Method for rapidly identifying partition type of ion adsorption type rare earth ore in field

Abstract

The invention discloses a method for rapidly identifying partition types of ion adsorption type rare earth ores in the field. The method comprises the following steps: analyzing a regional geological background and mineralization conditions; analyzing different rocks by using a handheld XRF (X-Ray Fluorescence) rapid analyzer; taking an ore sample; grinding the sample into powder; adding an ammonium sulfate solution into the powdery sample, stirring, and filtering to leave a soaking solution; dropwise adding a saturated oxalic acid solution into the soaking solution, and filtering again to obtain colorless transparent liquid; analyzing a result; dissolving the sample powder containing the ion adsorption type rare earth in an acid soluble reagent; preparing an EDTA standard solution; adding a proper amount of an ammonia-ammonium chloride buffer solution and a complexing indicator into the sample solution, stirring, and then slowly adding an EDTA (Ethylene Diamine Tetraacetic Acid) standard solution; and determining the rare earth partition type according to the volume and concentration of the consumed EDTA standard solution. According to the method, the ore-bearing property, the ore-bearing position and the rare earth partition type of the rare earth in different lithology can be quickly determined in the field.

Description

Technical Field

[0001] The invention relates to the technical field of geological mineral exploration, and in particular to a method for rapidly identifying the distribution type of ion adsorption rare earth ores in the field. Background Art

[0002] Rare earth elements are called "industrial vitamins" because of 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] The prospecting method for rare earth ores mainly relies on profile measurement, trenching, drilling and other methods to determine the mineralized strata, and to determine whether there is mineralization and the degree of mineralization through sample analysis and test results. This is the basic method currently used. Although this method can effectively determine the distribution type of rare earth ores, it also has obvious disadvantages, such as long test cycle, high labor and testing costs, especially large laboratory workload and long analysis time, and often there is a phenomenon of time lag in providing analysis results. Geologists cannot make timely judgments based on the analysis results to guide field ion adsorption type rare earth prospecting work. Summary of the invention

[0004] The purpose of the present invention is to provide a method for quickly identifying the distribution type of ion adsorption rare earth ore in the field, which can quickly determine the mineralization of rare earths in different strata and lithologies, the mineralization strata and the distribution type of ionic rare earths in the field.

[0005] The above technical objectives of the present invention are achieved through the following technical solutions:

[0006] A method for rapidly identifying the distribution type of ion adsorption type rare earth ore in the field comprises the following steps:

[0007] Step 1: Geological survey: Through the analysis of regional geological background and mineralization conditions, systematically collect regional geological, physical, geochemical, remote sensing and mineral data, clarify the regional strata, structure, magmatic rock and mineral distribution and its outcrop characteristics, 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: Use a handheld XRF rapid analyzer to quickly analyze the fresh surfaces of different rocks in the formation. The instrument will display the rare earth element composition contained in the rock, thereby quickly locking the mineral-bearing stratum;

[0009] Step 3: Sample collection: Continuously collect ore samples from the surface rock strata according to different lithology layers by digging or scraping;

[0010] Step 4: Sample processing: clean the surface impurities of the collected samples, put them in a drying oven to dry, let them cool to room temperature and take them out, wrap the samples with gauze and knock them into pieces, and then use a roller to grind the sample pieces into powder;

[0011] Step 5, extraction: put a certain amount of powdered sample into a container and add an appropriate proportion of ammonium sulfate solution, stir and soak for 30-50 minutes, then filter with filter paper to leave the soaking solution, then drip 2-3 drops of saturated oxalic acid solution into the soaking solution and stir for 30-60 seconds, then filter with filter paper again to obtain a colorless transparent liquid, then shake it well and let it stand for 15-25 minutes;

[0012] Step 6. Result analysis: Samples that produce white flocculent or milky white milk-like phenomena contain ion-adsorbed rare earths. The more violent the reaction phenomenon, the higher the content of ion-adsorbed rare earths. Samples without obvious reactions do not contain ion-adsorbed rare earths.

