Efficient extraction method for high-purity lanthanum oxide

Abstract

The invention relates to an efficient extraction method for high-purity lanthanum oxide. The efficient extraction method comprises the following steps of (1) extraction: mixing a lanthanum oxide feedliquid with an extraction agent at a volume ratio of 1:(2.5-3.5) for extraction separation, carrying out ultrasonic dispersion for 10-15 min, and carrying out separation after standing, wherein the extraction agent comprises the following raw materials including, by volume, 20%-24% of P507, 10%-15% of 1,2,5-thiadiazole-3,4-dithiol and the balance kerosene; (2) back extraction: carrying out back extraction on an oxalic acid solution with the organic-phase volume being 3.0-4.0 times at 50-60 DEG C, carrying out ultrasonic dispersion for 20-30 min, carrying out precipitation, and carrying out filtration to obtain a precipitate; and (3) oxidation: carrying out burning oxidation on the obtained precipitate at 800-900 DEG C for 12-15 h so as to obtain lanthanum oxide. According to the efficientextraction method provided by the invention, a specific amount of 1,2,5-thiadiazole-3,4-dithiol is added into an extraction system; through cooperation between the 1,2,5-thiadiazole-3,4-dithiol and the P507, the hydrophobicity of a lanthanum extraction complex can be higher; and accordingly, the entry into an organic phase can be easier, and the extraction efficiency and the distribution ratio canbe improved.

Description

Technical field

[0001] The invention belongs to the technical field of rare earth purification, and specifically relates to an efficient extraction method of high-purity lanthanum oxide. Background technique

[0002] Rare earth element (rare earth element) is the general name of the 17 elements of scandium, yttrium, and lanthanide in group IIIB of the periodic table. It mainly exists in the form of single mineral. There are more than 250 kinds of industrial minerals that are suitable for current processing conditions. There are only more than 10 species. China's rare earth resources account for 41.36% of the world's rare earth resources, and it is a veritable large country in rare earth resources, which has laid a solid foundation for the development of China's rare earth industry. Traditional rare earth separation methods include step crystallization, ion exchange, and solvent extraction. Now solvent extraction is the main method for rare earth separation. The step-by-step cry...

Examples

Embodiment 1

[0025] An efficient extraction method of high-purity lanthanum oxide, including the following steps:

[0026] (1) Extraction: Mix the lanthanum chloride feed liquid (1.5mol / L) and the extractant at a volume ratio of 1:3 for extraction and separation, and perform ultrasonic dispersion for 12 minutes (ultrasonic frequency is 25KHz), and separate after standing, and separate the solid phase Recycling, the organic phase is input to the back extraction procedure;

[0027] The extractant includes the following raw materials in volume percentages: 22% P507, 12% 1,2,5-thiadiazo-3,4-dithiol, and the balance is kerosene;

[0028] (2) Back-extraction: Take the oxalic acid solution (20wt%) 3.5 times the volume of the obtained organic phase to back-extract it at 55°C, and perform ultrasonic dispersion for 25 min (ultrasonic frequency is 35KHz), while precipitation is generated, and the precipitate is filtered out;

[0029] (3) Oxidation: The resulting precipitate was burned and oxidized at 850°C f...

Embodiment 2

[0036] An efficient extraction method of high-purity lanthanum oxide, including the following steps:

[0037] (1) Extraction: Mix the lanthanum chloride feed liquid (1.5mol / L) and the extractant at a volume ratio of 1:2.5 for extraction and separation, and perform ultrasonic dispersion for 15 minutes (ultrasonic frequency is 25KHz), and separate after standing, and separate the solid phase Recycling, the organic phase is input to the back extraction procedure;

[0038] The extractant includes the following raw materials in volume percentages: 20% P507, 10% 1,2,5-thiadiazo-3,4-dithiol, and the balance is kerosene;

[0039] (2) Back-extraction: Take the oxalic acid solution (20wt%) 3.0 times the volume of the obtained organic phase to back-extract it at 55°C, and carry out ultrasonic dispersion for 30 min (ultrasonic frequency is 35KHz), at the same time produce precipitation, filter to obtain precipitation;

[0040] (3) Oxidation: The resulting precipitate was burned and oxidized at 85...

