A method for identifying multiple types of niobium minerals

Abstract

The present invention discloses a method for identifying multiple types of niobium minerals. The method uses the obtained pure niobium minerals and their associated minerals as research objects; uses rock and mineral identification methods to accurately determine the types of minerals; uses light microscopy, electron microscopy, X-ray scanning and other means to conduct conventional mineral identification and component analysis on niobium iron ore, niobium iron rutile, etc.; determines the solubility of the minerals, screens reagents, and determines the analysis process; through microscopic observation, finds out the obvious similarities and differences of the microchemical reactions of each mineral based on the dissolution state, chemical reaction phenomenon, precipitation characteristics, optical properties, etc. of pure mineral particles. Through the microchemical analysis of niobium-containing minerals in Bayan Obo, a microchemical analysis method for quickly identifying niobium minerals is found, providing support for the industrialization of niobium resources and the rapid acquisition of niobium mineral data.

Description

Technical Field

[0001] The invention relates to the field of rock and mineral identification, and in particular to a rock and mineral identification method for identifying multiple types of niobium minerals. Background Art

[0002] Mineral microscopic chemical analysis (Microchemical analysis), also known as microanalysis, is a special rock and mineral analysis and identification method for qualitative determination of the chemical composition of minerals. This method places mineral powder on a glass slide to dissolve or melt it with a flux, adds identification reagents, and uses a microscope to observe the morphology, color, and optical properties of the reaction products (crystals, residues, or precipitates) to determine whether a certain element exists in the mineral. This method is simple, rapid, and relatively accurate, and requires a small amount of mineral samples and reagents. It has a strong targeting effect on certain minerals that cannot be normally identified by the naked eye under a microscope. Microscopic chemical identification is different from conventional chemical analysis methods. Conventional chemical analysis aims at quantification. Although microchemical identification is based on the chemical reaction phenomenon between substances, it takes mineral qualitative identification as the primary goal, aiming to broaden the analytical methods in the process of rock and mineral identification and rock naming of complex minerals.

[0003] Microscopic chemical analysis methods were introduced into China in the late 1960s. Academician Meng Xianmin, a famous geologist and ore deposit scientist, pioneered and laid the foundation for the theory of mineral microchemical identification in my country. Later, Professor Xu Chunfang of Jilin University, Professor Luo Minghui of Hunan University, and Zhong Zhicheng of Hunan Institute of Geology all conducted research on microchemical analysis of some common metal elements. Due to the popularity of a variety of emerging high-precision analytical and detection methods in recent years, microchemical analysis has not been studied in depth. The introduction of the concept of miniaturized quantitative analysis and identification of minerals has provided new ideas for the rapid identification of niobium-containing minerals in Bayan Obo. Moreover, micro-area identification and analysis methods such as high-power microscopes and scanning electron microscopes only conduct energy spectrum analysis on the surface of minerals, which is slightly less targeted and makes it difficult to quickly identify niobium-containing minerals. Therefore, in the analysis and research of niobium mineral types, it is very necessary to explore a set of relatively simple and accurate microchemical analysis methods.

[0004] The properties of niobium minerals are the basis for the comprehensive utilization of niobium resources and provide technical support for the industrialization of niobium. Many aspects of niobium resource utilization research require rapid acquisition of niobium mineral property data and accurate identification of niobium minerals. Due to the complexity and diversity of niobium-containing minerals in Bayan Obo, there is currently no easy and fast identification method. Therefore, it is very necessary to find a practical, effective and short-term niobium mineral identification method through research. Summary of the invention

[0005] The purpose of the present invention is to provide a method for identifying multiple types of niobium minerals. This method aims to solve the problem of identifying fine niobium minerals in the niobium beneficiation technology in Bayan Obo, which has long been a problem. It strives to provide a fast and easy identification method for geological research and mineral research in Bayan Obo, and to provide a fast and accurate method for identifying niobium-containing minerals for the research and optimization of niobium beneficiation technology and industrial applications. The purpose is to find a micro-analysis method for quickly identifying niobium minerals through micro-analysis of niobium-containing minerals in Bayan Obo, so as to provide support for the industrialization of niobium resources and the rapid acquisition of niobium mineral data.

[0006] This solution aims to solve the following problems:

[0007] The microchemical analysis of niobium-containing minerals in Bayan Obo was studied to find a microchemical analysis method for quickly identifying niobium minerals, providing support for the industrialization of niobium resources and the rapid acquisition of niobium mineral data.

