A vacuum distillation apparatus

Abstract

The present application belongs to the technical field of high-purity metal preparation, and particularly relates to a vacuum distillation device. The vacuum distillation furnace body is sequentially provided with an evaporation zone, a condensation zone and a melting zone from bottom to top. The evaporation zone is provided with a reflux plate. The condensation zone is provided with a gas guide pipe, a condensation disc, a flow guide pipe and a liquid seal assembly. The flow guide pipe is inserted into the gas guide pipe. The liquid seal assembly is provided with a liquid lithium valve on a liquid seal pipeline. The melting zone is provided with a cone valve and a feed inlet. The vacuum distillation furnace body is located in a heating furnace chamber. The vacuum distillation furnace body is in communication with a vacuum ingot casting box. The vacuum ingot casting box is provided with a crucible, a rotating unit, a motor and heating fins. The present application purifies lithium metal by using a vacuum distillation method, and realizes the preparation of high-purity lithium metal.

Description

Technical Field

[0001] This invention belongs to the field of high-purity metal preparation technology, specifically relating to a vacuum distillation apparatus. Background Technology

[0002] The unique properties of lithium metal make it play a crucial role in the nuclear industry, and the purity requirements for lithium metal have gradually increased with the development of the nuclear industry. Traditional refining methods generally involve filtration and oil refining, which are ineffective at removing non-metallic impurities from the metal, and the waste oil generated by oil refining pollutes the environment. Currently, high-purity lithium metal can be prepared using vacuum distillation. This method involves further vacuum distillation of the metal after sedimentation filtration, utilizing the difference in saturated vapor pressure to separate lithium metal from impurities, thereby producing high-purity lithium metal. Summary of the Invention

[0003] The purpose of this invention is to provide a vacuum distillation apparatus that can directly obtain metallic lithium of Li-2 or higher without generating any waste gas or waste oil, and has the characteristics of being pollution-free and low-cost.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0005] A vacuum distillation apparatus comprises, from bottom to top, an evaporation zone, a condensation zone, and a melting zone. The evaporation zone is equipped with a reflux plate. The condensation zone is equipped with a gas guide pipe, a condensation disc, a flow guide pipe, and a liquid seal assembly. The flow guide pipe is inserted into the gas guide pipe, and a liquid lithium valve is installed on the liquid seal pipe of the liquid seal assembly. The melting zone is equipped with a cone valve and a feed inlet. The vacuum distillation furnace body is located in a heating furnace chamber. The vacuum distillation furnace body is connected to a vacuum ingot casting box, which is equipped with a crucible, a rotating unit, a motor, and heating fins.

[0006] The reflux plate is circular.

[0007] The reflux plates are staggered and welded in the evaporation zone.

[0008] The reflow plate spacing is 40-80mm.

[0009] The number of reflux plates is 4-8.

[0010] The reflux plate is tilted at an angle of 3-10°.

[0011] The depth of the guide tube inserted into the air guide tube is 15-30mm.

[0012] The tilt angle of the condenser disk is 5-15°.

[0013] The heating furnace chamber consists of a lower furnace chamber and an upper furnace chamber from bottom to top, and the heating fin temperature is 300-400℃.

[0014] Liquid or solid metal is placed from the melting zone into the evaporation zone for vacuum distillation. The metal condenses on the outer wall of the gas delivery tube and is then deposited on a condensation disk to obtain high-purity lithium metal. The vacuum distillation temperature is 650-800℃, the vacuum degree is 0.1-50Pa, and the distillation time is 5-8h.

