Device for improving germanium deposition rate of residual acid

Abstract

The utility model discloses a device for improving the germanium deposition rate of residual acid, and belongs to the technical field of germanium tetrachloride production processes. The device comprises a carbon steel lining teflon jacket kettle, the carbon steel lining teflon jacket kettle comprises an inner kettle and a jacket, the inner kettle is arranged in the jacket, a gap is reserved between the outer wall of the inner kettle and the inner wall of the jacket, the top of the inner kettle is sealed through a flange cover, a residual acid inlet, a tail gas outlet and an observation hole are formed in the flange cover, and a residual acid outlet is formed in the middle of the side face of the inner kettle. A material outlet is formed in the bottom of the inner kettle, cooling water outlets are formed in two sides of the jacket, and a cooling water inlet is formed in the bottom of the jacket. The device can prevent high-temperature, volatile and highly corrosive germanium tetrachloride-containing residual acid from volatilizing into a tail gas absorption tower, can also prevent economic loss caused by volatilization of germanium tetrachloride due to corrosion and damage of a container, and can quickly lower the temperature of the residual acid to quickly separate out germanium tetrachloride and improve the re-evaporation recovery rate; and the risk that the germanium tetrachloride-containing residual acid volatilizes in the air to damage the environment and hurt people can be prevented.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the production process technical field of germanium tetrachloride, and particularly relates to a device for safely and environmentally protecting and rapidly reducing the temperature of high-temperature residual acid and timely precipitating germanium tetrachloride contained in the residual acid. BACKGROUND

[0002] The existing residual acid containing vessel device is a PP material round self-made welded barrel, a DN400mm PP pipe is adopted, and both ends are sealed and welded by PP plates. A hole is punched in one end of the PP plate to insert a residual acid pipeline and a tail gas pipeline, a pump is linked in the lower part of the barrel to pump away the residual acid, and a part of space is reserved at the bottom to contain germanium tetrachloride. The residual acid discharged by the existing process reboiling section has a temperature of about 50 DEG C, the high temperature is easy to cause leakage of the PP material for long-time containing, loss is caused, the service life is too short, and inconvenience is brought to inspection and maintenance; meanwhile, the high-temperature residual acid containing germanium tetrachloride is not easy to precipitate and is treated with the residual acid, germanium tetrachloride is taken away, and direct economic loss is caused. The high-temperature residual acid discharged needs a long time for natural cooling, the hot acid has strong volatility, pressure is brought to environmental protection, and the containing vessel is easy to be corroded to cause leakage; the existing containing vessel does not have an observation hole, the lower germanium tetrachloride exceeds the residual acid pump outlet, is treated with the residual acid, and yield reduction is caused. The residual acid containing vessel is full, and it cannot be determined that the residual acid overflows to cause harm to the operator. The existing device precipitates germanium tetrachloride in the bottom layer and needs to be pumped out by vacuum, a vacuum unit needs to be started, the large vacuum suction force takes away part of the germanium tetrachloride, causes germanium tetrachloride loss, and the germanium tetrachloride enters the vacuum unit to cause corrosion and damage of the vacuum unit. The hole punched by oneself is used as a residual acid inlet, a tail gas outlet, a vacuum pumping outlet and a residual acid discharge port in the middle of the barrel, the sealing performance is poor, a small part of residual acid gas volatilization causes harm to equipment, personnel and environment. CONTENT OF THE UTILITY MODEL

[0003] The utility model provides a device for improving residual acid germanium precipitation rate, aims at solving the problems that the existing containing vessel is easy to be corroded and damaged by residual acid, residual acid temperature is too high to precipitate germanium tetrachloride contained in the residual acid in time, and provides a device for safely and environmentally protecting and rapidly improving residual acid germanium precipitation rate.

[0004] A device for improving residual acid germanium precipitation rate, characterized by comprising a carbon steel lining tetrafluoro jacketed kettle, the carbon steel lining tetrafluoro jacketed kettle comprises an inner kettle and a jacket, the inner kettle is arranged in the jacket, a space is reserved between the outer wall of the inner kettle and the inner wall of the jacket, the top of the inner kettle is sealed by a flange cover, a residual acid inlet, a tail gas outlet and an observation hole communicating with the inside of the inner kettle are arranged on the flange cover, a circular pressure-resistant tempered glass is covered on the observation hole and is pressed tightly by a flange; a residual acid outlet communicating with the inside of the inner kettle is arranged on the middle of the side of the inner kettle, and the outer end of the residual acid outlet is on the outside of the jacket; a material outlet communicating with the inner kettle is arranged on the bottom of the inner kettle, and the outer end of the material outlet is on the outside of the jacket; cooling water outlets communicating with the inside of the jacket are arranged on both sides of the jacket, and a cooling water inlet communicating with the inside of the jacket is arranged on the bottom of the jacket.

[0005] Further, the residual acid inlet, material outlet and tail gas outlet are all DN25mm lined with a fluorotube, and a flange cover is provided.

[0006] Further, the tail gas outlet is provided in a number of two.

[0007] Further, the observation hole is a DN250mm tube.