[0008] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0009] The present invention provides an ore and rock identification method for identifying multiple types of niobium minerals, comprising:

[0010] (1) Microchemical Identification of Niobium Iron Ore

[0011] The specific steps include:

[0012] (1.1) Place an appropriate amount of sample powder on a coverslip and select under a microscope;

[0013] (1.2) After adding an appropriate amount of phosphoric acid to dissolve most of the "impurity minerals", the remaining solid matter is heated and melted with an appropriate amount of Na2CO3 to observe its reaction:

[0014] If melting decomposition occurs, continue to add sodium peroxide and dilute sulfuric acid solution to observe the reaction phenomenon. If a light yellow precipitate appears and the precipitate disappears after adding phosphoric acid solution again, it proves that it contains a certain amount of Fe 3+ cation;

[0015] If orange-red or orange-yellow precipitate is also present, it indicates that the sample particles contain a certain amount of Ti 2+ Cations, the color of this part of the precipitation is related to Ti 2+ Proportional to the content;

[0016] (1.3) For the part that does not decompose after melting with Na2CO3, add appropriate amount of tannic acid and ascorbic acid and observe the reaction phenomenon. If a light yellow precipitate is produced, add a certain amount of zinc powder for reduction. If the precipitate turns into an orange-red precipitate, it proves that the sample contains Nb 5+ cation;

[0017] If all of the above phenomena occur, it proves that the sample contains Fe 3+ 、T i 2+ and Nb 5+ , otherwise it means that the sample contains a certain amount of niobium iron rutile mineral;

[0018] (2) Microchemical Identification of Niobium Iron Rutile

[0019] The specific steps include:

[0020] (2.1) Take an appropriate amount of sample powder and place it on a cover glass. First, select it under a microscope (because niobium minerals are all opaque minerals, transparent minerals should be screened out first to improve the success rate of the experiment);

[0021] (2.2) After adding an appropriate amount of phosphoric acid to dissolve most of the "impurity minerals", the remaining solid matter is heated and melted with an appropriate amount of Na2CO3 to observe its reaction:

[0022] If melting decomposition occurs, add appropriate amount of distilled water to dilute, and then add appropriate amount of tannic acid and ascorbic acid to observe its reaction:

[0023] If a light yellow precipitate or sediment appears and turns into an orange-red precipitate after standing, it proves that there is Fe in the sample particles. 3+ and Nb 5+ , it proves that there are niobium iron ore particles in the sample, and tannic acid is added again, and the semi-quantitative analysis of niobium iron ore can be carried out through the color change reaction of the precipitate;

[0024] If no light yellow precipitate appears, but a purple-black precipitate appears, it proves that the sample contains Fe. 3+ , Mn 2+ , or prove the presence of manganese-containing ferromanganese or ferromanganese in the sample;

[0025] (2.3) If melting decomposition does not occur and no light yellow precipitate appears, but a brown precipitate appears, it proves that the sample particles are common iron minerals.

[0026] Furthermore, in the steps (1.1) and (2.1), the purpose of the microscopic selection is that since niobium minerals are all opaque minerals, transparent minerals are first screened out in order to improve the success rate of the experiment.

[0027] Furthermore, conventional mineral identification and composition analysis were carried out on niobium iron ore and niobium iron rutile using optical microscopy, electron microscopy and X-ray scanning.

[0028] Furthermore, the solubility of the minerals is determined, reagents are screened, and the analysis process is determined.

[0029] Furthermore, through microscopic observation, the obvious similarities and differences of each mineral micronization reaction are found out according to the dissolution state, chemical reaction phenomenon, precipitation characteristics and optical properties of pure mineral particles.

[0030] Compared with the prior art, the beneficial technical effects of the present invention are:

[0031] Find out the rapid microchemical analysis and identification methods for niobium-containing minerals such as columbite (Fe, Mn) Nb2O6, niobium rutile (Ti, Nb, Fe) O2, calcite (Ce, Nd)(Ti, Nb) 2O6, chalcanthite (Ca, Na, Ce) 2(Nb, Ti, Ta) 2O6(F, OH), and columbite (Ca, Ce)(Nb, Ti, Fe) 2(O, OH, F) 6. By finding the rapid microchemical analysis methods for identifying niobium minerals, we can provide support for the industrialization of niobium resources and the acquisition of niobium mineral data for scientific research. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] The present invention will be further described below in conjunction with the accompanying drawings.

