Device for preparing high-purity arsenic

Abstract

The utility model relates to a device for preparing high-purity arsenic, which comprises an electrode reaction tank, the electrode reaction tank comprises an anode plate, a cathode plate and a power supply, the anode plate and the cathode plate are arranged in the electrode reaction tank, the power supply is electrically connected with the anode plate and the cathode plate, and an oxygen outlet and an arsenious acid inlet are sequentially arranged on the side wall of the electrode reaction tank close to the anode plate from top to bottom. An arsenic hydride discharge port is formed in the upper part of the side wall, close to the cathode plate, of the electrode reaction tank; the arsenic hydride discharge port is connected with a tubular heater, an outlet of the tubular heater is connected with a condensation collecting tank, and an outlet of the condensation collecting tank is connected with a hydrogen peroxide washer. According to the device, the electrode reaction tank, the tubular heater and the condensation collection tank are connected to form the high-purity arsenic preparation device adopting the electrode and thermal decomposition method, and the device can be used for preparing high-purity arsenic, can be used for efficiently recovering arsenic elements in arsenide waste residues generated in the metallurgical process, and fully realizes resource recycling.

Description

Technical Field

[0001] This utility model relates to the field of arsenic extraction technology, specifically to an apparatus for preparing high-purity arsenic by arsine thermal decomposition. Background Technology

[0002] In the metallurgical industry, after refining the desired metals, arsenic-containing waste residue (mainly arsenic trioxide) is typically generated. The treatment and resource utilization of arsenic-containing waste residue has always been a challenging and hot research topic in the industry.

[0003] Currently, the main methods for preparing high-purity arsenic include the chlorination-reduction method, the lead alloy sublimation distillation method, and the thermal decomposition method of arsine. Among these, the thermal decomposition method of arsine readily separates heavy metals, ensuring the purity of the obtained arsenic. It first prepares arsine using chemical or electrolytic methods, then refines and purifies it through adsorption and other methods. At 600℃-800℃, the arsine automatically decomposes into arsenic and hydrogen. This method easily separates heavy metals, reduces impurity contamination, and yields high-purity arsenic. Its main drawback is the high toxicity of arsine, requiring stringent safety measures. Existing technologies primarily disclose equipment for the chlorination-reduction method and the lead alloy sublimation distillation method, such as Chinese patents "A hydrogenation reduction device and a method for preparing high-purity arsenic" (CN104975191B) and "A method for efficiently preparing high-purity aluminum arsenide" (CN107902695A). Utility Model Content

[0004] To address the aforementioned problems, this invention provides an apparatus for preparing high-purity arsenic by the thermal decomposition of arsine. It mainly employs an electrode + thermal decomposition method for preparing high-purity arsenic, thereby safely and stably producing high-purity arsenic products.

[0005] The specific technical solution of this utility model is as follows: an apparatus for preparing high-purity arsenic by thermal decomposition of arsine, comprising an electrode reaction tank, wherein the electrode reaction tank includes an anode plate and a cathode plate disposed within the tank, and a power supply electrically connected to the anode plate and the cathode plate; an oxygen outlet and an arsenous acid inlet are sequentially opened from top to bottom on the side wall of the electrode reaction tank near the anode plate; an arsine outlet is opened above the side wall of the electrode reaction tank near the cathode plate; a tubular heater is connected to the arsine outlet; a condensation collection tank is connected to the outlet of the tubular heater; and a hydrogen peroxide scrubber is connected to the outlet of the condensation collection tank.

[0006] Furthermore, preferably, a partition is also provided in the electrode reaction tank, and the partition is disposed between the anode plate and the cathode plate.

[0007] Furthermore, preferably, the distance between the anode plate and the cathode plate is not less than 10 cm.

[0008] Furthermore, preferably, the electrode reaction tank has a residual liquid drain outlet located below the side wall near the cathode plate.

[0009] Furthermore, preferably, the arsenic acid inlet, the arsine outlet, and the residual liquid outlet are all equipped with valves.

[0010] Furthermore, preferably, the electrode reaction tank is a PPR sealing tank.

