Processing method and optimization method of Tibetan medicine metal ash

Abstract

The invention provides a processing method and an optimizing method of Tibetan medicine metal ash, and belongs to the technical field of metal sulfide preparation. According to the Tibetan medicine metal ash processing method provided by the invention, overflow of elemental sulfur in a sulfur source is reduced by using an inverted container method in the processing process, so that the contact efficiency of metal and elemental sulfur is improved, and the efficiency of generating metal sulfide by reaction of metal, sulfur and realgar and the purity of sulfide in metal ash are improved; and moreover, the method is carried out in an incompletely closed container only by inversely buckling the container, so that the risk of explosion caused by sharp rise of the internal pressure of the container due to accumulation of volatile gas is prevented.

Description

Technical Field

[0001] This invention belongs to the field of metal sulfide preparation technology, specifically relating to a method for processing and optimizing Tibetan medicine metal ash. Background Technology

[0002] Metallic ash is a distinctive and indispensable mineral preparation in Tibetan medicine, widely used in the formulation of precious Tibetan medicines. Its core mechanism involves transforming metals such as gold, silver, copper, brass, bronze, iron, zinc, tin, and lead into pharmacologically active metal sulfides, arsenides, or sulfarsenides through unique processing techniques. Traditional Tibetan medicine processing typically involves high-temperature calcination of metals with sulfur and realgar (containing arsenic) in a sealed container, causing the metals to form metal sulfides or sulfarsenides, thereby altering the physicochemical properties of the metals, reducing toxicity, and enhancing efficacy. However, traditional methods suffer from the following technical bottlenecks: sulfur and realgar are prone to volatilization and diffusion at high temperatures. Sulfur and realgar readily sublimate and volatilize during heating, not only causing reactant loss and reducing the formation efficiency and yield of target metal sulfides, but also posing an explosion risk if carried out in a sealed container, as the accumulation of volatilized gases can lead to a rapid increase in internal pressure.

[0003] In existing technologies, mechanical forging of thinner metal foils improves reaction efficiency, but it still cannot solve the core defect of sulfur leakage during the sublimation of the sulfur source in the preparation of metallic ash. Therefore, developing a novel metallic ash processing technology that can effectively solve the problem of sulfur and realgar sublimation leakage and significantly improve the reaction efficiency of metals with sulfur / arsenic is of great significance for improving the production efficiency and quality control level of Tibetan medicine metallic ash. Summary of the Invention

[0004] The purpose of this invention is to provide a method and optimization method for processing Tibetan medicine metallic ash. This invention adopts the inverted container method, which solves the defect of sulfur source sublimation and diffusion at high temperature in the traditional metallic ash processing process.

[0005] To achieve the objectives of this invention, the following technical solutions are provided: A method for processing and optimizing metallic ash in Tibetan medicine includes the following steps: The metal is mixed with a sulfur source to obtain a mixture; the sulfur source is sulfur and / or realgar. The mixture is placed in a first container, and a second container is inverted over the outside of the first container. The mixture is then melted and sublimated under unsealed conditions to obtain the metallic ash. The first container and the second container are both single-sided open containers; the volume of the second container is larger than that of the first container.

[0006] Preferably, the metal includes one or more of gold, silver, copper, iron, zinc, tin, and lead.

[0007] Preferably, the metal is one or more of metal sheets, metal wires, and metal particles.

[0008] Preferably, the thickness of the metal sheet is 0.01~0.1 mm, the diameter of the metal wire is 0.01~0.1 mm, and the particle size of the metal particles is 5~500 μm.

[0009] Preferably, the weight ratio of the sulfur source to the metal is 2 to 20:1.

[0010] Preferably, the first container and the second container are high-temperature resistant containers with a heat resistance temperature of 1000~1800℃.

[0011] Preferably, the addition of a flux is also included; the flux is borax or sodium carbonate.

[0012] Preferably, the metal is further subjected to acid leaching pretreatment before use; the reagent used for acid leaching is an organic acid liquid.

[0013] Preferably, the first container and the second container are transparent containers; The melting and sublimation process also includes using a temperature measuring ring to monitor the heating temperature and holding time of the melting and sublimation process in real time.

[0014] Preferably, the sulfide content in the Tibetan medicine metallic ash is >97wt%.

[0015] This invention provides a method and optimization method for processing Tibetan medicine metallic ash, comprising the following steps: mixing a metal with a sulfur source to obtain a mixture; the sulfur source being sulfur and / or realgar; placing the mixture in a first container, and inverting a second container outside the first container, performing melt sublimation under unsealed conditions to obtain the metallic ash; the first and second containers are independently single-sided open containers; the volume of the second container is larger than that of the first container. This invention uses an inverted container method during the processing of Tibetan medicine metallic ash to reduce the leakage of elemental sulfur from the sulfur source, thereby improving the contact efficiency between the metal and elemental sulfur, thus increasing the efficiency of the reaction between the metal and sulfur and realgar to form metal sulfides and the purity of the sulfides in the metallic ash; furthermore, this invention, by using an inverted container in a partially sealed container, prevents the accumulation of volatile gases and the resulting rapid increase in internal pressure, thus avoiding the risk of explosion.

