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A method and device for continuous distillation and purification of tungsten hexafluoride

A tungsten hexafluoride and rectification technology, which is applied in tungsten halide, vacuum distillation, etc., can solve the problems of low production efficiency, high cost, and difficult application

Active Publication Date: 2016-04-13
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The tungsten hexafluoride is condensed at low temperature by condensation and vacuum pumping method, and the condensed tungsten hexafluoride liquid is solidified at 0°C, and the gas phase impurities are removed by vacuuming at the same time; then the tungsten hexafluoride is heated under pressure in a closed container, Make the gas dissolved in liquid tungsten hexafluoride overflow due to the decrease in solubility, and remove the non-volatile impurities by gas-phase pressure relief under controlled conditions, and then remove HF and SF 6 and CF 4 and other volatile impurities, and finally remove N 2 , Ar and other volatile impurities dissolved in liquid tungsten hexafluoride. This method has simple process and low production cost, but it is difficult to produce high-purity products
[0004] The batch rectification method performs rectification operation on the tungsten hexafluoride to be purified in batches. This method can overcome the defects of the above two methods and can obtain high-purity products, but the low production efficiency leads to high cost, and it is difficult to produce on a large scale. middle application

Method used

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  • A method and device for continuous distillation and purification of tungsten hexafluoride
  • A method and device for continuous distillation and purification of tungsten hexafluoride
  • A method and device for continuous distillation and purification of tungsten hexafluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093] Raw materials: the content of tungsten hexafluoride gas to be purified is 99.95%, and the content of impurities is shown in Table 1, which shows the content of impurities in the raw materials used in Example 1 of the present invention.

[0094] The impurity content in the raw material that table 1 embodiment of the present invention 1 adopts

[0095] components

[0096] Distillation unit: using figure 1 In the rectification device of the shown structure, wherein, the light removal tower 3 is 3000mm high, 500mm in diameter, and the number of trays is 30, with a built-in diameter of 5mm stainless steel θ ring packing; the weight removal tower 11 is 3000mm high, 500mm in diameter, and the number of trays is 40, Built-in diameter 5mm stainless steel θ ring packing. The body of light removal tower 3 and weight removal tower 11 as well as the reboiler, condenser and piping are made of stainless steel.

[0097] Distillation process:

[0098] Step 1: If figure 1 A...

Embodiment 2

[0107] Raw material: the content of tungsten hexafluoride gas to be purified is 99.99%, and the content of impurities is shown in Table 3, which shows the content of impurities in the raw materials used in Example 2 of the present invention.

[0108] The impurity content in the raw material that table 3 embodiment of the present invention 2 adopts

[0109] components

N 2

o 2 +Ar

CO

CO 2

SF 6

SiF 4

CF 4

MoF 6

N 2 o

HF

Content (×10 -6 )

10

8

9

4

3

2

7

12

5

35

[0110] Distillation unit: using figure 1 The rectification device of the shown structure, wherein, the weight removal tower 3 is 0.5m high, 0.1m in diameter, the number of trays is 20, and the built-in diameter is 1mm polytetrafluoroethylene Raschig ring packing; the weight removal tower 11 is 0.5m high, and the diameter is 0.1 m, the number of trays is 20, and the built-in PTFE Raschig ring packing with...

Embodiment 3

[0120] Raw material: the content of tungsten hexafluoride gas to be purified is 99%, and the impurity content is shown in Table 5, and Table 5 shows the impurity content in the raw material used in Example 3 of the present invention.

[0121] The impurity content in the raw material that table 5 embodiment of the present invention 3 adopts

[0122] components

N 2

o 2 +Ar

CO

CO 2

SF 6

SiF 4

CF 4

MoF 6

N 2 o

HF

Content (×10 -6 )

2500

1800

900

400

300

200

700

1200

500

1500

[0123] Distillation unit: using figure 1 In the rectification device of the shown structure, wherein, the weight removal tower 3 is 15000mm high, 3000mm in diameter, and the number of trays is 80, with a built-in diameter of 100mm stainless steel Pall ring packing; the weight removal tower 11 is 15000mm high, 3000mm in diameter, and the number of trays is 80, built-in diameter 100mm stainles...

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Abstract

Provided are a device and method for purifying tungsten hexafluoride by means of continuous rectification. The device comprises a light component removal tower (3) and a heavy component removal tower (11). The method comprises the steps of: conveying tungsten hexafluoride to be purified to the light component removal tower (3) for rectification, conveying products at the bottom of the light component removal tower to the heavy component removal tower (11) for rectification, and collecting the purified tungsten hexafluoride on the top of the heavy component removal tower. The purity of the tungsten hexafluoride obtained by using the method can reach 99.9999%. The method is simple to operate, has relatively high yield, and reduces the cost.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method and device for continuous rectification and purification of tungsten hexafluoride. Background technique [0002] Tungsten hexafluoride (WF 6 ) is a widely used gas. It is mainly used in the electronics industry as a raw material for metal tungsten chemical vapor deposition (CVD) process. Tungsten deposited by CVD process has low resistivity, high resistance to electromigration and filling Excellent flatness and other advantages when small through holes. The composite coating of tungsten and rhenium is prepared by the CVD process of mixed metals, which can be used in the manufacture of X-ray emitting electrodes and solar absorbers. In addition, WF 6 In the electronics industry, it is also used as a raw material for semiconductor electrodes and conductive pastes. The above applications require high purity of tungsten hexafluoride to ensure the stability and relia...

Claims

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Application Information

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IPC IPC(8): B01D3/10
CPCC01G41/04
Inventor 柳彤王占卫张长金李翔宇郑秋艳董云海冀延治
Owner PERIC SPECIAL GASES CO LTD
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