Hydrogen bromide purifying device and method

A purification method, hydrogen bromide technology, applied in directions such as hydrogen bromide, bromine/hydrogen bromide, etc., can solve problems such as difficulty in realizing industrialized continuous production, adsorbent desorption, difficulty in recovery, and no more than 2 ppm, etc. Small investment, reduced corrosion resistance requirements, and the effect of reducing dosage

Pending Publication Date: 2020-04-10
PERIC SPECIAL GASES CO LTD
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  • Abstract
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Problems solved by technology

[0003] Chinese patent application 95191144.9 uses crude hydrogen bromide to produce high-purity hydrogen bromide with a purity of 99.999% through continuous rectification. The moisture content is all above 10ppm, and the method has certain limitations
The adsorption method has low requirements on equipment and has a good effect on water treatment. However, molecular sieves and silica gel materials are mostly used as adsorbents at present, which are easy to absorb a certain amount of hydrogen bromide, and the heat release is relatively large when the water content is high. Larger, even can reach above 100 ℃, bringing greater safety hazards
In addition, it is difficult to desorb and recover the adsorbent, which is basically replaced, and the gas in the pipeline needs to be replaced before and after the replacement, resulting in a large waste of materials and time, affecting the actual production capacity
[0004] Other processes involving water removal, such as concentrated sulfuric acid method, chemical reaction adsorption method or phosphorus tribromide spray absorption (Chinese patent application 201310220850.8), are affected by adsorption balance or the introduction of new media, and it is difficult to completely realize industrial continuous production

Method used

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  • Hydrogen bromide purifying device and method
  • Hydrogen bromide purifying device and method

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Experimental program
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Effect test

Embodiment 1

[0043] In this embodiment, the weight removal tower 1 and the light removal tower 2 are packed towers, the weight removal tower 1 is 8m high, 0.5mm in diameter, 40 theoretical plates, and has a built-in diameter of 5mm θ ring packing. Among them, the light removal tower 2 is 8m high, 0.5mm in diameter, 30 theoretical plates, and has a built-in 5mm diameter θ ring packing. The feed pipeline and de-weight tower 1 are made of Hastelloy, and the de-light tower 2, product collector 3 and filling bottle 6 are made of stainless steel. Filling pump 5 adopts diaphragm pump.

[0044] The hydrogen bromide crude product flow rate is 30L / min.

[0045] The parameters of weight removal column 1 are set as follows: column temperature -15°C, pressure 0.9MPa, reflux ratio 20. In this state, the hydrogen bromide vaporizes and rises, and the heavy components such as water condense and collect in the bottom of the de-weighting tower in liquid or solid form to realize the removal of heavy compone...

Embodiment 2

[0049] In this embodiment, the weight removal tower 1 is 14 mm high, 1 m in diameter, 60 theoretical plates, and has a built-in Pall ring packing with a diameter of 25 mm. Light removal tower 2 is 14m high, 1m in diameter, 60 theoretical plates, and has a built-in Raschig ring packing with a diameter of 25mm. The feed pipeline and weight removal tower 1 are made of Hastelloy. Bottling 6 is in stainless steel. Filling pump 5 adopts diaphragm pump.

[0050] The hydrogen bromide crude product flow rate is 30L / min.

[0051] The parameters of weight removal tower 1 are set as follows: column temperature -64°C, pressure 0 MPa, reflux ratio 80.

[0052] The parameters of light removal tower 2 are set as follows: column temperature -70°C, pressure 0 MPa, reflux ratio 200.

[0053] After testing, the main components and contents of hydrogen bromide after purification are shown in Table 2.

Embodiment 3

[0055] In this embodiment, the weight removal tower 1 is 6 mm high, 0.1 m in diameter, 40 theoretical plates, and has a built-in Pall ring packing with a diameter of 3 mm. Light removal tower 2 is 6m high, 0.1m in diameter, 30 theoretical plates, and has a built-in Raschig ring packing with a diameter of 3mm. The filling bottle 6 is made of stainless steel. Filling pump 5 adopts diaphragm pump.

[0056] The hydrogen bromide crude product flow rate is 30L / min.

[0057] The parameters of weight removal tower 1 are set as follows: column temperature 30°C, pressure 2.3MPa, reflux ratio 80.

[0058] The parameters of light removal tower 2 are set as follows: column temperature 20°C, pressure 2.3MPa, reflux ratio 280.

[0059] After testing, the main components and contents of hydrogen bromide after purification are shown in Table 2.

[0060] Table 2

[0061]

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Abstract

The intention relates to a hydrogen bromide purifying device and method, and belongs to the technical field of fine chemical engineering. A hydrogen bromide crude product enters a heavy component removal tower from a heavy component removal tower feeding hole through a feeding pipeline to be rectified, heavy component impurities are removed from the tower bottom of the heavy component removal tower, hydrogen bromide in which the heavy component impurities are removed is discharged from a heavy component removal tower discharging hole and then enters a light component removal tower to be rectified through a light component removal tower feeding hole, light component impurities are removed from the tower top of the light component removal tower, hydrogen bromide in which the light componentimpurities are removed is discharged from a light component removal tower discharging hole and then enters a product collector through a feed port of the product collector, and liquid-phase hydrogen bromide is detected; the hydrogen bromide collected by the feeding port of the product collector is collected; the hydrogen bromide in the product collector is heated after the detection is qualified,and the liquid-phase hydrogen bromide passes through a filling pump along a filling pipeline led out from bottom to top in the product collector and then enters a filling bottle. The hydrogen bromidepurifying device is simple in process, small in equipment investment, low in energy consumption, small in environmental pollution, good in economical efficiency and easy to realize industrial production.

Description

technical field [0001] The invention relates to a hydrogen bromide purification device and method, belonging to the technical field of fine chemicals. Background technique [0002] Hydrogen bromide has become an indispensable raw material gas for polysilicon etching of 8-inch and 12-inch chips because of its high selectivity to etching raw materials and precise control of etching shape and angle. One of the core gases in the production process. However, hydrogen bromide is highly corrosive, especially in the presence of moisture, which is more corrosive and can corrode most metal products. Therefore, the purification of hydrogen bromide, especially the removal of water, is the key to process control. [0003] Chinese patent application 95191144.9 uses crude hydrogen bromide to produce high-purity hydrogen bromide with a purity of 99.999% through continuous rectification. The water content is above 10ppm, and the method has certain limitations. The adsorption method has l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/09
CPCC01B7/093
Inventor 闫达柳彤徐海云张明杰沙婷李海军袁瑞玲罗文键郑艺王云飞
Owner PERIC SPECIAL GASES CO LTD
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