A device capable of reducing the antimony content in industrial metal arsenic and its production method

Abstract

A device capable of reducing the antimony content in industrial metal arsenic and a production method thereof, the device comprising a heating furnace (1), a vacuum tank (2) with a lower middle portion located in the heating furnace and an upper portion extending out and exposed to the air, a volatilization inner sleeve (12) composed of a charging crucible (14) at the lower portion, a metal arsenic sublimation distributor (3) at the middle portion, and a tail gas condensation distribution baffle (6) at the top, a material collection plate (9) arranged between the vacuum tank and the volatilization inner sleeve and located at the upper portion of the vacuum tank, a cover plate (7) arranged at the top of the vacuum tank, and a vacuum pumping tube (8) arranged on the cover plate; a condensation diversion sieve plate (4) is arranged between the charging crucible (14) and the metal arsenic sublimation distributor. The device of the present invention has a reasonable structure, proper temperature gradient distribution, a short process flow, high production efficiency, high product quality after industrial metal arsenic treatment, good impurity separation effect, and low purification cost.

Description

Technical Field

[0001] The invention relates to the technical field of nonferrous metal smelting and purification, and in particular to a device and a method for reducing the antimony content in industrial metal arsenic. Background Art

[0002] At present, most of the domestic industrial metal arsenic production uses smelting dust as raw material. Due to the relatively complex composition of the raw materials, the industrial metal arsenic produced is of low grade, mainly due to the high content of impurity antimony (antimony 0.3-2%), and the sales price is low. High-grade metal arsenic has a lower antimony content requirement (antimony <0.01%), and the price is 28,000-35,000 yuan. The market demand is large and the supply is in short supply. The preparation of high-grade metal arsenic mainly uses arsenic trioxide produced from arsenic mines or low-antimony arsenic trioxide produced from industrial secondary materials. Due to the scarcity of raw materials, the amount of high-grade metal arsenic produced is decreasing. Various manufacturers are exploring ways to reduce the antimony content in industrial metal arsenic to improve the competitiveness of industrial metal arsenic market sales. Summary of the invention

[0003] The purpose of the present invention is to solve the problems existing in the prior art and to provide a device and method for reducing the antimony content in industrial metal arsenic.

[0004] The purpose of the present invention is achieved through the following technical solutions:

[0005] A device for reducing the antimony content in industrial metal arsenic comprises a heating furnace, a vacuum tank with a lower middle portion located in the heating furnace and an upper portion extending out and exposed to the air, a volatilization inner sleeve composed of a charging crucible at the lower portion, a metal arsenic sublimation distributor at the middle portion, and a tail gas condensation distribution baffle at the top, a material collecting plate arranged between the vacuum tank and the volatilization inner sleeve and located at the upper portion of the vacuum tank, a cover plate arranged at the top of the vacuum tank, and a vacuum pumping tube arranged on the cover plate; a condensation diversion sieve plate is arranged between the charging crucible and the metal arsenic sublimation distributor; the tail gas condensation distribution baffle naturally covers the top of the metal arsenic sublimation distributor, and the tail gas condensation distribution baffle and the metal arsenic sublimation distributor are separated and not connected.

[0006] Furthermore, a heat-insulating jacket is provided between the heating furnace and the vacuum tank above the charging crucible.

[0007] Furthermore, the heating furnace 1 includes a metal shell 15 and a refractory material layer built on the inner wall of the metal shell.

[0008] Furthermore, a support ear for fixing the vacuum tank is provided at the furnace opening of the heating furnace 1 .

[0009] Furthermore, the height of the exposed section of the vacuum tank extending outward and exposed to the air is 1 / 4 of the height of the vacuum tank, and the material collecting tray is arranged on the upper part of the exposed section.

[0010] The production method of the device for reducing the antimony content in industrial metal arsenic according to the present invention is as follows:

[0011] S1. Selecting industrial metal arsenic with an arsenic content of 97 to 99 wt% and an antimony content of 0.3 to 2 wt% as raw material, and adding the raw material to a charging crucible;

[0012] S2. The charging crucible is heated by a volatilizing inner sleeve, and the charging crucible is slowly heated to 500-530°C within 120-150 minutes, and then kept at a constant temperature for 50-70 minutes; then the temperature is continued to rise, and after the temperature is raised to 560-580°C within 50-70 minutes, the temperature is kept at a constant temperature for 20-22 hours; the material in the charging crucible is heated to generate arsenic vapor, and the arsenic vapor rises through the condensation diverter sieve plate, so that the antimony condensation is no longer volatile, and the arsenic vapor is dispersed, buffered and decelerated;

