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Method for purifying crude selenium

A purification method and crude selenium technology, applied in the field of purification and preparation of scattered metals, to achieve the effect of high purity and low content

Pending Publication Date: 2020-02-04
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It only studied the effect of tellurium on the purification of crude selenium, and did not involve other impurities; Ou Gaoyu et al. used hydrogen peroxide to oxidize the selenium in the selenium-containing waste into an ion state under strong acidic conditions, and then added an appropriate amount of Sodium chloride and ammonia, through solid-liquid separation to obtain selenium-containing filtrate, and then reduce the selenium-containing filtrate with hydrazine hydrate to obtain selenium simple substance, the purity can only reach more than 90%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A method for purifying crude selenium, comprising the following steps:

[0015] (1) Add sulfuric acid and water to the copper anode slime obtained by copper electrolysis, then pass through oxygen to oxidize and decopper, add sodium hypochlorite to the slag to deselenize, and obtain SeO-containing 3 2- solution, and then into SO 2 The thick selenium slag obtained by reduction, the massfraction of Se in the thick selenium slag is 90%, the massfraction of Te is 1%, the massfraction of Cu is 1%, the massfraction of Pb is 2%, and all the other are unavoidable impurities;

[0016] (2) Take 50 g of the coarse selenium slag obtained in step (1) and put it in a beaker, and slowly add a regulating agent, the regulating agent is H with a volume ratio of 1:1 2 o 2 solution and Na 2 CO 3 A mixed solution formed by mixing solutions, wherein, H 2 o 2 The mass concentration of the solution is 15%, Na 2 CO 3 The concentration of solution is 1mol / L, along with the stirring of gl...

Embodiment 2

[0018] A method for purifying crude selenium, comprising the following steps:

[0019] Get thick selenium slag 50g and put in beaker, the massfraction of Se in the thick selenium slag is 85%, the massfraction of Te is 4%, the massfraction of Cu is 2%, the massfraction of Pb is 2%, all the other are unavoidable Impurities, and slowly add the regulator, the regulator is H with a volume ratio of 1:2 2 o 2 solution and Na 2 CO 3 A mixed solution formed by mixing solutions, wherein, H 2 o 2 The mass concentration of the solution is 15%, Na 2 CO 3 The concentration of solution is 0.5mol / L, along with the stirring of glass rod, carry out pulping, record the pH value of mixed material with pH meter to be 6.69, stop adding mixed solution, the solid-liquid quality of coarse selenium slag and regulator now Volume ratio Kg:L is 0.5:1, filters, and obtains selenium 3.7g / L in the filtrate, obtains thick selenium filter cake simultaneously, thick selenium filter cake is weighed, puts ...

Embodiment 3

[0021] A method for purifying crude selenium, comprising the following steps:

[0022] Get thick selenium slag 50g and put in beaker, the massfraction of Se in the thick selenium slag is 88%, the massfraction of Te is 2%, the massfraction of Cu is 1.5%, the massfraction of Pb is 1.5%, all the other are unavoidable Impurities, and slowly add the regulator, the regulator is H with a volume ratio of 1:3 2 o 2 solution and Na 2 CO 3 A mixed solution formed by mixing solutions, wherein, H 2 o 2 The mass concentration of the solution is 15%, Na 2 CO 3 The concentration of solution is 0.6mol / L, along with the stirring of glass rod, carry out pulping, record the pH value of mixed material with pH meter to be 6.92, stop adding mixed solution, the solid-liquid quality of coarse selenium slag and regulator now Volume ratio Kg:L is 0.7:1, filters, and obtains selenium 1.2g / L in the filtrate, obtains thick selenium filter cake simultaneously, thick selenium filter cake is weighed, p...

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Abstract

A method for purifying crude selenium comprises adding a regulating agent into that coarse selenium slag for pulping until the pH value is 6.5-7, oxidizing and pulping the coarse selenium slag by theregulating agent simultaneously, shortening the process period and reducing the cost, pumping and filtering to obtain coarse selenium powder, and condensing filter cake after vacuum distillation to obtain refined selenium. According to the invention, the regulating agent is added into the crude selenium slag, wherein the regulating agent is a mixed solution of oxidant and alkali, and the mixed solution undergoes oxidation reaction with impurity elements in the crude selenium slag, so that the occurrence state of impurity components is changed and slurry is mixed at the same time; using the difference between the properties of impurity oxides with changed occurrence states and selenium under vacuum conditions, selenium and impurity elements are efficiently separated through vacuum distillation, the content of impurity elements in selenium is reduced, and selenium products with high purity are obtained.

Description

technical field [0001] The invention relates to the field of purification and preparation of scattered metals, in particular to a method for purifying crude selenium. [0002] technical background [0003] As a kind of scattered metal, selenium has become a key material supporting the development of high technology and new product development of materials (pharmaceuticals, agriculture, food). More than 90% of selenium in industry is produced from the comprehensive recovery and utilization process of copper anode slime. Copper anode slime is processed by sulfidation and roasting, Se is replaced by SeO 2 After gas volatilization and deselenization, it is dissolved in water to obtain SeO 3 2- solution, followed by SO 2 Reduction and precipitation to obtain coarse selenium powder; or leaching copper anode slime with sodium hypochlorite solution to obtain SeO 3 2- solution, followed by SO 2 Reduction and precipitation also give coarse selenium powder. Coarse selenium powde...

Claims

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Application Information

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IPC IPC(8): C01B19/02
CPCC01B19/02Y02P10/20
Inventor 徐宝强罗欢杨斌查国正蒋文龙杨佳刘大春王飞李一夫田阳熊恒孔祥峰曲涛孔令鑫戴永年
Owner KUNMING UNIV OF SCI & TECH
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