[0013] Step 7: Dissolving: dissolving the sample powder containing the ion-adsorbed rare earth in an acidic solvent;

[0014] Step 8. Prepare EDTA standard solution: weigh an appropriate amount of disodium ethylenediaminetetraacetate, dissolve it in distilled water and dilute to the corresponding concentration;

[0015] Step 9, titration: first add an appropriate amount of ammonia-ammonium chloride buffer solution to the sample solution and stir, then add the complex indicator and stir, after standing for a period of time, use a burette to slowly add the EDTA standard solution to the sample solution while stirring and observing the change in solution color. When the solution color changes from purple-red to pure blue, the titration endpoint is reached;

[0016] Step 10: Partition type: Calculate the content of rare earth elements in the sample based on the volume and concentration of the consumed EDTA standard solution, and determine the rare earth partition type of the sample based on the ratio of light rare earth and heavy rare earth.

[0017] Further: In step three, the collected ore samples need to be fresh and free of alteration and weathering.

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

[0019] Further: In step 4, the temperature of the drying oven is controlled at 102-107°C, and the drying time is 1.5-2h.

[0020] Further: In step 5, the weight of the sample is 100 g, and the weight of the ammonium sulfate solution is 100-150 g.

[0021] Further: In step seven, the acidic 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 complex indicator is chrome black T.

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

[0025] First, the present invention can quickly determine the mineralization of rare earths in different layers and lithologies, mineralization layers, and distribution types of ionic rare earths in the field;

[0026] Secondly, the present invention can directly collect samples from strata and rocks with high mineral content for analysis and testing, which not only shortens the cycle of sample analysis and testing, but also saves a lot of financial costs and manpower and material resources;

[0027] Thirdly, the present invention can not only determine whether the rare earth in different strata and lithologies has mineralization, but also further determine the distribution type of the rare earth according to the content ratio of the rare earth elements. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is an operation flow chart of the present invention;

[0029] Figure 2 This is a diagram of the field test results of the handheld XRF rapid analyzer of the present invention;

[0030] Figure 3 Mainly, it is a diagram of the solution reaction phenomenon of the sample result analysis of the present invention;

[0031] Figure 4 It is a comparison diagram of samples before and after titration in an embodiment of the present invention;

[0032] Figure 5 It is a comparison table of rock sample results in the embodiment of the present invention. DETAILED DESCRIPTION

[0033] The present invention is further described in detail below in conjunction with the accompanying drawings.

[0034] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by terms such as “upper”, “lower”, “left”, “right”, “front”, “back”, “inside” and “outside” are based on the directions or positional relationships shown in the accompanying drawings and are only for the convenience of describing the present invention and simplifying the description. They do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore should not be understood as a limitation on the present invention.

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

[0036] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "disposed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, a direct connection, or an indirect connection through an intermediate medium, or it can be the internal communication of two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0037] Embodiment 1

[0038] A rapid analysis was performed on the fresh surfaces of three rocks in the Xuanwei Formation, and the contents of yttrium (Y) and neodymium (Nb) were determined.

[0039] Reference Figure 1-5 A method for rapidly identifying the distribution type of ion adsorption type rare earth ore in the field comprises the following steps:

[0040] Step 1: Geological survey: Through the analysis of regional geological background and mineralization conditions, systematically collect regional geological, physical, geochemical, remote sensing and mineral data, clarify the regional strata, structure, magmatic rock and mineral distribution and its outcrop characteristics, analyze the regional mineralization anomaly characteristics and regional climate and geographical environment, and then preliminarily delineate the scope of the work area;

[0041] Step 2: Rock surface analysis: Use a handheld XRF rapid analyzer to quickly analyze the fresh surfaces of different rocks in the formation. The instrument will show that the rare earth element neodymium (Nb) content in the rock is 4000-9000ppm, with a local high of 1.51%, and yttrium (Y) content of 7451ppm, thus quickly locking a specific layer in the Xuanwei formation as a rare earth mineral-bearing layer;

[0042] Step 3: Sample collection: Continuously collect fresh, non-altered and weathered ore samples from the surface rock strata according to different lithology layers by digging or scraping;

[0043] Step 4: Sample processing: clean the surface impurities of the collected samples, then put the samples into a drying oven, control the temperature of the drying oven to 102°C, and dry for 1.5 hours, then let it cool to room temperature and take it out, then wrap the samples with gauze and knock them into pieces, then use a roller to grind the sample pieces into powder;

