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Short-flow method for preparing antimony or bismuth hydrolysis mother solution and composite cleaning agent for short-flow method

A purifying agent and mother liquor technology, applied in the field of metallurgy and chemical industry, can solve the problems of weak reducibility of sodium thiosulfate, slow arsenic reduction process, long arsenic removal process cycle, etc., and achieves improved raw material adaptability, easy process control, and raw material adaptability. strong effect

Inactive Publication Date: 2012-12-12
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0007] The use of sodium thiosulfate as an arsenic removal agent brings two major problems: ① sodium thiosulfate itself has weak reducibility, and it is prone to self-oxidation-reduction reactions in acidic systems, resulting in SO 2 and difficult to filter elemental sulfur; SO 2 Only after being dissolved in water to generate sulfurous acid, can trivalent arsenic be reduced to zero-valent arsenic by sulfite; SO 2 The reaction with water is a "gas-liquid" reaction, and the process is slow, resulting in a long cycle for the current arsenic removal process; ② Sodium thiosulfate is used as the arsenic removal agent, SO 2 The sulfite generated by dissolving in the solution has a low local concentration in the reaction system, causing the process of reducing arsenic to be slow, and the precipitated arsenic has fine particles, high activity, is difficult to filter, and is easy to return to the solution
This is the root cause of the difficulty in controlling arsenic in high-purity antimony trioxide (or bismuth trioxide) products produced by the existing process and easily exceeding the standard

Method used

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  • Short-flow method for preparing antimony or bismuth hydrolysis mother solution and composite cleaning agent for short-flow method
  • Short-flow method for preparing antimony or bismuth hydrolysis mother solution and composite cleaning agent for short-flow method

Examples

Experimental program
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Effect test

Embodiment 1

[0050] The composition of antimony concentrate provided by a company in Hunan is: Sb 37.31%, Fe 13.68%, SiO 2 6.33%, Pb 4.6%, S 26.5%, As 2.1%.

[0051] Take 100g of the above antimony concentrate powder, when the liquid-solid ratio (ml / g) is 5:1, and the acidity of hydrochloric acid is 4.5mol L -1 , oxidizing agent Cl 2 The amount of addition (in Sb 2 S 3 consumption) is twice the theoretical amount, and the leaching temperature is 80°C. After leaching for 120 minutes, cool, clarify, filter and separate, wash the filter residue with 1:1 hydrochloric acid 100ml as the washing liquid, combine the washing liquid and the filtrate, and dry the filter residue. Weigh dry. The antimony content in the filtrate and filter residue was analyzed, and the leaching rate of antimony was 98.7% (liquid meter) / 99.5% (residue meter).

[0052] Analyze the content of the main impurity components in the filtrate such as lead, arsenic, etc., add a composite reduction purifying agent of 1.2 tim...

Embodiment 2

[0054] The composition of bismuth concentrate provided by a company in Hunan is: Bi 45.1%, Fe 11.28%, SiO 2 4.13%, Pb 2.6%, S 22.5%, As 1.1%.

[0055] Take 1000g of the above-mentioned bismuth concentrate powder, when the liquid-solid ratio (ml / g) is 4:1, and the acidity of hydrochloric acid is 4.0mol L -1 , Oxidant NaClO 3 The amount of addition (by Bi 2 S 3 consumption) is 2.5 times of the theoretical amount, and the leaching temperature is 90°C. After leaching for 90 minutes, cool, clarify, filter and separate, wash the filter residue with 1:1 hydrochloric acid 500ml as the washing liquid, combine the washing liquid and the filtrate, and dry the filter residue. Weigh dry. Analyze the bismuth content in filtrate and filter residue, obtain the leaching rate of bismuth 97.9% (liquid meter) / 98.6% (residue meter).

[0056] Analyze the main impurity components in the filtrate such as the content of lead, arsenic etc., add the composite reducing purifying agent of 2 times of...

Embodiment 3

[0058]The composition of antimony concentrate provided by a company in Hunan is: Sb 27.11%, Fe 19.22%, SiO 2 6.33%, Pb 14.6%, S 16.5%, As 5.1%.

[0059] Take 10Kg of the above antimony concentrate powder, when the liquid-solid ratio (ml / g) is 4:1, and the acidity of hydrochloric acid is 5mol L -1 , oxidizing agent Cl 2 The amount of addition (in Sb 2 S 3 consumption) is 3 times of the theoretical amount, and the leaching temperature is 85°C. After leaching for 180 minutes, cool, clarify, filter and separate, wash the filter residue with 1:1 hydrochloric acid 1000ml as the washing liquid, combine the washing liquid and the filtrate, and dry the filter residue. Weigh dry. The antimony content in the filtrate and filter residue was analyzed, and the leaching rate of antimony was 98.2% (liquid meter) / 98.9% (residue meter).

[0060] Analyze the content of the main impurity components in the filtrate such as lead, arsenic, etc., add a composite reduction purifying agent of 3 t...

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Abstract

The invention discloses a short-flow method for preparing antimony or bismuth hydrolysis mother solution and a composite cleaning agent for the short-flow method. The short-flow method comprises a chlorinated acid leaching step and a composite restoring purification step; and the obtained qualified hydrolysis mother solution can be hydrolyzed, converted and washed to obtain high-purity diantimony trioxide (or bismuth trioxide). The short-flow method comprises the following specific steps of: firstly, carrying out chlorinated acid leaching on antimony sulfide ore concentrate (or bismuth sulfide ore concentrate); secondly, carrying out composite restoring purification on leachate; and filtering the composite restoring purification liquid to obtain antimony (or bismuth) hydrolysis mother solution, wherein main impurity metals of the mother solution comprise Pb<2+> of which the concentration can be smaller than 50mg / L, As<3+> of which the concentration is smaller than 30mg / L and the S<2-> of which the concentration can be smaller than 50mg / L. The quality of the obtained hydrolysis mother solution can completely meet the requirement of preparing special high-grade and high-purity diantimony trioxide (or bismuth trioxide) by hydrolysis. Compared with a traditional method, the short-flow method has the advantages that the flow is greatly shorten and the production period is shorten by over one third; the whiteness of a high-purity diantimony trioxide (or bismuth trioxide) product obtained by the hydrolysis mother solution can stably reach over 92 percent. The contents of iron, arsenic and aluminum impurities in the product are below 10ppm. A novel process has the remarkable advantages of strong adaptability of raw materials, short process flow, fewer process control points, stable quality of products and the like.

Description

[technical field] [0001] The invention belongs to the field of metallurgy and chemical industry, and relates to a short-flow method for preparing qualified antimony (or bismuth) hydrolysis mother liquor by using antimony sulfide concentrate (or bismuth sulfide concentrate) as a raw material. [Background technique] [0002] Using antimony sulfide (or bismuth sulfide) concentrate as raw material to produce qualified antimony (or bismuth) hydrolysis mother liquor through wet process route The traditional process includes the following steps: ① Using Cl 2 -HCl is the leaching agent for oxidative leaching of antimony sulfide (or bismuth sulfide), and then the solution is filtered through plate and frame to obtain antimony (or bismuth sulfide) leach solution; Afterwards, the solution is filtered through a plate and frame to obtain a primary reducing solution; ③ a certain amount of arsenic-removing agents such as sodium thiosulfate and sodium sulfide are added to the primary reduci...

Claims

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Application Information

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IPC IPC(8): C22B3/10C22B3/44C22B30/02C22B30/06
CPCY02P10/20
Inventor 杨建广邓自祥李俊源周群利
Owner CENT SOUTH UNIV
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