[0013] Use an insulation jacket to keep the temperature of the metal arsenic sublimation distributor at 350-400°C within 25 hours;

[0014] During the heating and insulation process, the volatilization rate of arsenic vapor is controlled by controlling the temperature and pressure in the vacuum tank;

[0015] S3. Arsenic vapor rises along the metal arsenic sublimation distributor, and is gradually cooled down when passing through a section of the vacuum tank exposed to the air. When the arsenic vapor rises to the top of the metal arsenic sublimation distributor, the exhaust gas condensation distribution baffle is lifted up by the steam pressure, and the arsenic vapor is ejected from the gap between the exhaust gas condensation distribution baffle and the metal arsenic sublimation distributor into the upper part of the condensation collection area, and falls into the material collection tray after being condensed, thereby obtaining an industrial metal arsenic product with an arsenic content of >99.5wt% and an antimony content of <0.01wt%.

[0016] Furthermore, in the above step S2, the pressure in the vacuum tank is controlled at 6-600 Pa, and the volatilization rate of arsenic vapor is controlled at 1-3 mm / s.

[0017] The heating furnace of the device of the present invention is provided with a material heating volatilization zone and a volatilization insulation zone from bottom to top. The loading crucible is located in the material heating volatilization zone for heating industrial metal arsenic and volatilizing the metal arsenic therein. The middle and lower parts of the metal arsenic sublimation distributor are located in the volatilization insulation zone, so that the volatilized metal arsenic is insulated and rises. The upper end of the vacuum tank is exposed to the air and naturally cools down, so that the metal arsenic is gradually cooled during the rising process, and the metal arsenic is condensed by the tail gas condensation distribution baffle to form a metal arsenic product which is collected in the material collection tray, which can prevent the arsenic vapor from being discharged. The condensation diversion sieve plate arranged between the loading crucible and the metal arsenic sublimation distributor can condense the high boiling point and high melting point element antimony and no longer volatilize it, and can also disperse, buffer and slow down the arsenic vapor, thereby improving the condensation effect of the metal arsenic. The loading crucible and the volatilization inner sleeve are both arranged in the vacuum tank, and the production of metal arsenic is completed in a full vacuum state, which is safe and efficient, and the collection effect of metal arsenic is good.

[0018] The device of the present invention is designed in combination with market demand and the characteristics of industrial metal arsenic, and has a reasonable structure, proper temperature gradient distribution, and little environmental pollution. The product obtained by the present invention after treating industrial metal arsenic is of high quality and has a good impurity separation effect. After treatment, industrial metal arsenic can achieve arsenic>99.5%, antimony<0.01%, low purification cost, and good market application prospects.

[0019] The device of the present invention has reasonable structure, proper temperature gradient distribution, high automation of device control, reduced labor intensity and little environmental pollution. The method of the present invention has short process flow, high production efficiency, high product quality after industrial metal arsenic treatment, good impurity separation effect and low purification cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic structural diagram of the device of the present invention. DETAILED DESCRIPTION