[0044] Step 5, extraction: put 100g of powdered sample into a container and add 100g of ammonium sulfate solution in an appropriate proportion, stir and soak for 30min, then filter with filter paper to leave the soaking solution; then drip 2 drops of saturated oxalic acid solution into the soaking solution and stir for 30S, then filter with filter paper again to obtain a colorless transparent liquid, then shake it well and let it stand for 15min;

[0045] Step 6. Result analysis: The samples that produce white flocculent or milky white milky phenomena contain ion-adsorbed rare earths. The more violent the reaction phenomenon is, the higher the content of ion-adsorbed rare earths is. The samples without obvious reaction do not contain ion-adsorbed rare earths (Table 1);

[0046] Step 7, dissolving: dissolving the sample powder containing the ion-adsorbed rare earth in an acidic solvent such as hydrochloric acid or nitric acid;

[0047] Step 8. Prepare EDTA standard solution: weigh an appropriate amount of disodium ethylenediaminetetraacetate, dissolve it in distilled water and dilute it to a concentration of 0.01 mol / L;

[0048] 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 complex indicator of chrome black T and stir, after standing for a period of time, use a burette to slowly add EDTA standard solution to the sample solution while stirring and observing the change of solution color, when the solution color changes from purple to pure blue, the titration end point is reached;

[0049] Step 10: Partition type: Calculate the content of rare earth elements in the sample based on the volume and concentration of the consumed EDTA standard solution, and determine the rare earth partition type of the sample based on the ratio of light rare earth and heavy rare earth.

[0050] Embodiment 2

[0051] A rapid analysis was performed on the fresh surfaces of three rocks in the Xuanwei Formation, and the contents of yttrium (Y) and neodymium (Nb) were determined.

[0052] Reference Figure 1-5 A method for rapidly identifying the distribution type of ion adsorption type rare earth ore in the field comprises the following steps:

[0053] Step 1: Geological survey: Through the analysis of regional geological background and mineralization conditions, systematically collect regional geological, physical, geochemical, remote sensing and mineral data, clarify the regional strata, structure, magmatic rock and mineral distribution and its outcrop characteristics, analyze the regional mineralization anomaly characteristics and regional climate and geographical environment, and then preliminarily delineate the scope of the work area;

[0054] Step 2: Rock surface analysis: Use a handheld XRF rapid analyzer to quickly analyze the fresh surfaces of different rocks in the formation. The instrument will show that the rare earth element neodymium (Nb) content in the rock is 4000-9000ppm, with a local high of 1.51%, and yttrium (Y) content of 7451ppm, thus quickly locking a specific layer in the Xuanwei formation as a rare earth mineral-bearing layer;

[0055] Step 3: Sample collection: Continuously collect fresh, non-altered and weathered ore samples from the surface rock strata according to different lithology layers by digging or scraping;

[0056] Step 4: Sample processing: clean the surface impurities of the collected samples, then put the samples into a drying oven, control the temperature of the drying oven to 107°C, and dry for 2 hours, then let them cool to room temperature and take them out, then wrap the samples with gauze and knock them into pieces, then use a roller to grind the sample pieces into powder;

[0057] Step 5, leaching: put 100g of powdered sample into a container and add 150g of ammonium sulfate solution in an appropriate proportion, stir and soak for 50min, then filter with filter paper to leave the soaking solution, then drip 3 drops of saturated oxalic acid solution into the soaking solution and stir for 60S, then filter with filter paper again to obtain a colorless transparent liquid, then shake it well and let it stand for 25min;

[0058] Step 6. Result analysis: Samples that produce white floccules or milky white milk-like phenomena contain ion-adsorbed rare earths. The more violent the reaction phenomenon, the higher the content of ion-adsorbed rare earths in the sample. Samples with no obvious reaction do not contain ion-adsorbed rare earths (Table 2).

