Thermal decomposition synthesis method of potassium fluotantalate

A technology of potassium fluorotantalate and potassium fluoride is applied in the field of preparation of potassium fluorotantalate, which can solve the problems of complicated operation process and high equipment requirements, and achieve the effects of low carbon content, simple operation and low cost.

Inactive Publication Date: 2012-07-18
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Abstract
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  • Application Information

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Problems solved by technology

Add KCl to the starting liquid, cool it to 40°C or lower at a rate of less than 15°C per hour, and produce potassium fluorotantalate precipitation. The concentration of HF acid in the starting liquid should not exceed 20%. This method can be directly Obtain high-purity, large-particle K 2 TaF 7 Crystal, but the operation process is complicated, HF acid is a strong acid, and requires high equipment

Method used

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  • Thermal decomposition synthesis method of potassium fluotantalate
  • Thermal decomposition synthesis method of potassium fluotantalate
  • Thermal decomposition synthesis method of potassium fluotantalate

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Experimental program
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Embodiment 1

[0024] Accurately weigh 7.2658g potassium fluoride (KF 2.12H 2 O, Sinopharm Chemical Reagent Co., Ltd., 99.0%), 10.7164g ammonium bifluoride (Sinopharm Chemical Reagent Co., Ltd., 98.0%) and 10.7609g tantalum hydroxide (Jiujiang Jinxin Nonferrous Metals Co., Ltd., 99.99%), w(Ta 2 o 5)=77.15%), put the three in a polytetrafluoroethylene mortar and grind them thoroughly, add 6mL of 99.5% methanol to make the mixture into a paste, in order to achieve full mixing, after grinding for 4-5 hours under the infrared lamp Evaporation of methanol and water yielded a homogeneously dispersed potassium fluorotantalate precursor. The precursor was calcined at 150°C, 200°C and 250°C for 180min. attached by figure 1 It can be seen that at 150 ° C, a single-phase potassium fluorotantalate crystal is obtained, but the K obtained at this temperature 2 TaF 7 The degree of crystallinity is not high. The K obtained when the calcination temperature is 200°C 2 TaF 7 , its XRD peak is strong an...

Embodiment 2

[0025] Embodiment 2 (comparative example):

[0026] Accurately weigh 7.5316g potassium fluoride (KF 2.12H 2 (2), 11.1084g ammonium bifluoride and 8.6057g tantalum pentoxide (Jiujiang Jinxin Nonferrous Metals Co., Ltd., 99.99%), the three are placed in a polytetrafluoroethylene mortar and fully ground, and then 4mL99.5% methanol will The mixture is made into a paste to achieve thorough mixing, and after grinding for 4-5 hours under an infrared lamp, methanol and water are evaporated to obtain a homogeneously dispersed precursor of potassium fluorotantalate. The precursor was calcined at 150°C, 200°C and 250°C for 180min. attached by figure 2 It can be seen that the single-phase K 2 TaF 7 , the K 2 TaF 7 , the product contains K 3 TaOF 6 . The trace amount of carbon in the sample was measured with a coulometric carbon meter, and the measured carbon content was 5 ppm.

Embodiment 3

[0028] Accurately weigh 7.2658g potassium fluoride (KF 2.12H 2 O, Sinopharm Chemical Reagent Co., Ltd., 99.0%, AR), 10.7164g ammonium bifluoride and 10.7609g tantalum hydroxide, the three are fully ground in a polytetrafluoroethylene mortar, and then 6mL99.5% methanol is added to the mixture Make into a paste to achieve thorough mixing, grind for 4-5 hours under an infrared lamp, evaporate methanol and water to obtain a uniformly dispersed precursor of potassium fluorotantalate. The precursor was calcined at 200°C for 15min, 30min, 60min, 90min and 120min, respectively. attached by image 3 It can be seen that the single-phase K 2 TaF 7 . The trace amount of carbon in the sample was measured with a coulometric carbon meter, and the measured carbon content was 6ppm.

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Abstract

The invention relates to a thermal decomposition preparation method of potassium fluotantalate. The method is simple and convenient in operation, low in cost and high in direct yield, all volatile components volatilize, and the problem of carbon impurities is solved. Hydrogen tantalum oxide or tantalum pentoxide, potassium fluoride and ammonium bifluoride serve as raw materials, small amount of carbinol, ethanol or water serves as solvent, and a precursor is obtained through full grinding and drying. The prepared precursor is roasted at the temperatures of 150 DEG C, 200 DEG C and 250 DEG C for 3 hours, wherein the precursor is roasted at the temperature of 200 DEG C for respectively 15 minutes, 30 minutes, 60 minutes, 90 minutes and 120 minutes. Influences of the roasting temperature and the roasting time on synthesis of the potassium fluotantalate are investigated. The research shows that K2TaF7 crystals can be obtained by roasting the precursor at the temperature of 200 DEG C for 15 minutes, and the K2TaF7 crystals have high relative crystallinity and small particle sizes.

Description

technical field [0001] The invention relates to a preparation method of potassium fluorotantalate. The thermal decomposition process and equipment are simple, and high-purity potassium fluorotantalate can be synthesized. Background technique [0002] Tantalum production technology has a history of about 80 years. Developments included liquid-liquid extraction instead of fractional precipitation and sodium reduction instead of electrolysis. However, tantalum technology is still based on the addition of potassium fluorotantalate-K 2 TaF 7 (commercial name is Potassium Salt) as an intermediate raw material based on. Usually niobium tantalum ore is dissolved in HF acid solution, separated and purified by liquid-liquid extraction with organic solvent, and the purified solution is used to produce small particle K 2 TaF 7 Crystal, metal tantalum was prepared by metal sodium or magnesium thermal reduction of potassium fluorotantalate. [0003] Potassium fluorotantalate, as the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G35/02
Inventor 姜恒林翠华宫红王锐苏婷婷
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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