[0008] The beneficial effects of the present application are as follows: the inner kettle lined with fluorine can prevent corrosion of residual acid and germanium tetrachloride, and cooling water is injected from the kettle bottom into the jacket, flows out from the highest part of the inner kettle for circulation cooling, and ensures that cooling water circulates in the entire jacket at any time, which is beneficial to the precipitation of germanium tetrachloride by rapidly reducing the temperature of residual acid. The observation hole can clearly observe the liquid level in the kettle, and the excess residual acid can be removed in time to prevent the liquid level from being too high and causing residual acid to overflow and corrode the equipment and environment. The precipitated germanium tetrachloride flows out from the material outlet at the bottom of the inner kettle, reduces the use of a vacuum unit, reduces environmental pressure, reduces the vacuum extraction of germanium tetrachloride, and improves the comprehensive recovery rate of the reboiling section. Resource waste and direct economic losses are avoided. The overall operating environment is improved, and damage to personnel and the environment is reduced; the residual acid inlet, residual acid outlet, tail gas outlet, cooling water inlet, cooling water outlet and material outlet are all sealed by flanges. BRIEF DESCRIPTION OF DRAWINGS

[0009] Figure 1 It is a device structure diagram for improving the residual acid germanium precipitation rate.

[0010] Wherein: 1-inner kettle, 2-jacket, 3-residual acid inlet, 4-residual acid outlet, 5-tail gas outlet, 6-observation hole, 7-cooling water inlet, 8-cooling water outlet, 9-material outlet. DETAILED DESCRIPTION

[0011] Embodiment 1: A device for improving the residual acid germanium precipitation rate, comprising a carbon steel inner kettle lined with a fluorine jacket, the carbon steel inner kettle lined with a fluorine jacket comprising an inner kettle 1 and a jacket 2, the inner kettle 1 being arranged in the jacket 2, a space being left between the outer wall of the inner kettle 1 and the inner wall of the jacket 2, the top of the inner kettle 1 being sealed by a flange cover, and a residual acid inlet 3, a tail gas outlet 5 and an observation hole 6 being arranged on the flange cover to communicate with the inside of the inner kettle, a circular pressure-resistant tempered glass being arranged on the observation hole 6 and being pressed tightly by a flange. A residual acid outlet 4 is arranged on the side of the inner kettle 1 to communicate with the inside of the inner kettle, and the outer end of the residual acid outlet 4 is arranged outside the jacket 2. A material outlet 9 is arranged at the bottom of the inner kettle 1 to communicate with the inner kettle, and the outer end of the material outlet 9 is arranged outside the jacket 2. Cooling water outlets 8 are arranged on both sides of the jacket 2 to communicate with the inside of the jacket 2, and a cooling water inlet 7 is arranged at the bottom of the jacket 2 to communicate with the inside of the jacket 2. The residual acid inlet 3, the residual acid outlet 4, the tail gas outlet 5, the cooling water inlet 7, the cooling water outlet 8 and the material outlet 9 are all sealed by flanges.

[0012] When in use, the high-temperature residual acid containing germanium tetrachloride is discharged into the inner kettle 1, the jacket 2 is always filled with cooling water through the cooling water inlet 7 and discharged from the cooling water outlet 8 to realize the cooling water circulation, rapidly reduce the temperature of the residual acid in the inner kettle 1, and be beneficial to the rapid precipitation of germanium tetrachloride in the residual acid and reduce the loss of high-temperature volatilization. Meanwhile, the inner kettle 1 can be loaded for a long time to avoid corrosion and damage. The flanges are used for connecting the various connecting parts to ensure the sealing effect, prevent the residual acid gas from volatilizing into the air, corrode the equipment and pollute the working environment. The observation hole 6 is used for timely understanding the material and residual acid liquid level in the kettle, convenient and timely recovery, and avoiding the material loss caused by improper operation. The bottom material outlet can avoid the material loss and economic loss caused by the use of the vacuum unit. The rapid reduction of the residual acid temperature can achieve the purpose of rapidly precipitating germanium to improve the comprehensive recovery rate of the re-distillation section.

Claims

1. An apparatus for improving the germanium precipitation rate of residual acid, characterized in that: The carbon steel lining Teflon jacketed kettle comprises an inner kettle and a jacket, the inner kettle is arranged in the jacket, a space is left between the outer wall of the inner kettle and the inner wall of the jacket, the top of the inner kettle is sealed by a flange cover, a residual acid inlet, a tail gas outlet and an observation hole which are connected with the inside of the inner kettle are arranged on the flange cover, a circular pressure-resistant tempered glass is arranged on the observation hole and is pressed by a flange; a residual acid outlet which is connected with the inside of the inner kettle is arranged on the middle of the side of the inner kettle, the outer end of the residual acid outlet is outside the jacket; a material outlet which is connected with the inner kettle is arranged on the bottom of the inner kettle, the outer end of the material outlet is outside the jacket; cooling water outlets which are connected with the inside of the jacket are arranged on both sides of the jacket, a cooling water inlet which is connected with the inside of the jacket is arranged on the bottom of the jacket.

2. The device for improving the rate of germanium deposition from residual acid according to claim 1, wherein The residual acid inlet, the material outlet and the tail gas outlet are all DN25mm lining Teflon pipes.

3. The apparatus of claim 1, wherein the apparatus is characterized by The number of the tail gas outlets is two.

4. The apparatus of claim 1, wherein the apparatus is characterized by The observation hole is a DN250mm pipe.

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