A method for rapidly identifying ion adsorption type rare earth ore distribution type in the field

Abstract

The application discloses a method for rapidly identifying ion-adsorption type rare earth ore distribution type in the field, which comprises the following steps: analyzing regional geological background and ore-forming conditions; analyzing different rocks by using a handheld XRF rapid analyzer; taking ore samples; grinding the samples into powder; adding an ammonium sulfate solution into the powdered samples, stirring and filtering to obtain a soaking solution; adding saturated oxalic acid solution dropwise into the soaking solution, filtering again to obtain a colorless transparent liquid; analyzing the result; dissolving sample powder containing ion-adsorption type rare earth in an acidic solution; preparing an EDTA standard solution; adding an appropriate amount of ammonia-ammonium chloride buffer solution and a complexing indicator into the sample solution, stirring, then slowly adding the EDTA standard solution; and determining the rare earth distribution type according to the volume and concentration of the consumed EDTA standard solution. The application can rapidly determine the ore-bearing nature, ore-bearing horizon and rare earth distribution type of rare earth in different lithology in the field.

Description

Technical Field

[0001] This invention relates to the field of geological and mineral exploration technology, and in particular to a method for rapidly identifying the distribution type of ion-adsorption type rare earth minerals in the field. Background Technology

[0002] Rare earth elements are known as "industrial vitamins" due to their wide applications in many fields such as national defense, aerospace, special materials, metallurgy, energy and agriculture. In recent years, the rapid development of aerospace, new energy and new materials has made rare earths a key strategic resource.

[0003] Rare earth prospecting methods mainly rely on methods such as profile surveying, trenching, and drilling to determine ore-bearing strata. The presence and degree of ore-bearing are then determined through sample analysis and testing. This is the basic method currently in use. Although this method can effectively determine the distribution type of rare earth minerals, it also has significant drawbacks, such as long testing cycles, high labor and testing costs, especially the large workload and long analysis time in the laboratory, which often results in a time lag in providing analysis results. Geologists cannot make timely judgments based on the analysis results to guide field ion adsorption rare earth prospecting. Summary of the Invention

[0004] The purpose of this invention is to provide a method for rapidly identifying the distribution type of ion-adsorption rare earth minerals in the field, which can quickly determine the mineralization of rare earths, the mineral-bearing strata, and the distribution type of ion-adsorption rare earths in different strata and lithologies in the field.

[0005] The above-mentioned technical objective of the present invention is achieved through the following technical solution:

[0006] A method for rapid field identification of ion-adsorption type rare earth mineral distribution types includes the following steps:

[0007] Step 1: Geological Survey: Through the analysis of the regional geological background and metallogenic conditions, systematically collect regional geological, physical, geochemical, remote sensing and mineral data, clarify the distribution and outcrop characteristics of regional strata, structures, igneous rocks and minerals, analyze the regional mineralization anomaly characteristics and regional climate and geographical environment, and then preliminarily delineate the scope of the work area.

[0008] Step 2, Rock Surface Analysis: Using a handheld XRF rapid analyzer, the fresh surfaces of different rocks in the strata are quickly analyzed. The instrument will display the rare earth element composition contained in the rocks, thereby quickly locating the ore-bearing strata.

[0009] Step 3, Sample Collection: Ore samples are continuously collected from the surface rock strata according to different lithologies by excavation or scraping.

[0010] Step four, sample processing: the surface impurities of the collected sample are cleaned, then the sample is placed in a drying oven for drying, then it is cooled to room temperature and taken out, then the sample is wrapped with gauze and knocked into pieces, then the sample pieces are ground into powder using a mortar;

[0011] Step five, leaching: a certain amount of powdered sample is placed in a container and an appropriate proportion of ammonium sulfate solution is added, stirred and soaked for 30-50 min, then filtered with filter paper to leave the soaking solution, then 2-3 drops of saturated oxalic acid solution are added to the soaking solution and stirred for 30-60 s, then filtered again with filter paper to obtain a colorless transparent liquid, then it is shaken and left to stand for 15-25 min;

[0012] Step six, result analysis: samples that produce white flocculent or milky white milk-like phenomena contain ion-adsorbed rare earths, the more intense the reaction phenomenon, the higher the content of ion-adsorbed rare earths in the sample, and samples with no obvious reaction do not contain ion-adsorbed rare earths;

[0013] Step seven, dissolution: the sample powder containing ion-adsorbed rare earths is dissolved in an acidic dissolving reagent;