Embodiment 3

[0047] An efficient extraction method of high-purity lanthanum oxide, including the following steps:

[0048] (1) Extraction: Mix the lanthanum chloride feed liquid (1.5mol / L) and the extractant at a volume ratio of 1:3.5 for extraction and separation, perform ultrasonic dispersion 10 (ultrasonic frequency 25KHz), separate after standing, and separate the solid phase Recycling, the organic phase is input to the back extraction procedure;

[0049] The extractant includes the following raw materials in volume percentage: 24% P507, 15% 1,2,5-thiadiazo-3,4-dithiol, and the balance is kerosene;

[0050] (2) Back-extraction: Take the oxalic acid solution (20wt%) 4.0 times the volume of the obtained organic phase to back-extract it at 55°C, perform ultrasonic dispersion for 20 minutes (ultrasonic frequency is 35KHz), and produce precipitation at the same time, filter to obtain the precipitate;

[0051] (3) Oxidation: The resulting precipitate was burned and oxidized at 850°C for 14 hours to ...

Technical field

[0001] The invention belongs to the technical field of rare earth purification, and specifically relates to an efficient extraction method of high-purity lanthanum oxide. Background technique

[0002] Rare earth element (rare earth element) is the general name of the 17 elements of scandium, yttrium, and lanthanide in group IIIB of the periodic table. It mainly exists in the form of single mineral. There are more than 250 kinds of industrial minerals that are suitable for current processing conditions. There are only more than 10 species. China's rare earth resources account for 41.36% of the world's rare earth resources, and it is a veritable large country in rare earth resources, which has laid a solid foundation for the development of China's rare earth industry. Traditional rare earth separation methods include step crystallization, ion exchange, and solvent extraction. Now solvent extraction is the main method for rare earth separation. The step-by-step cry...

Examples

Embodiment 1

[0025] An efficient extraction method of high-purity lanthanum oxide, including the following steps:

[0026] (1) Extraction: Mix the lanthanum chloride feed liquid (1.5mol / L) and the extractant at a volume ratio of 1:3 for extraction and separation, and perform ultrasonic dispersion for 12 minutes (ultrasonic frequency is 25KHz), and separate after standing, and separate the solid phase Recycling, the organic phase is input to the back extraction procedure;

[0027] The extractant includes the following raw materials in volume percentages: 22% P507, 12% 1,2,5-thiadiazo-3,4-dithiol, and the balance is kerosene;

[0028] (2) Back-extraction: Take the oxalic acid solution (20wt%) 3.5 times the volume of the obtained organic phase to back-extract it at 55°C, and perform ultrasonic dispersion for 25 min (ultrasonic frequency is 35KHz), while precipitation is generated, and the precipitate is filtered out;

[0029] (3) Oxidation: The resulting precipitate was burned and oxidized at 850°C f...

Embodiment 2

[0036] An efficient extraction method of high-purity lanthanum oxide, including the following steps:

[0037] (1) Extraction: Mix the lanthanum chloride feed liquid (1.5mol / L) and the extractant at a volume ratio of 1:2.5 for extraction and separation, and perform ultrasonic dispersion for 15 minutes (ultrasonic frequency is 25KHz), and separate after standing, and separate the solid phase Recycling, the organic phase is input to the back extraction procedure;

[0038] The extractant includes the following raw materials in volume percentages: 20% P507, 10% 1,2,5-thiadiazo-3,4-dithiol, and the balance is kerosene;

[0039] (2) Back-extraction: Take the oxalic acid solution (20wt%) 3.0 times the volume of the obtained organic phase to back-extract it at 55°C, and carry out ultrasonic dispersion for 30 min (ultrasonic frequency is 35KHz), at the same time produce precipitation, filter to obtain precipitation;

[0040] (3) Oxidation: The resulting precipitate was burned and oxidized at 85...

Embodiment 3

[0047] An efficient extraction method of high-purity lanthanum oxide, including the following steps:

[0048] (1) Extraction: Mix the lanthanum chloride feed liquid (1.5mol / L) and the extractant at a volume ratio of 1:3.5 for extraction and separation, perform ultrasonic dispersion 10 (ultrasonic frequency 25KHz), separate after standing, and separate the solid phase Recycling, the organic phase is input to the back extraction procedure;

[0049] The extractant includes the following raw materials in volume percentage: 24% P507, 15% 1,2,5-thiadiazo-3,4-dithiol, and the balance is kerosene;

[0050] (2) Back-extraction: Take the oxalic acid solution (20wt%) 4.0 times the volume of the obtained organic phase to back-extract it at 55°C, perform ultrasonic dispersion for 20 minutes (ultrasonic frequency is 35KHz), and produce precipitation at the same time, filter to obtain the precipitate;

[0051] (3) Oxidation: The resulting precipitate was burned and oxidized at 850°C for 14 hours to ...