[0015] The beneficial effects achieved by this invention are as follows:

[0016] High-purity lithium metal was prepared by purifying it using vacuum distillation. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of a vacuum distillation apparatus;

[0018] In the diagram: 1-Vacuum distillation furnace body; 2-Conical valve; 3-Feed inlet; 4-Upper furnace chamber; 5-Lower furnace chamber; 6-Thermocouple; 7-Gas guide pipe; 8-Condensing disc; 9-Flow guide pipe; 10-Reflux plate; 11-Insulation cotton; 12-Liquid seal assembly; 13-Liquid lithium valve; 14-Vacuum casting box; 15-Crucible; 16-Rotating unit; 17-Motor; 18-Heating fins; 19-Vacuum unit. Detailed Implementation

[0019] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0020] A vacuum distillation apparatus includes a vacuum distillation furnace body 1, a vacuum casting box 14, and a vacuum unit 19. The vacuum distillation furnace body 1 comprises, from bottom to top, an evaporation zone, a condensation zone, and a melting zone. The evaporation zone is equipped with reflux plates 10, which are circular and staggered in the evaporation zone with a spacing of 40-80 mm, a number of plates of 4-8, and an inclination angle of 3-10°. The condensation zone is equipped with a gas guide pipe 7, a condensation disc 8, a flow guide pipe 9, and a liquid seal assembly 12. The flow guide pipe 9... Inserted into the gas guide pipe 7, the insertion depth is 15-30mm, the tilt angle of the condensing disc 8 is 5-15°, and the liquid seal pipe of the liquid seal assembly 12 is equipped with a liquid lithium valve 13; the melting zone is equipped with a cone valve 2 and a feed port 3; the heating furnace is divided into two areas, from bottom to top: the lower furnace chamber 5 and the upper furnace chamber 4; the vacuum ingot casting box 14 is equipped with a crucible 15, a rotating unit 16, a motor 17 and heating fins 18, and the temperature of the heating fins 18 is 300-400℃.

[0021] A method for preparing high-purity lithium metal includes the following steps: placing liquid or solid metal (melted in a melting zone) from the melting zone into an evaporation zone, performing vacuum distillation, condensing on the outer wall of a gas delivery tube, and obtaining high-purity lithium metal on a condensation disk. The vacuum distillation temperature is 650-800℃, the vacuum degree is 0.1-50Pa, and the distillation time is 5-8h.

[0022] A vacuum distillation apparatus includes a vacuum distillation furnace body, a vacuum casting box, and a vacuum unit. The furnace body, from bottom to top, comprises an evaporation zone, a condensation zone, and a melting zone. The evaporation zone is equipped with reflux plates, which are circular and staggered, welded together at intervals of 40-80 mm, with 4-8 plates and an inclination angle of 3-10°. The condensation zone includes a gas guide pipe, a condensation disc, a flow guide pipe, and a liquid seal assembly. The flow guide pipe is inserted into the gas guide pipe, and the condensation disc has an inclination angle of 5-15°. A liquid lithium valve is installed on the liquid seal pipe. The melting zone includes a cone valve and a feed inlet. The heating furnace chamber is divided into two areas, from bottom to top: a lower furnace chamber and an upper furnace chamber. The vacuum casting box contains a crucible, a rotating unit, a motor, and heating fins, with the heating fins operating at a temperature of 300-400°C.

[0023] A method for preparing high-purity lithium metal includes the following steps: placing liquid or solid metal (melted in a melting zone) from the melting zone into an evaporation zone, performing vacuum distillation, condensing on the outer wall of a gas delivery tube, and obtaining high-purity lithium metal on a condensation disk. The vacuum distillation temperature is 650-800℃, the vacuum degree is 0.1-50Pa, and the distillation time is 5-8h.

[0024] A vacuum distillation apparatus includes a vacuum distillation furnace body, a vacuum casting box, and a vacuum unit.

[0025] The furnace body consists of an evaporation zone, a condensation zone, and a melting zone from bottom to top. The evaporation zone is equipped with reflux plates. The reflux plates are circular and staggered in the evaporation zone with a spacing of 60mm and a total of 6 plates. The tilt angle is 5°, which ensures that impurities are condensed on the reflux plates, ensures that the metal discharge rate meets the actual requirements, and saves costs.

