A method for purifying manganese metal flakes

Abstract

The present invention relates to the technical field of manganese metal purification, and specifically to a method for purifying manganese metal flakes. The method comprises the following steps: 1: placing a quartz tube, quartz glass slag, quartz wool, and impure manganese metal flakes containing impurities in a drying oven for drying; and 2: placing the quartz glass slag, quartz wool, and impure manganese metal flakes treated in step 1 together in a quartz tube, evacuating and sealing the tube, and then heating and keeping the tube warm, to finally prepare high-purity manganese metal flakes. The preparation method of the present invention improves the purity of chemical raw materials, increases the success rate of chemical reactions and material synthesis, performs purification under relatively low vacuum conditions, and reduces impurities in chemical reactions. The method has a short reaction time and is particularly suitable for purifying small batches of materials. The quartz raw materials required for the purification process are relatively stable, easy to obtain, and low in cost. After purification, the quartz raw materials will not adhere to the surface of the manganese flakes, making separation simple and eliminating the need for specialized purification equipment.

Description

Technical Field

[0001] The present invention relates to the technical field of purification of metallic manganese, and in particular to a method for purifying metallic manganese sheets. Background Art

[0002] Manganese metal is a common chemical metal element. In the laboratory, experiments usually require the use of high-purity manganese metal. However, the purity of manganese metal flakes sold on the market does not meet the purity standards marked on the product, because the purity marked on commercial products generally refers to the purity relative to metal elements such as iron, calcium, and cobalt during the industrial production and refining process, and does not include the purity of oxygen or other light elements such as hydrogen, carbon, and nitrogen. In particular, when synthesizing the magnetic topological insulator MnBi2Te4, a popular material in the field of condensed matter physics in this laboratory, it is necessary to purchase chemical raw materials Mn, Bi, and Te to synthesize the product through a solid-phase reaction method. However, directly using the manganese metal raw materials purchased from the manufacturer cannot successfully synthesize the high-purity target product, and the main product often contains many impurities.

[0003] Therefore, in order to obtain more high-purity experimental products and accurate experimental data, the purchased metallic manganese raw material needs to be purified. In addition, the metallic manganese single substance that has not been used for a long time in the laboratory will react chemically with carbon dioxide, water, oxygen, etc. in the air over time, forming impurities on the surface of the manganese single substance, so that the purity of the manganese single substance is reduced. And for these light elements, even if they are very trace, they will greatly affect the product and result of the chemical reaction. Therefore, the purpose of this technical invention is to effectively remove the trace impurities such as oxides and water that are not easily detected in the metallic manganese raw material, improve the purity of chemical raw materials, improve the success rate of chemical reactions and material synthesis, and quickly and conveniently obtain purer manganese raw materials for laboratory use, without the need for special purification equipment, and is particularly suitable for the purification of small batches of materials, with low cost and high speed. Summary of the Invention

[0004] In response to the above-mentioned technical problems, the present invention proposes a method for purifying metallic manganese flakes, which can further purify metallic manganese flakes or purify elemental metallic manganese flakes that have been unused in the laboratory for a long time, and remove various impurities that are difficult to detect, including oxides and hydrates.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is as follows:

[0006] A method for purifying metallic manganese flakes, comprising:

[0007] Step 1: Place the quartz tube, quartz glass slag, quartz wool and impure manganese metal sheets containing impurities in a drying oven for drying;

[0008] Step 2: placing the quartz glass slag, quartz wool and impure manganese metal flakes processed in step 1 together in a quartz tube, evacuating and sealing the tube, and then heating and keeping the tube warm to finally prepare high-purity manganese metal flakes.

[0009] Preferably, the step 1 is specifically:

[0010] Place the quartz tube, quartz glass slag and quartz wool in a constant temperature forced air drying oven, keep it at 120°C for 8-12 hours, and then take it out.

[0011] Preferably, the step 2 is specifically as follows:

[0012] Step 2.1: Place the quartz glass slag, quartz wool and impure manganese flakes dried in step 1 into a quartz tube, purge with inert gas three times, and evacuate to 5×10 -2 Seal below 10 Torr and keep at 1000℃ for 12 hours;

[0013] Step 2.2: After heating, black matter adheres to the surface of the quartz wool, quartz glass slag, and quartz tube, and the surface of the manganese sheet turns silvery white with a metallic luster. Knock open the quartz tube and clean the manganese sheet three times with anhydrous ethanol.