[0021] like Figure 1The device for reducing the antimony content in industrial metal arsenic shown in the figure comprises a heating furnace 1, a vacuum tank 2 whose lower middle part is located in the heating furnace and whose upper part is extended out and exposed to the air, a volatilization inner sleeve 12 composed of a charging crucible 14 at the lower part, a metal arsenic sublimation distributor 3 at the middle part, and a tail gas condensation distribution baffle 6 at the top, a material collection tray 9 arranged between the vacuum tank 2 and the volatilization inner sleeve 12 and located at the upper part of the vacuum tank, a cover plate 7 arranged at the top of the vacuum tank, and a vacuum pipe 8 arranged on the cover plate. The tail gas condensation distribution baffle 6 naturally covers the top of the metal arsenic sublimation distributor 3, the tail gas condensation distribution baffle is separated from the metal arsenic sublimation distributor, and the tail gas condensation distribution baffle is not fixedly connected to the metal arsenic sublimation distributor. When the arsenic vapor in the metal arsenic sublimation distributor rises and forms a certain pressure in the metal arsenic sublimation distributor, the tail gas condensation distribution baffle will be slightly lifted, and the arsenic vapor will be ejected from the gap between the tail gas condensation distribution baffle and the metal arsenic sublimation distributor. A condensation diversion screen plate 4 is arranged between the charging crucible 14 and the metal arsenic sublimation distributor 3, which can condense the high boiling point and high melting point element antimony in the volatile atmosphere and no longer volatilize, and can also disperse, buffer and slow down the arsenic vapor, thereby improving the condensation effect and efficiency of the metal arsenic. The bottom of the vacuum tank 2 is placed at the bottom of the heating furnace 1, and a support ear 5 for fixing the vacuum tank 2 is arranged at the furnace mouth of the heating furnace. The height of the exposed section of the vacuum tank extending outward and exposed to the air is 1 / 4 of the height of the vacuum tank, and the material collection tray 9 is arranged on the upper part of the exposed section. The exposed section of the vacuum tank is naturally cooled in the air and is the condensation collection area 10 of the product. The heating furnace 1 includes a metal shell 15 and a refractory material layer 16 built on the inner wall of the metal shell. The refractory material layer is built in the same way as the inner wall refractory material layer of the existing smelting furnace. An insulation cover 11 made of aluminum silicate wool is arranged between the heating furnace 1 and the vacuum tank above the charging crucible 14. The charging crucible and the volatilization inner sleeve are both arranged in the vacuum tank, and the production of metallic arsenic is completed in a full vacuum state, which is safe, efficient, clean and environmentally friendly, and the collection effect of metallic arsenic is good.

[0022] The production method of the device of the present invention is as follows:

[0023] S1. Select an industrial metal arsenic content of 97 to 99wt% and an antimony content of 0.3 to 2wt% as a raw material, and add the raw material to the charging crucible 14;

[0024] S2. The charging crucible 14 is heated by a trough-type heating jacket 13. The charging crucible is slowly heated to 500-530°C within 120-150 minutes, and then kept at a constant temperature for 50-70 minutes; then the temperature is continued to rise, and within 50-70 minutes, the temperature is raised to 560-580°C, and then kept at a constant temperature for 20-22 hours; the material in the charging crucible is heated to generate arsenic vapor, and the arsenic vapor rises through the condensation diversion sieve plate 4, and the high boiling point and high melting point element antimony is condensed and no longer volatilized, and the arsenic vapor is dispersed, buffered and decelerated; the insulation jacket is used for insulation to ensure that the temperature of the metal arsenic sublimation distributor 3 is maintained at 350-400°C within 25 hours;

[0025] During the heating and heat preservation process, the volatilization speed of the arsenic vapor is controlled by controlling the temperature and pressure in the vacuum tank 2; the pressure in the vacuum tank is controlled at 6-600 Pa, and the volatilization speed of the arsenic vapor is controlled at 1-3 mm / s;

[0026] During this heating process, the tail gas condensation distribution baffle 6 covers the top of the metal arsenic sublimation distributor 3 to prevent the material in the metal arsenic sublimation distributor from being heated;

[0027] S3. Arsenic vapor rises along the metal arsenic sublimation distributor 3, and is gradually cooled down when passing through a section of the vacuum tank exposed to the air. When the arsenic vapor rises to the top of the metal arsenic sublimation distributor, the tail gas condensation distribution baffle is slightly lifted up by the remaining steam pressure, and the arsenic vapor is ejected from the gap between the tail gas condensation distribution baffle and the metal arsenic sublimation distributor into the upper part of the condensation collection area 10, and falls into the material collection tray 9 after being condensed, to obtain an industrial metal arsenic product with an arsenic content of >99.5wt% and an antimony content of <0.01wt%.

[0028] The heating furnace 1 of the present invention is provided with a material heating and volatilization zone and a volatilization and heat preservation zone from bottom to top, and a bottom sink-type heating jacket 13 and a heat preservation jacket 11 of aluminum silicate wool are respectively provided outside the material heating and volatilization zone and the volatilization and heat preservation zone. The volatilization inner jacket 12 includes a charging crucible 14 at the bottom, a metal arsenic sublimation distributor 3 in the middle, and a tail gas condensation distribution baffle 6 at the top. The charging crucible 14 is located in the material heating and volatilization zone for heating the industrial metal arsenic in the crucible and volatilizing the metal arsenic therein. The middle and lower parts of the metal arsenic sublimation distributor 3 are located in the volatilization and heat preservation zone, so that the volatilized metal arsenic is heat-insulated and rises. The upper end of the vacuum tank is exposed to the air and naturally cools down, so that the metal arsenic is gradually cooled during the rising process. The arsenic vapor rising to the top of the metal arsenic sublimation distributor 3 pushes open the tail gas condensation distribution baffle 6, and is ejected from the gap formed between the metal arsenic sublimation distributor and the tail gas condensation distribution baffle and then condensed to form an industrial metal arsenic product with reduced antimony content and falls into the material collection tray 9 for centralized collection.