[0014] Step eight, preparation of EDTA standard solution: an appropriate amount of disodium ethylenediaminetetraacetate is dissolved in distilled water and diluted to the corresponding concentration;

[0015] Step nine, titration: an appropriate amount of ammonia-ammonium chloride buffer solution is added to the sample solution and stirred, then a complexing indicator is added and stirred, after standing for a period of time, EDTA standard solution is slowly added to the sample solution using a burette while stirring and observing the color change of the solution, and when the solution color changes from purple red to pure blue, the titration endpoint is reached;

[0016] Step ten, partition type: according to the volume and concentration of the consumed EDTA standard solution, the content of rare earth elements in the sample is calculated, and according to the proportion of light rare earths and heavy rare earths, the rare earth partition type of the sample is determined.

[0017] Further: in step three, the collected ore sample needs to be fresh and free of alteration weathering.

[0018] By adopting the above technical scheme, the accuracy of the sample analysis result can be improved.

[0019] Further: in step four, the temperature of the drying oven is controlled at 102-107℃, and the drying time is 1.5-2h.

[0020] Further: in step five, the weight of the sample is 100g, and the ammonium sulfate solution is 100-150g.

[0021] Further, in step seven, the acid solution is hydrochloric acid or nitric acid.

[0022] Further, in step eight, the dilution concentration of the EDTA standard solution is 0.01 mol / L.

[0023] Further, in step nine, the PH value of the ammonia-ammonium chloride buffer solution is 10, and the complexing indicator is chrome black T.

[0024] In summary, the present application has the following beneficial effects:

[0025] Firstly, the present application can quickly determine the ore-bearing nature, ore-bearing horizon and ion-type rare earth element partition type in different horizons and different lithologies in the field.

[0026] Secondly, the present application can directly collect samples from strata and rocks with high ore-bearing nature for analysis and testing, which not only shortens the sample analysis and testing period, but also saves a large amount of fund cost and manpower and material resources.

[0027] Thirdly, the present application can not only determine whether the rare earth elements in different horizons and different lithologies have ore-bearing nature, but also further determine the partition type of rare earth elements according to the content ratio of rare earth elements. DETAILED DESCRIPTION

[0028] Figure 1 is the operation flowchart of the present application;

[0029] Figure 2 is the field test result graph of the handheld XRF rapid analyzer of the present application;

[0030] Figure 3 is mainly the solution reaction phenomenon graph of sample result analysis of the present application;

[0031] Figure 4 is the control graph of the sample before and after titration in the embodiment of the present application;

[0032] Figure 5 is the rock sample result control table in the embodiment of the present application. DETAILED DESCRIPTION

[0033] The present application will be further described in detail below with reference to the accompanying drawings.

[0034] In the description of the present application, it should be understood that the terms "upper", "lower", "left", "right", "front", "back", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application.

[0035] In addition, the terms "horizontal", "vertical" and the like do not mean that the components must be absolutely horizontal or vertical, but can be slightly inclined. For example, "horizontal" only means that it is more horizontal than "vertical", and does not mean that the structure must be completely horizontal, but can be slightly inclined.

[0036] In the description of the present application, it should be noted that, unless otherwise specified and limited, the terms "arrangement", "connection", "connection" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, it can be directly connected, or indirectly connected through an intermediate medium, it can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0037] Example one

[0038] The fresh surface of three rocks in Xuanwei group strata is analyzed quickly to determine the content of yttrium (Y) and neodymium (Nb) elements.

[0039] Reference Figures 1-5 A method for quickly identifying the distribution type of ion adsorption type rare earth ore in the field, comprising the following steps:

[0040] Step one, geological investigation: through the analysis of regional geological background and ore-forming conditions, the regional geology, physical, geochemical, remote sensing and mineral resources and other data are collected systematically, the regional strata, structure, magmatic rock and mineral distribution and its outcrop characteristics are clarified, the regional mineralization anomaly characteristics and regional climate and geography are analyzed, and then the working area range is preliminarily delineated;

[0041] Step two, rock surface analysis: the fresh surface of different rocks in the strata is analyzed quickly by using handheld XRF rapid analyzer, the instrument will show that the content of rare earth element neodymium (Nb) in the rock is 4000-9000ppm, locally up to 1.51%, and the content of yttrium (Y) is 7451ppm, so as to quickly lock the certain layer of Xuanwei group strata as rare earth ore-bearing layer;

[0042] Step three, sample collection: fresh and unaltered weathered ore samples are continuously collected from the surface rock layer according to different lithology by digging or scraping;