[0059] Step 7, dissolving: dissolving the sample powder containing the ion-adsorbed rare earth in an acidic solvent such as hydrochloric acid or nitric acid;

[0060] Step 8. Prepare EDTA standard solution: weigh an appropriate amount of disodium ethylenediaminetetraacetate, dissolve it in distilled water and dilute it to a concentration of 0.01 mol / 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 complex indicator of chrome black T and stir, after standing for a period of time, use a burette to slowly add EDTA standard solution to the sample solution while stirring and observing the change of solution color, when the solution color changes from purple to pure blue, the titration end point is reached;

[0062] Step 10: Partition type: Calculate the content of rare earth elements in the sample based on the volume and concentration of the consumed EDTA standard solution, and determine the rare earth partition type of the sample based on the ratio of light rare earth and heavy rare earth.

[0063] This specific embodiment is only an explanation of the present invention, and it is not a limitation of the present invention. After reading this specification, those skilled in the art can make creative modifications to this embodiment as needed, but as long as it is within the scope of the claims of the present invention, it will be 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 following steps are involved: Step 1: Geological survey: Through the analysis of regional geological background and mineralization conditions, systematically collect regional geological, physical, geochemical, remote sensing and mineral data, clarify the regional strata, structure, magmatic rock and mineral distribution and its outcrop characteristics, analyze the regional mineralization anomaly characteristics and regional climate and geographical environment, and then preliminarily delineate the scope of the work area; Step 2: Rock surface analysis: Use a handheld XRF rapid analyzer to quickly analyze the fresh surfaces of different rocks in the formation. The instrument will display the rare earth element composition contained in the rock, thereby quickly locking the mineral-bearing stratum; Step 3: Sample collection: Continuously collect ore samples from the surface rock strata according to different lithology layers by digging or scraping; Step 4: Sample processing: clean the surface impurities of the collected samples, put them in a drying oven to dry, let them cool to room temperature and take them out, wrap the samples with gauze and knock them into pieces, and then use a roller to grind the sample pieces into powder; Step 5, extraction: put a certain amount of powdered sample into a container and add an appropriate proportion of ammonium sulfate solution, stir and soak for 30-50 minutes, then filter with filter paper to leave the soaking solution, then drip 2-3 drops of saturated oxalic acid solution into the soaking solution and stir for 30-60 seconds, then filter with filter paper again to obtain a colorless transparent liquid, then shake it well and let it stand for 15-25 minutes; Step 6. Result analysis: Samples that produce white flocculent or milky white milk-like phenomena contain ion-adsorbed rare earths. The more violent the reaction phenomenon, the higher the content of ion-adsorbed rare earths. Samples without obvious reactions do not contain ion-adsorbed rare earths. Step 7: Dissolving: dissolving the sample powder containing the ion-adsorbed rare earth in an acidic solvent; Step 8. Prepare EDTA standard solution: weigh an appropriate amount of disodium ethylenediaminetetraacetate, dissolve it in distilled water and dilute to the corresponding concentration; Step 9, titration: first add an appropriate amount of ammonia-ammonium chloride buffer solution to the sample solution and stir, then add the complex indicator and stir, after standing for a period of time, use a burette to slowly add the EDTA standard solution to the sample solution while stirring and observing the change in solution color. When the solution color changes from purple-red to pure blue, the titration endpoint is reached; Step 10: Partition type: Calculate the content of rare earth elements in the sample based on the volume and concentration of the consumed EDTA standard solution, and determine the rare earth partition type of the sample based on the ratio of light rare earth and heavy rare earth.

2. The method for rapid identification of the distribution type of ion adsorption type rare earth ore in the field according to claim 1, characterized in that: In step three, the collected ore samples need to be fresh and free of alteration and weathering.

3. The method for rapid identification of the distribution type of ion adsorption type rare earth ore in the field according to claim 1, characterized in that: In step 4, the temperature of the drying oven is controlled at 102-107° C., and the drying time is 1.5-2 hours.

4. The method for rapid identification of the distribution type of ion adsorption type rare earth ore in the field according to claim 1, characterized in that: In step 5, the weight of the sample is 100 g, and the weight of the ammonium sulfate solution is 100-150 g.

5. The method for rapid identification of 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.

6. The method for rapid identification of the distribution type 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.

7. The method for rapid identification of the distribution type 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 complex indicator is chrome black T.

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