[0033] Figure 1 It is the technical roadmap of the present invention;

[0034] Figure 2 Flow chart for micronization identification of niobium iron ore by melting-tannin method;

[0035] Figure 3 Flow chart for the micronization identification of niobium iron rutile by zinc powder reduction method;

[0036] Figure 4 This is a scanning electron microscope photo of niobium iron ore;

[0037] Figure 5 This is a scanning electron microscope photo of niobium iron ore;

[0038] Figure 6 This is a scanning electron microscope photo of niobium iron rutile;

[0039] Figure 7 Spectroscopic analysis of elemental composition of niobium iron rutile. DETAILED DESCRIPTION

[0040] 1. Microchemical Identification of Niobium Iron Ore

[0041] Drop 1:3 phosphoric acid into the mineral particles or powder to be tested. The insoluble part is mixed with sodium carbonate and melted, then dissolved in distilled water. Add tannin solution, and the solution will first turn light yellow and then quickly turn orange-red.

[0042] The addition of ascorbic acid is helpful to prevent Fe 3+ and Mn 2+If ascorbic acid is not added, brown or purple-black precipitates will appear after adding the tannin reagent, which will seriously pollute the precipitation reaction of niobium and tannin.

[0043] If the niobium iron ore sample is melted with potassium pyrosulfate, a pungent corrosive gas will be generated (see formula 7-1) and a white film will appear. It is difficult to change color after adding tannin, and the success rate of identification is low. The final niobium iron ore identification process is shown in Figure 2 .

[0044] The specific steps include:

[0045] 1.1. Take an appropriate amount of sample powder to be tested and place it on a cover glass. First, select it under a microscope (because niobium minerals are all opaque minerals, transparent minerals should be screened out first to improve the success rate of the experiment);

[0046] 1.2. After adding an appropriate amount of phosphoric acid to dissolve most of the "impurity minerals", the remaining solid matter is heated and melted with an appropriate amount of Na2CO3 to observe its reaction:

[0047] If melting decomposition occurs, continue to add sodium peroxide and dilute sulfuric acid solution to observe the reaction phenomenon. If a light yellow precipitate appears and the precipitate disappears after adding phosphoric acid solution again, it proves that it contains a certain amount of Fe 3+ cation;

[0048] If orange-red or orange-yellow precipitate is also present, it indicates that the sample particles contain a certain amount of Ti 2+ Cations, the color of this part of the precipitation is related to Ti 2+ Proportional to the content;

[0049] 1.3. For the part that does not decompose after melting with Na2CO3, add appropriate amount of tannic acid and ascorbic acid and observe the reaction phenomenon. If a light yellow precipitate is produced, add a certain amount of zinc powder for reduction. If the precipitate turns into an orange-red precipitate, it proves that the sample contains Nb 5+ cation;

[0050] If all of the above phenomena occur, it proves that the sample contains Fe 3+ 、Ti 2+ and Nb 5+ , it means that this sample contains a certain amount of niobium iron rutile minerals. The flow charts are all Y / N yes / no charts, where Y represents the reaction has occurred and N represents no obvious reaction or no obvious reaction phenomenon and reaction products; it can also be understood that Y represents the part that has reacted and N represents the part that has not reacted. The details are as follows:

[0051] 2Fe(NbO3)2+10K2S2O7→4K5NbO5+Fe2(SO4)3+16SO3↑+SO2↑

[0052] 2 Microchemical Identification of Niobium Iron Rutile

[0053] Niobium iron rutile is a niobium-rich variant of rutile and is a low-niobium mineral. Since niobium exists in isomorphous form in niobium iron rutile, the microchemical identification of niobium iron rutile should not only identify niobium, but also Ti. 2+ Accurate identification.

[0054] As mentioned above, adding zinc powder can effectively improve the sensitivity of ferroniobium rutile identification. The final identification method is shown in Figure 3 .

[0055] The specific steps include:

[0056] 2.1. Place an appropriate amount of sample powder on a cover glass and select it under a microscope (niobium minerals are all opaque minerals, so in order to improve the success rate of the experiment, transparent minerals should be screened out first);

[0057] 2.2. After adding an appropriate amount of phosphoric acid to dissolve most of the "impurity minerals", the remaining solid matter is heated and melted with an appropriate amount of Na2CO3 to observe its reaction:

[0058] If melting decomposition occurs, add appropriate amount of distilled water to dilute, and then add appropriate amount of tannic acid and ascorbic acid to observe its reaction:

[0059] If a light yellow precipitate or sediment appears and turns into an orange-red precipitate after standing, it proves that there is Fe in the sample particles. 3+ and Nb 5+ , it proves that there are niobium iron ore particles in the sample, and tannic acid is added again, and the semi-quantitative analysis of niobium iron ore can be carried out through the color change reaction of the precipitate;

[0060] If no light yellow precipitate appears, but a purple-black precipitate appears, it proves that the sample contains Fe. 3+ , Mn 2+ , or prove the presence of manganese-containing ferromanganese or ferromanganese in the sample;

[0061] 2.3. If melting decomposition does not occur and no light yellow precipitate appears, but a brown precipitate appears, it proves that the sample particles are common iron minerals.

