CN2661700Y - Vacuum rectifying apparatus for extracting high purity metal - Google Patents

Abstract

The utility model discloses a vacuum distillation device which extracts high pure metal. The utility model is characterized in that: the device comprises a distillation raw material reactor (1), a condense pipe (2), a diffusion pump (3), a mechanical pump (4) and a distillation product reactor (5); wherein the distillation raw material reactor is arranged at the pre-stage of the condense pipe which is arranged at the pre-stage of the distillation product reactor; the side tube of the condense pipe is communicated with the diffusion pump and the mechanical pump; each device and each part are connected into an integrity through the fitting and the electrical control circuit. The utility model has the advantages of simple structure, conveniently manufacturing and operating, large output, little pollution, high quality of products, stability and reliability, remarkable economic benefit and social benefit.

Description

Vacuum rectification device for refining high-purity metals

1. Technical field

The utility model relates to a vacuum rectification device for refining high-purity metals, which belongs to the field of smelting high-purity metal elements in the metallurgical industry.

2. Background technology

In aerospace, navigation, infrared and other fields, all kinds of high-purity metals are required as the basic raw materials for key components. Such as tellurium, cadmium, zinc, etc., which are synthetic raw materials for tellurium, cadmium, and zinc wafers used for infrared detection. Due to the process and technical requirements of the device, these metals need to have a purity of more than 5N-7N. However, the metal purity that can be achieved by traditional smelting technology is generally around 4N, and the performance of components made of this material is far from meeting the requirements. Chinese patents 00107360.5, 91104023.4, and 99115939.x report that the high-purity metals extracted by the distillation equipment are obviously far from meeting the requirements of modern technology. At present, the production of high-purity metals generally adopts wet production technology, which has disadvantages such as small output, large pollution, and unstable product quality.

3. Contents of the invention

The purpose of this utility model is to provide a vacuum rectification device for refining high-purity metals in view of the deficiencies of the prior art. .

The purpose of this utility model is achieved by the following technical measures:

The vacuum rectification device for extracting high-purity metals is composed of a rectification raw material kettle, a condensation pipe, a diffusion pump, a mechanical pump and a rectification product kettle. The rectification raw material kettle is installed at the front stage of the condensation pipe, and the condensation pipe is installed at the front stage of the rectification product kettle. The branch pipe of the condensation pipe is connected to the diffusion pump and the mechanical pump, and the various devices and devices are connected through pipe fittings and electric control lines. constitute a whole.

The rectification raw material kettle is provided with a feeding port and a condenser pipe connection, and a residual material discharge port is provided under the kettle. The feeding port and the discharging port are respectively connected with the vacuum piston valve through connecting pipes. The condensation tube is equipped with quartz packing, the rectification raw material kettle is placed in the silicon carbide tube on the heating furnace, the silicon carbide tube is equipped with a heating resistance wire and a thermocouple, the resistance wire is connected with the electric control circuit, and the furnace shell and the silicon tube are filled with heat insulation Silk protection material, the furnace shell is covered to form a rectification raw material kettle.

One end of the condensation pipe is connected to the rectification raw material tank, the other end is connected to the rectification product tank, and the branch pipe is connected in series with the diffusion pump and the mechanical pump.

The structure of the rectification product kettle is the same as that of the rectification raw material kettle. Only the condensation pipe interface and the product outlet are arranged on the rectification product kettle, and they are placed in the silicon carbide tube in the heating furnace with the same structure as before.

The rectification raw material kettle, condensation pipe, distillation product kettle and metal contact fittings are all made of quartz material.

The data acquisition, processing and parameter setting of the electronic control circuit are amplified, converted and phase-shifted by the circuit amplification, conversion and phase-shifting of the intelligent regulator LU906M and the intelligent phase-shift trigger module XJH-B1.

The utility model has the following advantages:

1. This utility model is an elemental vacuum gas-phase gap rectification device, which has the advantages of large output, low pollution and high product quality, as shown in Table 1 for details.

2. The horizontal rectification condenser simplifies the structure of the equipment, reduces the damage rate of the equipment, improves the operating efficiency of the equipment, and reduces the cost of the product.

3. It is convenient to load and discharge materials, and the vacuum piston valve, vacuum pump and rectification system are connected easily, with good sealing performance, easy maintenance and easy operation.

4. Small pollution, good working conditions, and the toxic steam produced by vacuum distillation can be discharged through the vacuum system.

4. Description of drawings

Figure 1 is a block diagram of a vacuum distillation device for refining high-purity metals.

Figure 2 is a schematic diagram of the structure of a vacuum rectification device.

1 Rectification raw material kettle, 2 Condenser pipe, 3 Diffusion pump, 4 Mechanical pump, 5 Rectification product kettle, 6 Feeding pipe, 7 Condenser pipe interface, 8 Residue discharge port, 9 Connecting pipe, 10 Piston valve, 11 Quartz packing , 12 silicon carbide tubes, 13 resistance wires, 14 thermocouples, 15 insulation materials, 16 condensation pipe interfaces, 17 product outlets.

Figure 3 is the electric control circuit diagram.

5. Specific implementation

The utility model is described in detail through the following examples, but it cannot be understood as a limitation to the protection scope of the utility model.

Example

The utility model has the advantages of simple structure and convenient manufacture, as shown in Figures 1-3.