[0043] Step four, sample processing: the surface impurities of the collected sample are cleaned, then the sample is put into a drying box, the temperature of the drying box is controlled at 102℃, and dried for 1.5h, then cooled to room temperature and taken out, then the sample is wrapped with gauze and knocked into pieces, then the sample pieces are ground into powder with a mortar;

[0044] Step five, leaching: 100g of powdered sample is placed in a container and an appropriate proportion of 100g ammonium sulfate solution is added. After stirring and soaking for 30min, the soaking solution is filtered using filter paper; then 2 drops of saturated oxalic acid solution are added to the soaking solution and stirred for 30S. The colorless transparent liquid is filtered again using filter paper, then shaken and left to stand for 15min;

[0045] Step six, result analysis: samples that produce white flocculent or milky white milk phenomenon contain ion-adsorbed rare earths. The more intense the reaction phenomenon, the higher the content of ion-adsorbed rare earths in the sample. Samples that do not show obvious reaction do not contain ion-adsorbed rare earths (Table 1);

[0046] Step seven, dissolution: the sample powder containing ion-adsorbed rare earths is dissolved in an acidic solution of hydrochloric acid or nitric acid;

[0047] Step eight, preparation of EDTA standard solution: an appropriate amount of ethylenediaminetetraacetic acid disodium salt is dissolved in distilled water and diluted to a concentration of 0.01mol / L;

[0048] Step nine, titration: an appropriate amount of ammonia-ammonium chloride buffer solution with a pH of 10 is first added to the sample solution and stirred, then a complexing indicator of chrome black T is added and stirred. After standing for a period of time, the EDTA standard solution is slowly added to the sample solution using a burette while stirring and observing the color change of the solution. When the solution color changes from purple red to pure blue, the titration endpoint is reached;

[0049] Step ten, partition type: according to the volume and concentration of the consumed EDTA standard solution, the content of rare earth elements in the sample is calculated, and according to the proportion of light rare earth and heavy rare earth, the rare earth partition type of the sample is determined.

[0050] Example two

[0051] The fresh surface of three rocks in the Xuanwei group strata is analyzed quickly to determine the content of yttrium (Y) and neodymium (Nb) elements.

[0052] Reference Figures 1-5 A method for quickly identifying the partition type of ion-adsorbed rare earth ore in the field, comprising the following steps:

[0053] Step one, geological investigation: through analysis of regional geological background and ore-forming conditions, systematically collect regional geological, physical, geochemical, remote sensing and mineral resources data, clarify regional strata, structure, magmatic rock and mineral distribution and their outcrop characteristics, analyze regional mineralization anomaly characteristics and regional climate and geography, and then preliminarily delineate the working area range;

[0054] Step two, rock surface analysis: use a handheld XRF rapid analyzer to quickly analyze the fresh surface of different rocks in the stratum, the instrument will show that the rare earth element neodymium (Nb) content in the rock is 4000-9000ppm, locally up to 1.51%, yttrium (Y) content 7451ppm, so as to quickly lock a certain layer of xuanwei group stratum as rare earth ore-bearing layer;

[0055] Step three, sample collection: by digging or scraping, the fresh unaltered weathered ore samples are continuously collected from the rock layer on the ground according to different lithology;

[0056] Step four, sample processing: clean the surface impurities of the collected sample, then put the sample into a drying box, control the temperature of the drying box to 107℃, and dry for 2h, then cool it to room temperature and take it out, then wrap the sample with gauze and knock it into pieces, then use a mill to grind the sample pieces into powder;

[0057] Step five, leaching: put 100g of powdered sample into a container and add appropriate proportion of 150g ammonium sulfate solution, stir and soak for 50min, then filter with filter paper to leave the soaking solution, then add 3 drops of saturated oxalic acid solution to the soaking solution and stir for 60S, then filter again with filter paper to obtain a colorless transparent liquid, then shake it well and stand for 25min;

[0058] Step six, result analysis: the sample producing white flocculent or milky white milk phenomenon contains ion adsorption type rare earth, the more intense the reaction phenomenon, the higher the content of ion adsorption type rare earth in the sample, and the sample without obvious reaction does not contain ion adsorption type rare earth (Table 2).

