filtration and drying. By regulating the pH value of a crude ammonium perrhenate solution, the dissolving concentration, dissolving temperature, crystallization time, crystallization temperature, stirring rate and special resin are selected, thus preparing the ammonium perrhenate with purity being higher than 99.999%. The problem that the content ofsulfur, arsenic, selenium, copper, iron, lead, zinc and other ions in the copper smelting byproduct ammonium perrhenate is high is solved, the impurities are effectively removed, 73 impurity elementsin the copper smelting byproduct ammonium perrhenate reach 1-5 ppm or below, the recovery rate of ammonium perrhenate is guaranteed, and the recovery rate of ammonium perrhenate is 95% or above.

Application Domain

Rhenium compounds preparation

Technology Topic

ArsenicLead zinc +5

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Examples

Experimental program(1)

Example Embodiment

[0023] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present invention.

[0024] In the description of the present invention, it should be understood that the terms "opening", "upper", "lower", "thickness", "top", "middle", "length", "inner", "around", etc. The indication of the orientation or position relationship is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the component or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention .

[0025] Such as figure 1 As shown, the present invention provides a purification process of ammonium perrhenate by-product from copper smelting, which specifically includes the following steps:

[0026] Step S1, dissolving: dissolve the low-purity ammonium perrhenate produced by copper smelting in hot water at 60-80°C with a concentration of about 6-12%, control the speed of the stirring paddle at 60-90 revolutions per minute, and add ammonia water Adjust to alkaline, PH value range 9-10.

[0027] Step S2, vacuum filtration: Put the above solution into the filter tank, and perform hot filtration through the filter. The filter is made of non-metallic polymer material, 200 mesh, and the vacuum is about -30kPa~-60kPa. In the later stage of filtration, low vacuum is used. Filter to ensure that there is no residual solution on the filter.

[0028] Step S3, resin exchange: the above-mentioned filtrate is adsorbed by a dedicated anion and cation resin to remove impurities anion and cation respectively to obtain the adsorption mother liquor. The anion resin is required to have a good adsorption effect on sulfur, arsenic and selenium. Lead and zinc have good adsorption effect.

[0029] Step S4, evaporation and concentration: the mother liquor obtained after adsorption and removal of impurities is transported to a two-stage concentration tank for evaporation and concentration, and the concentration of ammonium perrhenate after concentration is about 16-20%.

[0030] Step S5, freeze crystallization: transport the concentrated ammonium perrhenate solution to the freezing crystallization kettle for freezing crystallization, the freezing crystallization time is 4-6h, before freezing crystallization, add dilute acid or dilute alkali to adjust the pH to below 6, control The crystallization temperature is 0-5℃, and the stirring speed is 90-120 revolutions per minute.

[0031] Step S6, filtration and drying: put the crystal mixture into a filter tank, filter through an 80-mesh non-metal filter, the moisture content of the ammonium perrhenate crystals collected on the filter is less than 5%, and vacuum filtration is used in the later stage of the filtration to obtain The ammonium perrhenate crystals are dried at a drying temperature of 100-120°C and a drying time of 10-12h to obtain the finished ammonium perrhenate.

[0032] The purification process of copper smelting by-product ammonium perrhenate provided by the present invention includes six steps of dissolution, vacuum filtration, resin exchange, evaporation and concentration, freezing crystallization, and filtration and drying. By adjusting the PH value of crude ammonium rhenate solution, For the selection of dissolution concentration, dissolution temperature, crystallization time, crystallization temperature, stirring rate and special resin, more than 99.999% of ammonium perrhenate is obtained, which solves the problem of sulfur, arsenic, selenium, copper, The high content of iron, lead, and zinc plasma effectively removes the above-mentioned impurities, so that the 73 impurity elements are below 1-5 ppm, and the recovery rate of ammonium perrhenate is guaranteed. above 95.

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