[0014] Step 2.3: If the surface of the manganese flakes does not have a clear metallic luster, repeat step 2.1 for multiple purifications until high-purity manganese metal flakes are obtained.

[0015] Compared with the prior art, the present invention has the following beneficial effects:

[0016] 1. Improve the purity of chemical raw materials, increase the success rate of chemical reactions and material synthesis, purify under lower vacuum conditions, and reduce impurities in chemical reactions.

[0017] 2. The reaction time is short, and relatively pure manganese raw materials can be quickly obtained for laboratory use. It is particularly suitable for small-batch material purification.

[0018] 3. The quartz raw materials required for the purification process are relatively stable, easy to obtain, and low in cost. After purification, they will not adhere to the surface of the manganese sheet, and the separation is simple, and no special purification equipment is required. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The accompanying drawings are used to provide further understanding of the present invention and constitute a part of the specification. They are used to explain the present invention together with the embodiments of the present invention and do not constitute a limitation of the present invention.

[0020] In the attached figure:

[0021] Figure 1 is a flow chart of the method of the present invention;

[0022] Figure 2 (a)(b)(c)(d) are all impure manganese metal flakes containing impurities;

[0023] Figure 3 This is a diagram showing the oxidation of the surface of a small amount of manganese metal sheet placed in a quartz tube;

[0024] Figure 4 This is a diagram showing the oxidation of the surface of a large amount of manganese metal sheets placed in a quartz tube;

[0025] Figure 5 This is a test tube for purifying a small amount of metallic manganese after heating the quartz tube at 1000℃ for 12 hours;

[0026] Figure 6 This is a test tube for purifying a large amount of metallic manganese after heating the quartz tube at 1000℃ for 12 hours;

[0027] Figure 7 (a) is a photo of the manganese metal sheet after one purification. Figure 7 (b) is a photo of the manganese metal sheet still in the quartz tube after two purifications. DETAILED DESCRIPTION

[0028] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0029] Example 1

[0030] A method for purifying metallic manganese flakes, comprising:

[0031] Step 1: Place the quartz tube, quartz glass slag, quartz wool and impure manganese flakes containing impurities in a constant temperature blast drying oven, keep it at 120℃ for 8-12 hours, and then take it out.

[0032] There are no special requirements for the quartz tube used. If quartz glass slag is the primary reactant, its mass should be at least 10 times the mass of the manganese flakes to be purified. In this case, the mass of the quartz wool is related to the quartz tube diameter. After inserting the quartz wool into the quartz tube, it is sufficient to limit the movement of the quartz glass slag. If the mass of the manganese flakes to be purified is less than 300mg, quartz wool can be the primary reactant, and its mass should be at least 1.5 times the mass of the manganese flakes to be purified. In this case, the mass of the quartz glass slag is related to the quartz tube diameter. Place the quartz glass slag so that the quartz wool does not touch the bottom of the quartz tube.

[0033] Step 2: Place the quartz glass slag, quartz wool and impure manganese metal flakes processed in step 1 together in a quartz tube, evacuate and seal, then heat and keep warm to finally prepare high-purity manganese metal flakes.

[0034] Step 2.1: If Figure 2 As shown in the figure, the quartz wool dried in step 1 and the unpurified manganese metal sheet were placed in a quartz tube, and purged with argon gas three times (vacuuming-flushing with argon gas was counted as one purge), and then evacuated to 5×10 -2 Torr and sealed. If the vacuum degree is not high enough, more manganese oxide and manganous oxide that is difficult to handle will be introduced into the metallic manganese sheet.