[0016] Furthermore, this invention can use devices such as temperature measuring rings and transparent containers to observe the processing of Tibetan medicine metal ash in real time, and achieves effective optimization of process parameters such as reaction reagents, heating temperature, heating time, sealing, and fluxing agents in an economical and feasible manner. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of different crucible combinations in Embodiment 1 of the present invention; Figure 2 This is an example of the sulfur spillover and condensation after heating for 30 minutes with different crucible combinations in Example 1 of the present invention. Figure 3 The results of the temperature measuring ring diameter test in Embodiment 2 of the present invention are shown. Detailed Implementation

[0019] This invention provides a method and optimization method for processing metallic ash in Tibetan medicine, comprising the following steps: The metal is mixed with a sulfur source to obtain a mixture; the sulfur source is sulfur and / or realgar. The mixture is placed in a first container, and a second container is inverted over the outside of the first container. The mixture is then melted and sublimated under unsealed conditions to obtain the metallic ash. The first container and the second container are both single-sided open containers; the volume of the second container is larger than that of the first container.

[0020] In this invention, unless otherwise specified, all raw materials used in the preparation are commercially available products well known to those skilled in the art.

[0021] This invention involves mixing a metal with a sulfur source to obtain a mixture. In this invention, the metal includes one or more of gold, silver, copper, iron, zinc, tin, and lead; in a specific embodiment, it can be copper. The metal is one or more of metal sheets, metal wires, and metal particles; in a specific embodiment, it can be metal particles or metal sheets. The thickness of the metal sheet is 0.01~0.1 mm, the diameter of the metal wire is 0.01~0.1 mm, and the particle size of the metal particles is 5~500 μm.

[0022] In this invention, the metal is further subjected to acid leaching pretreatment before use; the reagent used for acid leaching is a liquid containing organic acid, which in a specific embodiment can be Tibetan sour wine and / or sea buckthorn juice, and the pH value of the organic acid liquid is 2-4. This invention removes oxides and other impurities from the metal surface through acid leaching pretreatment.

[0023] In this invention, the sulfur source is sulfur and / or realgar; the weight ratio of the sulfur source to the metal is 2 to 20:1, and in specific embodiments it can be 5:1, 8:1, 10:1 or 13:1.

[0024] In this invention, the method of mixing the metal with the sulfur source includes: applying a paste of sulfur and / or realgar to the surface of a metal sheet and wrapping it with cotton cloth; embedding metal wires into the sulfur and / or realgar powder; and stirring and mixing the sulfur and / or realgar powder with the metal powder.

[0025] After obtaining the mixture, the present invention places the mixture in a first container, inverts a second container on the outside of the first container, and performs melting and sublimation under unsealed conditions to obtain the metal ash.

[0026] In this invention, the first and second containers are high-temperature resistant containers with a heat resistance temperature of 1000~1800℃; the material is ceramic, quartz, or corundum; the shape is cylindrical, cup-shaped, or square, and in a specific embodiment, it can be a crucible, further specifically a transparent quartz crucible; the first and second containers are independently single-sided open containers; the volume of the second container is larger than that of the first container. During the processing of this invention, the inverted container method reduces the leakage of elemental sulfur from the sulfur source, thereby improving the contact efficiency between the metal and elemental sulfur, thus increasing the efficiency of the reaction between the metal and sulfur and realgar to form metal sulfides and the purity of the sulfides in the metal ash; furthermore, this invention only uses inverted containers, conducted in a not completely sealed container, preventing the accumulation of volatile gases and a rapid increase in internal pressure, thus avoiding the risk of explosion.

[0027] In this invention, the heating method for molten sublimation is open flame heating or electric heating box-type high-temperature furnace; the molten sublimation temperature is 500~1800℃, and the holding time is 1~10h.

[0028] In this invention, the melt sublimation also includes a flux; the flux is borax or sodium carbonate.

[0029] This invention also includes using an alumina temperature measuring ring to measure the actual temperature and time of molten sublimation, in order to optimize parameters such as heating temperature, heating time, reaction reagents, sealing properties, and fluxing agents in actual production.

[0030] The sulfide content in the Tibetan medicine metallic ash prepared by the above-described processing method is >97wt%; the particle size of the Tibetan medicine metallic ash is 0.1~100μm, and in specific embodiments it can be 3, 10, 27, 32, 45 or 60μm.

[0031] The present invention also provides the application of the Tibetan medicine metallic ash described in the above technical solution in the preparation of Tibetan medicine.