[0059] Step seven, dissolution: dissolve the sample powder containing ion adsorption type rare earth in an acidic solution of hydrochloric acid or nitric acid;

[0060] Step eight, preparation of EDTA standard solution: weigh an appropriate amount of disodium ethylenediaminetetraacetate and dissolve it in distilled water, and dilute it to a concentration of 0.01mol / L;

[0061] Step nine, titration: first add an appropriate amount of ammonia-ammonium chloride buffer solution with a pH value of 10 to the sample solution and stir, then add a complexing indicator of chrome black T and stir, stand for a period of time, then slowly add EDTA standard solution to the sample solution using a burette while stirring and observing the color change of the solution, when the solution color changes from purple red to pure blue, the titration endpoint is reached;

[0062] Step ten, partition type: according to the volume and concentration of the consumed EDTA standard solution, the content of rare earth elements in the sample is calculated, and according to the proportion of light rare earth and heavy rare earth, the rare earth partition type of the sample is determined.

[0063] The specific embodiments are only illustrative of the present application, and are not intended to limit the present application. Those skilled in the art can make creative contributions to the embodiments according to the needs after reading the specification, and as long as the embodiments are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A method for rapidly identifying the distribution type of ion-adsorption type rare earth ore in the field, characterized in that, The method comprises the following steps: Step one, geological survey: through the analysis of regional geological background and metallogenic conditions, the regional geology, physics, geochemical exploration, remote sensing and mineral resources data are collected systematically, the regional strata, structure, magmatic rock and mineral distribution and its outcrop characteristics are clarified, the regional mineralization anomaly characteristics and regional climate and geographical environment are analyzed, and then the working area range is preliminarily delineated; Step two, rock surface analysis: the fresh surface of different rocks in the stratum is analyzed quickly by using a handheld XRF rapid analyzer, and the rare earth element composition contained in the rock is displayed on the instrument, so that the ore-bearing layer is quickly locked; Step three, sample collection: the fresh and unweathered ore samples are continuously collected from the surface stratum by digging or scraping according to different lithology; Step four, sample processing: the surface impurities of the collected sample are cleaned, then the sample is placed in a drying box for drying, and then it is cooled to room temperature and taken out, then the sample is wrapped with gauze and knocked into pieces, then the sample pieces are ground into powder using a mortar; Step five, leaching: a certain amount of powdered sample is placed in a container and an appropriate proportion of ammonium sulfate solution is added, stirred and soaked for 30-50 min, then filtered with filter paper to leave the soaking solution, then 2-3 drops of saturated oxalic acid solution are added to the soaking solution and stirred for 30-60 s, then filtered again with filter paper to obtain a colorless transparent liquid, then shake it evenly and stand for 15-25 min; Step six, result analysis: the sample containing ion adsorption type rare earth elements shows white flocculent or milky white milk phenomenon, the more intense the reaction phenomenon, the higher the content of ion adsorption type rare earth elements in the sample, and the sample without obvious reaction does not contain ion adsorption type rare earth elements; Step seven, dissolution: the sample powder containing ion adsorption type rare earth elements is dissolved in an acidic solution; Step eight, preparation of EDTA standard solution: a proper amount of disodium ethylenediaminetetraacetate is dissolved in distilled water and diluted to the corresponding concentration; Step nine, titration: an appropriate amount of ammonia-ammonium chloride buffer solution is added to the sample solution and stirred, then a complexing indicator is added and stirred, after standing for a period of time, EDTA standard solution is slowly added to the sample solution using a burette while stirring and observing the color change of the solution, and when the solution color changes from purple red to pure blue, the titration end point is reached; Step ten, partition type: according to the volume and concentration of the consumed EDTA standard solution, the content of rare earth elements in the sample is calculated, and according to the proportion of light rare earth and heavy rare earth, the rare earth partition type of the sample is determined.

2. The method for rapidly identifying the distribution pattern of ion-adsorption type rare earth ore in the field according to claim 1, characterized in that: In step four, the temperature of the drying box is controlled at 102-107℃, and the drying time is 1.5-2h.

3. The method for rapidly identifying the distribution pattern of ion-adsorption type rare earth ore in the field according to claim 1, characterized in that: In step five, the weight of the sample is 100g, and the ammonium sulfate solution is 100-150g.

4. The method for rapidly identifying the distribution type of ion-adsorption type rare earth ore in the field according to claim 1, characterized in that: In step seven, the acidic solution is hydrochloric acid or nitric acid.

5. The method for rapidly identifying the distribution pattern of ion-adsorption type rare earth ore in the field according to claim 1, characterized in that: In step eight, the dilution concentration of the EDTA standard solution is 0.01 mol / L.

6. The method for rapidly identifying the distribution pattern of ion-adsorption type rare earth ore in the field according to claim 1, characterized in that: In step nine, the pH value of the ammonia-ammonium chloride buffer solution is 10, and the complexing indicator is chrome black T.

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