[0062] Niobium mineral identification and verification

[0063] The obtained pure niobium mineral was tested and verified by the method of "scanning electron microscope-energy spectrum analysis":

[0064] SEM photos of niobium iron ore are shown in Figure 4 , niobium iron ore energy spectrum analysis element composition see Figure 5 .

[0065] Table 4-2 Results of niobium iron ore energy spectrum analysis

[0066]

[0067] Niobium iron rutile

[0068] SEM photos of niobium iron rutile are shown in Figure 6 , ferroniobium rutile energy spectrum analysis element composition see Figure 7 .

[0069] Table 4-3 Spectrum analysis results of ferroniobium rutile

[0070]

[0071]

[0072] In summary, the obtained pure niobium minerals were verified by scanning electron microscopy-energy spectrum analysis, and the purity was >98%.

[0073] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A method for identifying multiple types of niobium minerals, characterized in that: include: (1) Microchemical Identification of Niobium Iron Ore The specific steps include: (1.1) Place an appropriate amount of sample powder on a coverslip and select under a microscope; (1.2) After adding an appropriate amount of phosphoric acid to dissolve most of the "impurity minerals", the remaining solid matter is heated and melted with an appropriate amount of Na2CO3 to observe its reaction: If melting decomposition occurs, continue to add sodium peroxide and dilute sulfuric acid solution to observe the reaction phenomenon. If a light yellow precipitate appears and the precipitate disappears after adding phosphoric acid solution again, it proves that it contains a certain amount of Fe 3+ cation; If orange-red or orange-yellow precipitates are also present, it indicates that the sample particles contain a certain amount of Ti. 2+ Cations, the color of this part of the precipitation is related to Ti 2+ Proportional to the content; (1.3) For the part that does not decompose after melting with Na2CO3, add appropriate amount of tannic acid and ascorbic acid and observe the reaction phenomenon. If a light yellow precipitate is produced, add a certain amount of zinc powder for reduction. If the precipitate turns into an orange-red precipitate, it proves that the sample contains Nb 5+ cation; If all of the above phenomena occur, it proves that the sample contains Fe 3+ 、Ti 2+ and Nb 5+ , otherwise it means that the sample contains a certain amount of niobium iron rutile mineral; (2) Microchemical Identification of Niobium Iron Rutile The specific steps include: (2.1) Place an appropriate amount of sample powder on a coverslip and select under a microscope; (2.2) After adding an appropriate amount of phosphoric acid to dissolve most of the "impurity minerals", the remaining solid matter is heated and melted with an appropriate amount of Na2CO3 to observe its reaction: If melting decomposition occurs, add appropriate amount of distilled water to dilute, and then add appropriate amount of tannic acid and ascorbic acid to observe its reaction: If a light yellow precipitate or sediment appears and turns into an orange-red precipitate after standing, it proves that there is Fe in the sample particles. 3+ and Nb 5+ , it proves that there are niobium iron ore particles in the sample, and tannic acid is added again, and the semi-quantitative analysis of niobium iron ore can be carried out through the color change reaction of the precipitate; If no light yellow precipitate appears, but a purple-black precipitate appears, it proves that the sample contains Fe. 3+ , Mn 2+ , or prove the presence of manganese-containing ferromanganese or ferromanganese in the sample; (2.3) If melting decomposition does not occur and no light yellow precipitate appears, but a brown precipitate appears, it proves that the sample particles are common iron minerals.

2. The ore and rock identification method for identifying multiple types of niobium minerals according to claim 1, characterized in that: The purpose of selecting under the microscope in the steps (1.1) and (2.1) is that since niobium minerals are all opaque minerals, transparent minerals are first screened out in order to improve the success rate of the experiment.

3. The ore and rock identification method for identifying multiple types of niobium minerals according to claim 1, characterized in that: Conventional mineral identification and composition analysis of niobium iron ore and niobium iron rutile are carried out using optical microscopy, electron microscopy and X-ray scanning.

4. The ore and rock identification method for identifying multiple types of niobium minerals according to claim 1, characterized in that: Determine the solubility of minerals, screen reagents, and determine the analysis process.

5. The ore and rock identification method for identifying multiple types of niobium minerals according to claim 1, characterized in that: Through microscopic observation, the obvious similarities and differences of each mineral micronization reaction are found out according to the dissolution state, chemical reaction phenomenon, precipitation characteristics and optical properties of pure mineral particles.

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