As shown in Figure 1, the rectification raw material kettle 1, the condensation pipe 2, the diffusion pump 3, the mechanical pump 4 and the rectification product kettle 5 are composed. The rectification raw material kettle 1 is installed in the front stage of the condensation pipe 2, and the condensation pipe 2 is installed in the front stage of the rectification product kettle 5. The branch pipe of the condensation pipe 2 is connected with the diffusion pump 3 and the mechanical pump 4. Lines connect devices and devices to form a whole.

As shown in Figure 2, the rectification raw material kettle 1 is provided with a feeding port and a condensation pipe interface, and a residual material discharge port 8 is provided under the kettle. The feeding port and the discharging port are respectively connected to the vacuum piston valve 10 through the connecting pipe 9, and the condensing pipe is equipped with a quartz filler 11; the rectification raw material kettle is placed in the silicon carbide tube 12 on the heating furnace, and a heating resistance wire is installed outside the silicon tube. A heating resistance wire 13 and a thermocouple 14 are installed outside the silicon tube and connected to an electric control circuit. An insulating wire insulation material 15 is filled between the silicon tube and the furnace shell, and the furnace shell is covered to form a rectification raw material kettle.

One end of the condensation pipe 2 is connected to the rectification raw material kettle, and the other end is connected to the distillation product kettle 5, and the branch pipe of the condensation pipe 2 is connected in series with a diffusion pump and a mechanical pump.

The structure of the distillation product kettle 5 is the same as the rectification raw material kettle, only the condensation pipe interface and the product discharge port 17 are arranged on the rectification product kettle, and placed in the silicon carbide tube in the heating furnace with the previous structure.

The rectification raw material kettle, condensation pipe, distillation product kettle and metal contact fittings are all made of quartz material.

As shown in Figure 3, the data acquisition, processing and parameter setting of the electronic control circuit are all completed independently through the industrial intelligent regulator LU906M. The thermocouple signal is input from pins 10 and 11. After internal processing, the amplified control signal is from 15, 16-pin output, XJH-B1 is a product produced and sold by Sichuan Xinju Mining Resources Development Co., Ltd., an intelligent thyristor phase-shift trigger module, and the 4-20mA control current signal is input from the 6 and 7 corners of the module. The internal circuit is amplified, and the converted phase shift trigger signal is output through corners 3 and 4 to directly drive the thyristors K1 and K2 to conduct and provide control current to the load _RL .

In the figure, R ₁ is the current limiting resistor, and R ₂ and capacitor C form a resistance-capacitance absorption circuit.

The working principle of the rectification device for refining high-purity metals is to use the characteristics of different vapor pressures of different metal elements at a certain temperature, and at the same time use the filler in the condensation to continuously condense other metals, and exchange heat and mass with gaseous metals to make the high boiling point The impurities are condensed and deposited, and flow back into the rectification raw material kettle, and the low-boiling point impurities are removed by a vacuum device, so as to achieve the purpose of separating metals and impurities. Rectification of high-purity metals is carried out at a vacuum degree of 1×10 ^-2 ~ 1×10 ^-3 Pa, at a temperature higher than the melting point of the metal at room temperature, through one rectification, and the temperature of the rectification raw material tank and the temperature of the condenser are strictly controlled. , The temperature of the rectification product kettle, the temperature error is ±0.2%, and it is realized by strictly controlling the reflux ratio under the auxiliary vacuum condition.

Table 1 Selenium produced by the utility model and the analysis and comparison of selenium produced by prior art ^*

^* Se specification 5N, unit ppm.

Claims (6)

1, the vacuum rectifying apparatus of refining hihg purity metal, it is characterized in that this vacuum rectifying apparatus is made up of rectifying raw material still (1), prolong (2), diffusion pump (3), mechanical pump (4) and rectifying product still (5), rectifying raw material still is installed in the prime of prolong, prolong is installed in the prime of rectifying product still, the prolong arm is connected conducting with diffusion pump, mechanical pump, by pipe fitting and automatically controlled circuit each device and device is connected and composed integral body.

2, the vacuum rectifying apparatus of refining hihg purity metal according to claim 1, it is characterized in that offering on the rectifying raw material still (1) charging opening (6) and prolong (7), have defective material discharge outlet (8) under the rectifying raw material still, charging opening is connected with vacuum piston valve (10) by pipe connecting (9) respectively with discharge gate, and quartz filler (11) is housed in the prolong; Rectifying raw material still is placed in the carborudum tube (12) on the process furnace, carborudum tube is installed resistive heater (13) outward and is connected with thermopair (14) and with automatically controlled circuit, the adiabatic silk of filling is protected material (15) between furnace shell and the silicone tube, and furnace shell is added a cover the back and constituted rectifying raw material still.

3, the vacuum rectifying apparatus of refining hihg purity metal according to claim 1 is characterized in that an end of prolong (2) is connected with rectifying raw material still, and the other end is connected with rectifying product still, and the arm of prolong (2) and diffusion pump and mechanical pump are connected in series.

4, the vacuum rectifying apparatus of refining hihg purity metal according to claim 1, the structure and the rectifying raw material still (1) that it is characterized in that rectifying product still (5) are identical, only establish prolong interface (16) and outlet for product (17) on the rectifying product still, and be placed on in the carborudum tube in the process furnace of pre-structure.

5, the vacuum rectifying apparatus of refining hihg purity metal according to claim 1 is characterized in that the pipe fitting of rectifying raw material still, prolong, rectifying product still and metallic contact is quartz material.

6, the vacuum rectifying apparatus of refining hihg purity metal according to claim 1 is characterized in that the data gathering of automatically controlled circuit, handles and automatically controlled circuit that parameter setting is made up of industrial intelligent adjusting apparatus and intelligent phase shift trigger module is finished.

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