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A method for rapidly decomposing sedimentary rare earth ore

A rare earth ore, sedimentary technology, applied in the analysis of materials, thermal excitation analysis, material excitation analysis, etc., can solve the problem of no better decomposition method of sedimentary rare earth ore, poor air tightness of the sample solution tank, no better, etc. problem, to achieve the effect of good sealing, strong solvent resistance and short use time

Active Publication Date: 2022-03-18
INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at the same time, there are also the following disadvantages: Although the boiling point of PTFE is 327°C, if the heating temperature exceeds 150°C, waxy and soft deformation will occur, and the airtightness of the sample dissolution tank will deteriorate after long-term use (rock mineral analysis • No. Fourth Edition, Volume One, Geological Press, 2011, p205)
[0010] Therefore, it can be seen that there is no better method for quickly decomposing sedimentary rare earth ores in the high-pressure closed sample dissolution technology, especially for the sedimentary rare earth ores in the Bijie-Liupanshui area of ​​Guizhou.

Method used

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  • A method for rapidly decomposing sedimentary rare earth ore

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Weigh 0.050g (accurate to 0.001g) of CJX1# sample into the polyphenylene inner tank of the closed sample dissolver, add 1mL HNO 3 , 3 g NH 4 HF 2 Solid, cover the polyphenylene inner tank lid, put it into the steel sleeve, and tighten the steel sleeve cover.

[0041] 2. Place the sample dissolving device in an oven at 160°C for 1 hour, then rise to 250°C for 9 hours.

[0042] 3. Take it out, open the lid after cooling, take out the inner tank, add 0.25mL H 2 SO 4 , steamed on a hot plate at 220°C to H 2 SO 4 Smoke dry.

[0043] 4. Add 3mL distilled water, 1.25g solid tartaric acid, 2mL (1+1) HCl in sequence, and heat on a hot plate for 15 minutes until the solution is clear.

[0044] 5. Take off the cooling tube and adjust the volume to 25mL. At the same time as a blank test. According to the actual content, dilute different times to determine by ICP-OES / ICP-MS. The measurement results are shown in Table 1.

Embodiment 2

[0046] The operation mode of this embodiment is the same as that of embodiment 1, the difference is that the sample CJX1# is changed to the sample CJX2#. The measurement results are shown in Table 1.

Embodiment 3

[0048] 1. Weigh 1.000g (accurate to 0.001g) of CJX2# sample into the polyphenylene inner tank of the closed sample dissolver, add 2mL HNO 3 , 1 g NH 4 HF 2 Solid, cover the polyphenylene inner tank lid, put it into the steel sleeve, and tighten the steel sleeve cover.

[0049] 2. Place the sample dissolving device in an oven at 150°C for 2 hours, then raise it to 240°C for 11 hours.

[0050] 3. Take it out, open the lid after cooling, take out the inner tank, add 0.5mL H 2 SO 4 , steamed on a hot plate at 200°C to H 2 SO 4 Smoke dry.

[0051] 4. Add 2mL of distilled water, 1.75g ​​of solid tartaric acid, and 3mL of (1+1) HCl in sequence, and heat on a hot plate for 10 minutes until the solution is clear.

[0052] 5. Take off the cooling tube and adjust the volume to 25mL. At the same time as a blank test. According to the actual content, dilute different times to determine by ICP-OES / ICP-MS. The measurement results are shown in Table 1.

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Abstract

The present invention proposes a novel method for quickly decomposing sedimentary rare earth ores for specific sedimentary clay-type rare earth ores in the Bijie-Liupanshui area of ​​Guizhou, that is, high-strength polyphenylene polymer engineering plastics are used as the material for the inner tank for digestion. NH with high boiling point 4 HF 2 Instead of HF, use NH 4 HF 2 and HNO 3 Perform a high-pressure closed digestion program at 240-250 °C. Digest solution with 0.25~0.5mL H 2 SO 4 Catching acid to destroy rare earth fluorides, using 5% HCl~5% tartaric acid as the dissolution medium, realized the rapid and complete decomposition of rare earth, Zr, and Nb in sedimentary rare earth ores. The decomposition effect of this method on zircon and rutile in sedimentary rare earth ores in Bijie-Liupanshui area, Guizhou Province is equivalent to that of the closed polytetrafluoroethylene digestion method, but the temperature used is higher, the pressure is higher, and the time is shortened by nearly 2 / 3, which reflects It has the advantages of fast, efficient, green and energy saving.

Description

technical field [0001] The invention belongs to the technical field of rock ore analysis sample pretreatment, in particular to a method for rapidly decomposing sedimentary rare earth ores. Background technique [0002] The Bijie-Liupanshui area in Guizhou is an important energy and mineral resource base in southern my country, and the area is rich in new-type three-rare mineral resources represented by sedimentary rare earth ores. According to the results of previous exploration and research, the total amount of rare earths and associated Nb, Zr and other elements have been enriched to a relatively high degree, and the potential for development and utilization is huge. The mineral composition of this type of rare earth ore is mainly kaolinite, and contains limonite, a small amount of rutile, and accessory minerals such as zircon and quartz. Most of the rare earths exist in kaolinite and iron oxides in the form of isomorphism. Accurate and rapid determination of rare earth,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N1/44G01N21/73G01N27/626C22B3/44G01N27/62
CPCG01N1/28G01N1/44G01N21/73G01N27/62C22B3/44Y02P10/20
Inventor 邵坤惠博李可及龚大兴
Owner INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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