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Method using wet alkaline process of cobalt-nickel (Co-Ni) residue containing arsenic to prepare arsenate

A technology of arsenic-cobalt-nickel slag and arsenate, which is applied in the direction of arsenate/arsenite, process efficiency improvement, etc., can solve the problems such as inability to realize arsenic extraction, promote a large amount of rapid crystallization, and eliminate the crystallization induction period , the effect of simple operation

Inactive Publication Date: 2013-02-13
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Description
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Problems solved by technology

Chinese invention patent CN1101010A proposes a method for directly producing sodium arsenate by wet method of roasting arsenic-containing fumes with tin. After slurrying arsenic-containing fumes with water, slowly add limestone powder under stirring, and adjust the pH value of the slurry to 5~6, heat up the slurry and maintain it at 50~75°C, add soda ash solution and industrial hydrogen peroxide (As:H 2 o 2 =1.8:1), make the arsenic oxidized and leached, filter, add NaOH solution to the filtrate to adjust the pH value to 12~14, boil for 30 minutes, filter out the sediment, and the purified liquid is concentrated and crystallized to produce high-quality sodium arsenate; this method is used to realize The resource utilization of arsenic in the arsenic-containing dust is achieved, but when this process is used to process the arsenic-containing cobalt-nickel slag of the present invention, due to the strong stability of arsenic in the alloy form, the weak alkali conditions adopted in the above method cannot realize the arsenic-containing cobalt-nickel slag Extraction of arsenic in

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  • Method using wet alkaline process of cobalt-nickel (Co-Ni) residue containing arsenic to prepare arsenate

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Prepare a NaOH solution with an alkali concentration of 200g / L, mix the arsenic-containing cobalt-nickel slag and NaOH solution evenly according to the liquid-solid ratio of 4:1, and place them in an alkali-resistant high-pressure reaction kettle for heating and stirring; when the temperature of the slurry reaches 150°C, Introduce 0.5MPa oxygen into the reaction kettle, and start timing; after leaching for 2 hours, cool the slurry to below 90°C and take it out; dilute the slurry until the NaOH concentration is 150g / L and filter, and use 80~90°C for the slag phase Hot water is used for multi-stage countercurrent washing, and the arsenic content in the slag is reduced to 0.17%; the filtrate is evaporated until the NaOH concentration is 200g / L, and 3% sodium arsenate seeds are added to the concentrated lye, stirred and gradually Cool to 30°C, crystallize for 24 hours and then filter and separate. The solid phase is sodium arsenate crystals, and the liquid phase is NaOH solu...

Embodiment 2

[0021] Prepare a KOH solution with an alkali concentration of 100g / L, mix arsenic-containing cobalt-nickel slag and KOH solution at a liquid-solid ratio of 5:1 to form a uniform slurry and place it in an alkali-resistant high-pressure reactor for heating and stirring; when the temperature of the slurry reaches 250°C Finally, inject 1.0MPa oxygen-enriched gas into the reactor, and start timing; after leaching for 1 hour, cool the slurry to below 90°C and take it out; filter the slurry, and carry out multi-stage countercurrent flow with hot water at 80-90°C for the slag phase After washing, the arsenic content in the slag was reduced to 0.6%; the filtrate was evaporated until the KOH concentration was 250g / L, and 1% potassium arsenate seed crystals were added to the evaporated lye, stirred and gradually cooled to 50°C to crystallize After 16 hours, filter and separate, the solid phase is potassium arsenate crystal, and the liquid phase is KOH solution containing a small amount of...

Embodiment 3

[0023] Prepare a NaOH solution with an alkali concentration of 50g / L, mix the arsenic-containing cobalt-nickel slag and NaOH solution according to the liquid-solid ratio of 10:1 to form a uniform slurry and place it in an alkali-resistant high-pressure reaction kettle for heating and stirring; when the temperature of the slurry reaches 250°C Finally, inject 2.0MPa air into the reactor and start timing; after leaching for 4 hours, cool the slurry to below 90°C and take it out; filter the slurry, and wash the slag phase with hot water at 80~90°C for multi-stage countercurrent washing. The arsenic content in the slag was reduced to 1.0%; the filtrate was evaporated until the NaOH concentration was 300g / L, and 0.1% sodium arsenate seeds were added, stirred and gradually cooled to 60°C, crystallized for 10 hours, filtered and separated, and the solid phase was arsenic The liquid phase is NaOH solution containing a small amount of arsenic, and the alkali concentration is adjusted and...

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Abstract

The invention relates to a method using wet alkaline process of cobalt-nickel (Co-Ni) residue containing arsenic to prepare arsenate, and then preparing an arsenate product by using evaporative cooling and crystallizing method. The method comprises the steps of evenly mixing the Co-Ni residue containing the arsenic with sodium hydroxide or potassium hydroxide solution of certain density, placing mixture in a alkali-resistant high-pressure reaction kettle, introducing oxygen or oxygen-enriched gas of certain pressure as an oxidant, and reacting at a certain temperature, adjusting alkali density of slurry after reaction to less than 150g / L with water or low-density alkali liquid when the reaction is over, carrying out liquid-solid separation, obtaining arsenic-enriched liquid, evaporating the arsenic-enriched liquid, adding little seed crystal to cool and crystallize, and obtaining qualified arsenate crystal products after the liquid-solid separation. Crystallized mother liquid can be returned to be used for material distribution of the Co-Ni residue containing the arsenic. Recycling rate of the arsenic is over 99%, the method can prevent the arsenic from volatilizing during baking process and arsenic hydride gas from being generated during acid leaching. The method is simple in process, and can achieve recycle and reuse of the arsenic of the Co-Ni residue containing the arsenic.

Description

technical field [0001] A method for preparing arsenate by using arsenic-containing cobalt-nickel slag wet-alkali method, which involves a method of using sodium hydroxide or potassium hydroxide solution to pressurize and oxidize low-valence arsenic in arsenic-containing cobalt-nickel slag, so that the slag phase The arsenic component in the arsenic is transformed into arsenate such as sodium arsenate or potassium arsenate in a high-valence state, enters the liquid phase, and is separated by evaporation and crystallization to prepare arsenate. Background technique [0002] Arsenic is carcinogenic to the human body and is one of the five heavy metals targeted for prevention and control in the first category of my country's "Twelfth Five-Year Plan for Comprehensive Prevention and Control of Heavy Metal Pollution". At present, there are many studies on the treatment of arsenic-containing wastewater and arsenic-containing waste residue, but most of them are to solidify and store ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B3/12C22B3/22C01G28/02C22B30/04
CPCY02P10/20
Inventor 张盈郑诗礼余国林张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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