[0035] If the amount of manganese metal to be purified is large and the mass is greater than 300 mg, a certain amount of quartz glass slag should be added to the manganese flakes. The mass of the quartz glass slag should be more than 10 times that of the manganese flakes. After thorough mixing, add it to the quartz tube. The manganese flakes should be wrapped by the quartz glass slag as much as possible without touching the quartz tube wall. Figure 3 As shown. At the same time, in order to increase the contact area between the manganese element fragments and the quartz, a small amount of quartz wool can be added on top of the manganese sheet. Then place the vacuum-sealed quartz tube flat in a box or tube furnace and keep it at 1000℃ for 12 hours;

[0036] Step 2.2: After heating is completed, Figure 4 As shown in the figure, the quartz wool in the middle of the quartz tube changes from white to black, and there are dark attachments on the inner wall of the upper part. If the wall of the selected quartz tube is thin, the purified manganese flakes are of large mass but quartz glass slag is not added, the tube wall will have messy, small and evenly distributed cracks. If quartz glass slag is added to purify more manganese flakes, such as Figure 5 As shown in the figure, there are dark attachments on the quartz tube wall and the surface of the internal quartz glass slag, but the quartz wool does not show obvious blackening.

[0037] It can be seen that after 12 hours of heat preservation, impurities such as manganese oxide and manganese hydrate reacted chemically with the quartz tube wall and quartz wool.

[0038] Knock open the quartz tube, such as Figure 7 As shown in (a), the surface of the manganese sheet turned silvery white with a metallic luster. The sheet was washed with anhydrous ethanol three times.

[0039] Step 2.3: If the surface of the manganese sheet does not have a clear metallic luster, repeat steps 1 and 2.1. Place the dried quartz wool, quartz glass slag and the purified manganese sheet in a quartz tube. Wash the tube with inert gas three times and then evacuate to 5×10 -2 Torr, and seal, heat and keep warm. Figure 7 As shown in (b), the surface of the manganese sheet turned silvery white with a metallic luster. The manganese sheet was washed three times with anhydrous ethanol.

[0040] Energy dispersive X-ray spectroscopy (EDS) analysis was performed on a random number of measurement points on both unpurified and purified manganese metal flakes. The measurement data are shown in Table 1. The EDS data for the purified manganese flakes show that the oxygen content at some locations on the surface of the flakes is significantly lower than that of the unpurified flakes, such as measurement points 2, 3, 7, and 8. The oxygen content at measurement points near the cross-section is even lower, confirming the effectiveness of the purification process.

[0041] Table 1 EDS measurement of oxygen atom content at various locations on the manganese sheet

[0042]

[0043] Note: The unpurified, once-purified, and twice-purified manganese flake samples used for EDS testing are not the same samples, but are randomly taken from the same batch of purchased or purified samples, and the measurement points are randomly selected in the test.

[0044] The basic principles, main features, and advantages of the present invention are shown and described above. Those skilled in the art should understand that the present invention is not limited to the foregoing embodiments. The foregoing embodiments and descriptions are merely illustrative of the principles of the present invention. Various changes and modifications may be made to the present invention without departing from the spirit and scope of the present invention. Such changes and modifications are intended to fall within the scope of the present invention. The scope of protection claimed in the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for purifying metallic manganese flakes, characterized by: include: Step 1: Place the quartz tube, quartz glass slag, quartz wool and impure manganese metal sheets containing impurities in a drying oven for drying; Step 2: placing the quartz glass slag, quartz wool and impure manganese metal flakes processed in step 1 together in a quartz tube, evacuating and sealing the tube, and then heating and keeping the tube warm to finally prepare high-purity manganese metal flakes.

2. The method for purifying a metallic manganese sheet according to claim 1, wherein: The step 1 is specifically as follows: Place the quartz tube, quartz glass slag and quartz wool in a constant temperature forced air drying oven, keep it at 120°C for 8-12 hours, and then take it out.

3. The method for purifying a metallic manganese sheet according to claim 2, wherein: The step 2 is specifically as follows: Step 2.1: Place the quartz glass slag, quartz wool and impure manganese flakes dried in step 1 into a quartz tube, purge with inert gas three times, and evacuate to 5×10 -2 Seal below 10 Torr and keep at 1000℃ for 12 hours; Step 2.2: After heating, black matter adheres to the surface of the quartz wool, quartz glass slag, and quartz tube, and the surface of the manganese sheet turns silvery white with a metallic luster. Knock open the quartz tube and clean the manganese sheet three times with anhydrous ethanol. Step 2.3: If the surface of the manganese flakes does not have a clear metallic luster, repeat step 2.1 for multiple purifications until high-purity manganese metal flakes are obtained.

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