[0029] The present invention has high production efficiency and good quality of the obtained metal arsenic. The production cycle of each furnace is 25-30 hours. Finally, the mass content of arsenic after treatment of industrial metal arsenic is greater than 99.5%, and antimony is less than 0.01%, which can meet the requirements of the products needed by the market.

Claims

1. A device for reducing the antimony content in industrial metal arsenic, characterized in that: The invention comprises a heating furnace (1), a vacuum tank (2) with a lower middle portion located in the heating furnace and an upper portion extending out and exposed to the air, a volatilization inner sleeve (12) composed of a charging crucible (14) at the lower portion, a metal arsenic sublimation distributor (3) at the middle portion, and a tail gas condensation distribution baffle (6) at the top portion, a material collection tray (9) arranged between the vacuum tank (2) and the volatilization inner sleeve (12) and located at the upper portion of the vacuum tank, a cover plate (7) arranged at the top of the vacuum tank, and a vacuum pumping tube (8) arranged on the cover plate; a condensation diversion sieve plate (4) is arranged between the charging crucible (14) and the metal arsenic sublimation distributor (3); the tail gas condensation distribution baffle (6) naturally covers the top of the metal arsenic sublimation distributor (3), and the tail gas condensation distribution baffle and the metal arsenic sublimation distributor are separated and not connected; the height of the exposed section of the vacuum tank extending out and exposed to the air is 1 / 4 of the height of the vacuum tank, and the material collection tray (9) is arranged at the upper portion of the exposed section.

2. The device for reducing the antimony content in industrial metal arsenic according to claim 1, characterized in that: A heat-insulating sleeve (11) is provided between the heating furnace (1) and the vacuum tank and above the charging crucible (14).

3. A device for reducing the antimony content in industrial metal arsenic according to claim 1 or 2, characterized in that: The heating furnace (1) comprises a metal shell (15) and a refractory material layer (16) built on the inner wall of the metal shell.

4. A device for reducing the antimony content in industrial metal arsenic according to claim 1 or 2, characterized in that: A support lug (5) for fixing the vacuum tank (2) is provided at the furnace opening of the heating furnace (1).

5. The method for producing the device for reducing the antimony content in industrial metal arsenic according to any one of claims 1 to 4, characterized in that: Here’s how: S1. Selecting industrial metal arsenic with an arsenic content of 97 to 99 wt% and an antimony content of 0.3 to 2 wt% as raw material, and adding the raw material to the charging crucible (14); S2. The charging crucible (14) is heated by a volatilizing inner sleeve (12), and the charging crucible is slowly heated to 500-530°C within 120-150 minutes, and then kept at a constant temperature for 50-70 minutes; then the temperature is continued to be raised to 560-580°C within 50-70 minutes, and then kept at a constant temperature for 20-22 hours; the material in the charging crucible is heated to generate arsenic vapor, and the arsenic vapor rises through the condensation diverter sieve plate (4), so that the antimony condensation is no longer volatile, and the arsenic vapor is dispersed, buffered and decelerated; Using a heat preservation jacket to keep the temperature of the metal arsenic sublimation distributor (3) at 350-400°C for 25 hours; During the heating and heat preservation process, the volatilization rate of the arsenic vapor is controlled by controlling the temperature and pressure in the vacuum tank (2); S3. The arsenic vapor rises along the metal arsenic sublimation distributor (3), and is gradually cooled when passing through a section of the vacuum tank exposed to the air. When the arsenic vapor rises to the top of the metal arsenic sublimation distributor, the exhaust gas condensation distribution baffle is lifted up by the steam pressure, and the arsenic vapor is ejected from the gap between the exhaust gas condensation distribution baffle and the metal arsenic sublimation distributor into the upper part of the condensation collection area (10), and falls into the material collection plate (9) after being condensed, thereby obtaining an industrial metal arsenic product with an arsenic content of >99.5wt% and an antimony content of <0.01wt%.

6. The production method according to claim 5, characterized in that In the above step S2, the pressure in the vacuum tank is controlled at 6-600 Pa, and the volatilization speed of arsenic vapor is controlled at 1-3 mm / s.

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