[0032] To further illustrate the present invention, the processing method and optimization method of Tibetan medicine metallic ash provided by the present invention will be described in detail below with reference to the accompanying drawings and embodiments, but these should not be construed as limiting the scope of protection of the present invention.

[0033] Example 1 The effect of using an inverted crucible to reduce sulfur spillage loss: (1) Weigh out two portions of sulfur powder, 0.1g each, and place them into quartz crucibles with a volume of 10 mL respectively; (2) According to Figure 1 As shown on the left, place a 10 mL quartz crucible into a 30 mL quartz crucible that is upright and covered, and then place a 150 mL quartz crucible inside. (3) According to Figure 1 (Right side) Invert a 30 mL quartz crucible over the outside of a 10 mL quartz crucible, and then place a 150 mL quartz crucible inside. (4) The above-mentioned quartz crucible assembly containing sulfur is heated by a Bunsen lamp; Observe the leakage and condensation of sulfur during the heating process. The results are as follows: Figure 2 As shown (the left side is the combination with all crucibles upright, and the right side is the combination with crucibles upside down), after heating for 30 minutes, the color in the combination with all crucibles upright was significantly lighter than that in the combination with 30 mL crucibles upside down, indicating that the gaseous sulfur in the combination with 30 mL crucibles upside down was less than that in the combination with all crucibles upright.

[0034] Example 2 The specific steps for preparing copper metal ash for Tibetan medicine are as follows: (1) Take a pure copper foil with a thickness of 0.08 mm, cut it into a rectangle of 0.6 cm × 1.0 cm, boil it in acetic acid for 1 hour to destroy the oxide layer on the surface of the copper foil and obtain pretreated copper foil; (2) Apply the paste-like sulfur (solid content controlled at 80±5%) prepared with pure water to the surface of the copper foil, wrap it with cotton cloth, and let it air dry to obtain copper material. (4) Place the above copper material into a 10mL quartz crucible, and place an alumina temperature measuring ring (such as...) next to the quartz crucible. Figure 3 As shown in the figure, a 30mL quartz crucible is placed upside down on the outside, and then a 150mL quartz crucible is placed inside and kept warm through a quartz sleeve. (5) Heating the quartz crucible assembly containing the above materials by Bunsen burner; (6) Observe the changes of copper material during the heating process. The observation content includes: changes in the color and shape of copper material, and the diffusion and condensation of sulfur. (7) After heating is stopped, take out the alumina temperature measuring ring, measure its outer diameter, and calculate the actual maximum temperature of the material based on the correlation between the alumina deformation coefficient and temperature. Combine the observed material change process and the results of the quality analysis of the processed products to determine the optimal temperature in the processing process.

[0035] Observations showed that the color and shape of the copper material remained unchanged after heating for 45 minutes. Based on the outer diameter of the temperature measuring ring, the actual highest temperature in the quartz crucible was 600℃. These results indicate that the required reaction time for processing Tibetan medicine copper metal ash at 600℃ is 45 minutes.

[0036] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for processing and optimizing metallic ash in Tibetan medicine, characterized in that, Includes the following steps: The metal is mixed with a sulfur source to obtain a mixture; the sulfur source is sulfur and / or realgar. The mixture is placed in a first container, and a second container is inverted over the outside of the first container. The mixture is then melted and sublimated under unsealed conditions to obtain the metallic ash. The first container and the second container are both single-sided open containers; the volume of the second container is larger than that of the first container.

2. The processing method and optimization method according to claim 1, characterized in that, The metal includes one or more of gold, silver, copper, iron, zinc, tin, and lead.

3. The processing method and optimization method according to claim 2, characterized in that, The metal is one or more of the following: metal sheet, metal wire, and metal particles.

4. The processing method and optimization method according to claim 3, characterized in that, The metal sheet has a thickness of 0.01~0.1 mm, the metal filament has a diameter of 0.01~0.1 mm, and the metal particles have a particle size of 5~500 μm.

5. The processing method and its optimization method according to claim 1, characterized in that, The weight ratio of the sulfur source to the metal is 2~20:

1.

6. The processing method and its optimization method according to claim 1, characterized in that, The first and second containers are high-temperature resistant containers with a heat resistance temperature of 1000~1800℃.

7. The processing method and its optimization method according to claim 1, characterized in that, It also includes the addition of a flux; the flux is borax or sodium carbonate.

8. The processing method and its optimization method according to claim 1, characterized in that, The metal is further subjected to acid leaching pretreatment before use; the reagent used for acid leaching is an organic acid liquid.

9. The processing method and its optimization method according to claim 1, characterized in that, The first and second containers are transparent containers; The melting and sublimation process also includes using a temperature measuring ring to monitor the heating temperature and holding time of the melting and sublimation process in real time.

10. The processing method and optimization method according to claim 1, characterized in that, The sulfide content in the Tibetan medicine metallic ash is >97wt%.

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