[0026] The condensation zone is equipped with a gas guide pipe, a condensation disc, a flow guide pipe, and a liquid seal assembly. The flow guide pipe is inserted into the gas guide pipe to a depth of 20mm to ensure that the liquid metal does not flow into the condensation disc when it is discharged from the melting zone, while ensuring that the metal vapor is fully cooled to avoid affecting the cone valve.

[0027] The condensation disc is tilted at a 10° angle to effectively ensure condensation reflux, and a liquid lithium valve is installed on the liquid seal pipeline for quantitative ingot casting;

[0028] The melting zone is equipped with a cone valve and a feed inlet;

[0029] The heating furnace is divided into two areas, from bottom to top: the lower furnace chamber and the upper furnace chamber.

[0030] The vacuum casting box is equipped with a crucible, a rotating unit, a motor, and heating fins, with the heating fins having a temperature of 350℃.

[0031] A method for preparing high-purity lithium metal: 50.8 kg of solid metal is melted in a melting zone and then placed in an evaporation zone for vacuum distillation. The vacuum distillation temperature is 700℃, the vacuum degree is 1 Pa, and the distillation time is 7.2 h.

[0032] The test results showed that the direct metal recovery rate of the ingot was 42.9 kg, with a recovery rate of 84.5%. The impurity situation is shown in Table 1.

[0033] Table 1 Chemical composition of metals

[0034]

[0035] After melting 51.2 kg of solid metal in the melting zone, it was placed in the evaporation zone for vacuum distillation. The vacuum distillation temperature was 750℃, the vacuum degree was 5 Pa, and the distillation time was 5.8 h.

[0036] The test results showed that the direct metal recovery rate of the ingot was 42.8 kg, with a recovery rate of 83.7%. The impurity situation is shown in Table 2.

[0037] Table 2 Chemical composition of metals

[0038]

[0039]

Claims

1. A vacuum distillation apparatus, characterized in that: The vacuum distillation furnace body consists of an evaporation zone, a condensation zone, and a melting zone from bottom to top. The evaporation zone is equipped with a reflux plate. The condensation zone is equipped with a gas guide pipe, a condensation disc, a flow guide pipe, and a liquid seal assembly. The flow guide pipe is inserted into the gas guide pipe, and a liquid lithium valve is installed on the liquid seal pipe of the liquid seal assembly. The melting zone is equipped with a cone valve and a feed inlet. The vacuum distillation furnace body is located in the heating furnace chamber. The vacuum distillation furnace body is connected to a vacuum ingot casting box, which contains a crucible, a rotating unit, a motor, and heating fins.

2. The vacuum distillation apparatus according to claim 1, characterized in that: The reflux plate is circular.

3. The vacuum distillation apparatus according to claim 1, characterized in that: The reflow plates are staggered and welded in the evaporation zone.

4. The vacuum distillation apparatus according to claim 1, characterized in that: The reflow plate spacing is 40-80mm.

5. The vacuum distillation apparatus according to claim 1, characterized in that: The number of reflux plates is 4-8.

6. The vacuum distillation apparatus according to claim 1, characterized in that: The reflux plate is tilted at an angle of 3-10°.

7. The vacuum distillation apparatus according to claim 1, characterized in that: The depth of the guide tube inserted into the air guide tube is 15-30mm.

8. The vacuum distillation apparatus according to claim 1, characterized in that: The tilt angle of the condenser disk is 5-15°.

9. The vacuum distillation apparatus according to claim 1, characterized in that: The heating furnace chamber consists of a lower furnace chamber and an upper furnace chamber from bottom to top, and the heating fin temperature is 300-400℃.

10. The vacuum distillation apparatus according to claim 1, characterized in that: Liquid or solid metal is placed from the melting zone into the evaporation zone for vacuum distillation. The metal condenses on the outer wall of the gas delivery tube and is then deposited on a condensation disk to obtain high-purity lithium metal. The vacuum distillation temperature is 650-800℃, the vacuum degree is 0.1-50Pa, and the distillation time is 5-8h.

Images