A process for the comprehensive recovery of fluorine and phosphorus by alkali decomposition of mixed rare earth concentrate liquid

A technology of mixed rare earth and concentrate, which is applied in the separation and recovery of sodium fluoride, sodium phosphate in the process of rare earth smelting, and the field of comprehensive recovery of fluorine and phosphorus by alkali decomposition of mixed rare earth concentrate liquid, which can solve the problems of shortening the process flow and achieve technological The effect of short process and reduced energy consumption

Active Publication Date: 2019-01-15
BAOTOU RES INST OF RARE EARTHS +1
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Problems solved by technology

[0004] The purpose of the present invention is to solve the separation and recovery of sodium fluoride and sodium phosphate in the industrial production of rare earth concentrate liquid alkali decomposition, shorten the process flow and realize the efficient recovery of resources such as fluorine and phosphorus, and provide a simple process flow and low production cost. Low and pollution-free mixed rare earth concentrate liquid alkali decomposition process for comprehensive recovery of fluorine and phosphorus

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  • A process for the comprehensive recovery of fluorine and phosphorus by alkali decomposition of mixed rare earth concentrate liquid

Examples

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Effect test

Embodiment 1

[0020] Take 500g of sodium hydroxide to make a 65wt% solution, add 100g of mixed rare earth ore (REO 65wt%), mix and heat up to 155°C in a reactor, keep the temperature for reaction, stop the reaction, cool down to a temperature of 110°C, and heat filter to obtain concentrated The lye and alkali cake are rinsed with a small amount of hot water to ensure that the temperature of the system after filtration is greater than 80°C. Continue to cool the concentrated lye to 45°C, and then filter to obtain the sodium phosphate product. After filtering, add the consumed sodium hydroxide to the lye for recycling, and add 100g of mixed rare earth ore (REO65wt%) for the second cycle test. Add 150 mL of water to the alkali cake, stir and wash it, and filter to obtain a primary washing alkali solution. Continue to wash the alkali cake until neutral, then dissolve it with 9M hydrochloric acid, and control the pH of the solution to 4~5 to obtain a rare earth chloride solution. The primary wa...

Embodiment 2

[0023] Take 450g of sodium hydroxide to make a 65wt% solution, add 100g of mixed rare earth ore (REO 65wt%), mix and heat to 150°C in the reactor, keep the temperature for reaction, then stop the reaction and cool down to the temperature of 110°C, filter while it is hot, and get Concentrated lye and alkali cake, then rinse with a small amount of hot water to ensure that the system temperature after filtration is greater than 80°C. Concentrated lye continues to cool down to 50°C, and then filtered to obtain sodium phosphate product. After filtering, add the consumed sodium hydroxide to the lye for recycling, and add 100g of mixed rare earth ore (REO 65wt%) for the second cycle test. Add 200 mL of water to the alkali cake, stir and wash it, and filter to obtain a primary washing alkali solution. Continue to wash the alkali cake until neutral, then dissolve it with 9M hydrochloric acid, and control the pH of the solution to 4~5 to obtain a rare earth chloride solution. The prim...

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Abstract

The invention relates to a comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate. The comprehensive fluorine and phosphorous recovery technology is characterized by including mixing the high-grade mixed rare earth concentrate with a 60wt% sodium hydroxide solution according to a weight ratio of 1:3.5-7.5, reacting for 0.2-1 hour at 150-160 DEG C, conducting hot filtration at 80 DEG C to obtain strong liquid caustic soda and caustic soda cakes, cooling the strong liquid caustic soda to 30-70 DEG C and filtering so as to obtain a sodium phosphate product; mixing the caustic soda cakes into paste prior to washing, and filtering so as to obtain primary caustic soda washed liquid; continuing washing the caustic soda cakes until the caustic soda cakes become neutral, dissolving the neutral caustic soda cakes with 6-10 mol / L hydrochloric acid, and controlling a pH value to be 4-5 so as to obtain a rare earth chloride solution; concentrating the primary caustic soda washed liquid, and filtering so as to obtain a sodium fluoride product. The comprehensive fluorine and phosphorous recovery technology has the advantages that the comprehensive fluorine and phosphorous recovery technology is short in technological process and low in production energy consumption; fluorine and phosphorous recovery and cyclic utilization of liquid caustic soda are achieved, wastewater discharge is avoided, and clean production and comprehensive resource utilization are achieved.

Description

technical field [0001] The invention relates to a process for the comprehensive recovery of fluorine and phosphorus by alkali decomposition of mixed rare earth concentrate liquid, especially the separation and recovery of sodium phosphate and sodium fluoride in the rare earth smelting process, belonging to the field of hydrometallurgy and resource comprehensive utilization. Background technique [0002] Mixed rare earth concentrates account for more than 60% of my country's smelting rare earth concentrates, and are the main raw materials for extracting rare earth elements. In addition to rare earths, there are also scarce resources such as fluorine and phosphorus in concentrates. In the current acid process for decomposing mixed rare earth concentrates, fluorine is discharged from the high-temperature roasting tail gas, which is difficult to recover; phosphorus enters the radioactive leaching slag, which cannot be recycled. [0003] In the alkaline process of decomposing mix...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/30C01B3/14C01D3/02
CPCC01B25/305C01D3/02C01D3/14C01P2006/80
Inventor 许延辉马升峰田皓张丞刘铃声王英杰胡卫红
Owner BAOTOU RES INST OF RARE EARTHS
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