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Method for rapidly decomposing sedimentary rare earth ore

A rare earth ore and sedimentary technology, which is applied in the direction of material analysis, thermal excitation analysis, material excitation analysis, etc., can solve the problem of no better decomposition method for sedimentary rare earth ore, poor air tightness of dissolution tank, waxy soft deformation, etc. problems, to achieve the effect of good sealing, accelerated dissolution, and increased reaction temperature

Active Publication Date: 2019-12-20
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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  • Method for rapidly decomposing sedimentary rare earth ore

Examples

Experimental program
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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 1mLHNO 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 in the polyphenylene inner tank of the closed sample dissolver, add 2mLHNO 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 invention provides a novel method for rapidly decomposing sedimentary rare earth ore specific to the sedimentary rare earth ore in a Bijie-Liupanshui area in Guizhou, namely high-strength polyhenylene macromolecular engineering plastic is taken as a digestion inner tank material, HF is replaced by NH4HF2 with a high boiling point, and NH4HF2 and HNO3 are adopted for performing a high pressureclosed vessel digestion process at the temperature of 240-250 DEG C. Digestion solution adopts 0.25-0.5mL H2SO4 for removing acid and destroying rare earth fluorides, and 5% HCl and 5% tartaric acid are taken as dissolving mediums, thus rapid and complete decomposition on rare earth, Zr and Nb in the sedimentary rare earth ore is realized. The decomposition effect, on zircons and rutile in the sedimentary rare earth ore in the Bijie-Liupanshui area in Guizhou, of the method provided by the invention is equivalent to that of a polytetrafluoroethylene closed vessel digestion method, but temperature used is higher, pressure is higher, time is shortened by about 2 / 3, and the advantages of speediness, high efficiency, environmentally friendliness and energy conservation are embodied.

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 Applications(China)
IPC IPC(8): G01N1/28G01N1/44G01N21/73G01N27/62C22B3/44
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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