[0011] Furthermore, preferably, the partition is made of PPR material.

[0012] Furthermore, preferably, the condensate collection tank is equipped with a baffle.

[0013] Furthermore, preferably, a thermometer is also installed on the condensate collection tank.

[0014] The beneficial effects of this invention are as follows: The device described in this invention forms a high-purity arsenic preparation device using an electrode + thermal decomposition method by connecting an electrode reaction tank, a tubular heater, and a condensation collection tank. This device can produce high-purity arsenic, which can be used to efficiently recover arsenic from arsenic-containing waste slag generated during metallurgical processes, fully realizing resource recycling. Moreover, the device's simple structure and fully sealed operation can effectively improve operational efficiency and safety performance, making it valuable for widespread application. Attached Figure Description

[0015] Figure 1 This is an overall structural diagram of an apparatus for preparing high-purity arsenic according to the present invention;

[0016] Figure 2 for Figure 1 The structural diagrams of the anode plate and cathode plate are shown, with the left diagram being the front view and the right diagram being the side view.

[0017] In the diagram: 1-Electrode reaction tank, 11-Anode plate, 12-Cathode plate, 13-Power supply, 14-Oxygen outlet, 15-Arsenic acid inlet, 16-Arsenic trioxide outlet, 18-Baffle, 17-Residual liquid outlet; 2-Tube heater; 3-Condensation collection tank, 31-Baffle, 32-Thermometer; 4-Hydrogen peroxide scrubber. Detailed Implementation

[0018] To make the technical problems and solutions solved by this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present utility model and are not intended to limit the present utility model.

[0019] In the description of this utility model, it should be understood that the terms "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0020] In the description of this utility model, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," and "connect" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0021] like Figure 1 As shown, an apparatus for preparing high-purity arsenic includes an electrode reaction tank 1. The electrode reaction tank 1 includes an anode plate 11 and a cathode plate 12 disposed within the tank, and a power supply 13 electrically connected to the anode plate 11 and the cathode plate 12 (the anode plate 11 is connected to the positive terminal of the power supply 13, and the cathode plate 12 is connected to the negative terminal of the power supply 13). An oxygen outlet 14 and an arsenic acid inlet 15 are sequentially provided from top to bottom on the side wall of the electrode reaction tank 1 near the anode plate 11. An arsine outlet 16 is provided above the side wall of the electrode reaction tank 1 near the cathode plate 12, and a residual liquid outlet 17 is provided below it. Valves are provided for the arsenic acid inlet 15, the arsine outlet 16, and the residual liquid outlet 17. A tubular heater 2 is connected to the arsine outlet 16, and a condensation collection tank 3 is connected to the outlet of the tubular heater 2. A hydrogen peroxide scrubber 4 is connected to the outlet of the condensation collection tank 3.

[0022] like Figure 2 As shown, both the anode plate 11 and the cathode plate 12 are composed of conductive copper strips 51 and electrode plates 52, wherein the electrode plates are made of 316 stainless steel.

[0023] Preferably, a partition 18 is also provided inside the electrode reaction tank 1, and the partition 18 is disposed between the anode plate 11 and the cathode plate 12. Meanwhile, the distance between the anode plate 11 and the cathode plate 12 is not less than 10 cm. The arrangement of the partition 18 and the control of the distance between the two electrode plates can ensure that the gases generated by the two electrode reactions escape into the air above their respective electrode regions and enter their respective processes through the exhaust ports above them.

[0024] The electrode reaction tank 1 is a PPR sealed tank, and the partition 18 is made of PPR material. The chemical corrosion resistance of PPR material can effectively resist the erosion of arsenic acid solution and extend the service life of the equipment.

[0025] Preferably, the condensation collection tank 3 is equipped with a baffle 31, which can prolong the time of metallic arsenic vapor in the condensation collection tank 3 and improve the arsenic condensation and recovery effect; a thermometer 32 is also inserted on the condensation collection tank 3 to facilitate observation of temperature changes inside the condensation collection tank 3.

[0026] Working principle: First, nitrogen gas is introduced into the arsenic acid inlet 15 to expel the air in the entire device. Then, arsenic acid liquid (electrode liquid) is added into the electrode reaction tank 1 through the arsenic acid inlet 15. The liquid surface of the arsenic acid liquid covers the partition 18 to a depth of not less than 10cm. In this way, the liquid surface and the partition 18 form a liquid seal effect, allowing the anode plate and cathode plate on both sides of the partition 18 to react independently, and the gas generated by the reaction escapes to the air above their respective electrode areas.

[0027] Then, power supply 13 is turned on, energizing the anode plate 11 and cathode plate 12, causing the arsenic acid solution to undergo the electrode reaction: 2H3AsO3 = 2AsH3↑ +3O2↑; A small amount of water in the solution undergoes the reaction: 2H2O↑=2H2↑+O2↑.

[0028] Oxygen (O2) is generated at the anode of electrode reaction tank 1 and escapes from the anode end through oxygen outlet 14 for collection; arsine (AsH3) and a small amount of hydrogen (H2) are generated at the cathode and escape from the cathode end through arsine outlet 16 into tubular heater 2.

[0029] The tubular heater 2 is started and heated to 800~900℃. The arsine entering it decomposes into arsenic vapor and hydrogen gas 2AsH3=2As+3H2. The arsenic vapor and hydrogen gas enter the condenser collection tank 4. The arsenic vapor is cooled and deposited in the condenser collection tank 4 to obtain high-purity arsenic ash. The hydrogen gas and a very small amount of arsenic vapor continue to enter the hydrogen peroxide scrubber 5 for further processing.

[0030] Experiments have verified that high-purity arsenic can be produced using the aforementioned device. The raw material for producing high-purity arsenic is arsenic trioxide, which reacts with water to produce arsenous acid solution: As₂O₃ + 3H₂O = 2H₃AsO₃. Therefore, this device can be used to recover arsenic from arsenic compound waste generated during metallurgical processes.

[0031] The present invention has been described in detail above through specific and preferred embodiments. However, those skilled in the art should understand that the present invention is not limited to the embodiments described above. Any modifications or equivalent substitutions made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. An apparatus for preparing high-purity arsenic, characterized in that: The device includes an electrode reaction tank (1), which includes an anode plate (11) and a cathode plate (12) disposed in the tank, and a power supply (13) electrically connected to the anode plate (11) and the cathode plate (12). An oxygen outlet (14) and an arsenic acid inlet (15) are sequentially opened from top to bottom on the side wall of the electrode reaction tank (1) near the anode plate (11). An arsine outlet (16) is opened above the side wall of the electrode reaction tank (1) near the cathode plate (12). A tubular heater (2) is connected to the arsine outlet (16). A condensation collection tank (3) is connected to the outlet of the tubular heater (2). A hydrogen peroxide scrubber (4) is connected to the outlet of the condensation collection tank (3).

2. The apparatus for preparing high-purity arsenic according to claim 1, characterized in that: The electrode reaction tank (1) is also provided with a partition (18), which is located between the anode plate (11) and the cathode plate (12).

3. The apparatus for preparing high-purity arsenic according to claim 2, characterized in that: The distance between the anode plate (11) and the cathode plate (12) is not less than 10cm.

4. The apparatus for preparing high-purity arsenic according to claim 3, characterized in that: The electrode reaction tank (1) has a residual liquid outlet (17) located below the side wall near the cathode plate (12).

5. The apparatus for preparing high-purity arsenic according to claim 4, characterized in that: The arsenic acid inlet (15), arsine outlet (16), and residual liquid outlet (17) are all equipped with valves.

6. The apparatus for preparing high-purity arsenic according to claim 1, characterized in that: The electrode reaction tank (1) is a PPR sealing tank.

7. The apparatus for preparing high-purity arsenic according to claim 2, characterized in that: The partition (18) is made of PPR material.

8. The apparatus for preparing high-purity arsenic according to claim 1, characterized in that: The condensate collection tank (3) is equipped with a baffle (31).

9. The apparatus for preparing high-purity arsenic according to claim 8, characterized in that: A thermometer (32) is also installed on the condensate collection tank (3).

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