CN212299665U

CN212299665U - Device for recovering argon tail gas in monocrystalline silicon production

Info

Publication number: CN212299665U
Application number: CN202021831785.4U
Authority: CN
Inventors: 王耀亮; 王传瑞; 吴丹红
Original assignee: Shanghai Yueshen Energy Technology Co ltd
Current assignee: Shanghai Yueshen Energy Technology Co ltd
Priority date: 2020-08-27
Filing date: 2020-08-27
Publication date: 2021-01-05
Anticipated expiration: 2030-08-27

Abstract

The utility model discloses a retrieve argon gas tail gas's in monocrystalline silicon production device. The method comprises the steps of removing dust in recycled mixed argon through a dust filter, then compressing the dust, cooling and dewatering the dust through a cooling dryer, conveying the mixed argon subjected to cooling and dewatering into a heat regenerator, calculating the content of oxidative impurities such as methane, carbon monoxide and the like and the content of oxygen in the mixed argon, supplementing oxygen after calculation, increasing the temperature of the mixed argon, removing the impurity gases in the mixed argon through a first catalytic reactor and a second catalytic reactor to obtain rough-filtered argon, allowing the rough-filtered argon to sequentially pass through a cooler and a normal-temperature adsorber to obtain fine-filtered argon, cooling the fine-filtered argon through a heat exchanger, conveying the fine-filtered argon to a rectifying tower to fractionate to obtain pure liquid argon and rectified waste gas, and completing the recovery of the argon. Under the condition that hydrogen is not introduced as intermediate reaction gas, the efficiency of argon recovery is improved, the flow of argon recovery is simplified, and the cost of argon recovery is reduced.

Description

Device for recovering argon tail gas in monocrystalline silicon production

Technical Field

The utility model belongs to the technical field of the argon gas is retrieved, is a retrieve device of argon gas tail gas in monocrystalline silicon production particularly.

Background

Single crystal silicon is currently produced by the czochralski method. The most common Czochralski method for producing single crystal silicon adopts a reduced pressure crystal pulling process; the decompression process is characterized in that high-purity argon is continuously and uniformly introduced into a hearth of a single crystal furnace in the silicon single crystal drawing process, and meanwhile, a vacuum pump continuously pumps the argon outwards from the hearth to keep the vacuum degree in the hearth stable. The argon gas carries silicon oxide and impurity volatiles generated due to high temperature during the single crystal pulling process, and is discharged to the atmosphere by pumping of a vacuum pump. Through the analysis of the discharged argon, the main impurity components are as follows: alkanes such as oxygen, nitrogen, carbon monoxide, carbon dioxide, methane, etc. The recycling of the argon has great practical significance, the production cost can be greatly reduced, and adverse effects such as gas supply and transportation can be avoided.

As for the argon recovery and purification method, in the prior art, argon recovered from a single crystal furnace is dedusted and then compressed by a compressor; then, hydrocarbons such as methane and the like and carbon monoxide react with oxygen to produce water and carbon dioxide through high-temperature catalysis, and the excessive oxygen is ensured in the catalytic reaction; and finally, reacting oxygen with the added hydrogen to generate water under the action of a catalyst after cooling, ensuring excessive reaction hydrogen, removing water and carbon dioxide by a molecular sieve normal-temperature adsorption mode and removing nitrogen and hydrogen by a low-temperature method, wherein the impurity components in the treated argon comprise water, carbon dioxide, hydrogen and nitrogen. The method has the defects that the equipment is complex to control and occupies a large area due to the use of hydrogen, a hydrogen production device or a hydrogen storage tank is required to be arranged in a system, so that the investment cost and the safety of equipment operation and maintenance are greatly increased, the method is limited by increasingly strict control on the production of hazardous chemicals in various places, and the recovery process flow using the hydrogen cannot meet the industrial requirements.

SUMMERY OF THE UTILITY MODEL

1. Technical problem to be solved by the utility model

The utility model aims to solve the problem that the current argon gas is recovered with high costs and the flow is complicated.

2. Technical scheme

In order to achieve the above purpose, the utility model provides a technical scheme does:

the utility model discloses a retrieve argon gas tail gas's in monocrystalline silicon production device, including dust filter, compressor, cold machine, regenerator, catalytic reactor two, cooler and the normal atmospheric temperature adsorber that communicates in proper order, the regenerator still communicates heater and catalytic reactor one, the export intercommunication of normal atmospheric temperature adsorber has the heat exchanger, the exit intercommunication of heat exchanger has the rectifying column.

Preferably, the normal temperature adsorber comprises at least two adsorption cylinders, and an outlet of each adsorption cylinder is communicated with the heat exchanger.

Preferably, the heat exchanger is provided with A, B, C three warming pipelines and a cooling pipeline, the normal temperature adsorber is communicated with the cooling pipeline inlet of the heat exchanger, the cooling pipeline outlet of the heat exchanger is communicated with a first rectifying tower, the lower layer outlet of the first rectifying tower is communicated with a first condenser, and the outlet of the first condenser is communicated with the inlet of the warming pipeline C.

Preferably, an upper outlet of the first rectifying tower is communicated with a second rectifying tower, an upper outlet of the second rectifying tower is communicated with an inlet of a warming pipeline B, an outlet of the warming pipeline B is communicated with a replacement gas inlet of a normal-temperature adsorber, an upper outlet of the second rectifying tower is communicated with a second condenser, an outlet of the second condenser is communicated with an inlet of the warming pipeline A, and an outlet of the warming pipeline A is communicated with an inlet of a compressor.

Preferably, the outlet of the warming pipeline C is connected with an argon gas recovery pipe, and the inlets of the first condenser and the second condenser are both communicated with liquid argon conveying pipes.

Preferably, a vent pipe is communicated with a pipeline between the outlet of the heating pipeline B and the replacement gas inlet of the normal-temperature adsorber, and an oxygen supplementing pipe (290) is communicated between the cold dryer (130) and the heat regenerator (140).

3. Advantageous effects

Adopt the technical scheme provided by the utility model, compare with prior art, have following beneficial effect:

the utility model discloses a retrieve argon gas tail gas's in monocrystalline silicon production device, including dust filter, compressor, cold machine, regenerator, catalytic reactor two, cooler and the normal atmospheric temperature adsorber that communicates in proper order, the regenerator still communicates heater and catalytic reactor one, the export intercommunication of normal atmospheric temperature adsorber has the heat exchanger, the exit intercommunication of heat exchanger has the rectifying column. The method comprises the steps of removing dust in recycled mixed argon through a dust filter, then compressing the dust, cooling and dewatering the dust through a cooling dryer, conveying the mixed argon subjected to cooling and dewatering into a heat regenerator, calculating the content of oxidative impurities such as methane, carbon monoxide and the like and the content of oxygen in the mixed argon, supplementing oxygen after calculation, increasing the temperature of the mixed argon, removing the impurity gases in the mixed argon through a first catalytic reactor and a second catalytic reactor to obtain rough-filtered argon, allowing the rough-filtered argon to sequentially pass through a cooler and a normal-temperature adsorber to obtain fine-filtered argon, cooling the fine-filtered argon through a heat exchanger, conveying the fine-filtered argon to a rectifying tower to fractionate to obtain pure liquid argon and rectified waste gas, and completing the recovery of the argon. Under the condition that hydrogen is not introduced as intermediate reaction gas, the efficiency of argon recovery is improved, the flow of argon recovery is simplified, and the cost of argon recovery is reduced.

Drawings

Fig. 1 is a schematic structural diagram of the device for recovering argon tail gas in the production of monocrystalline silicon.

The reference numerals in the schematic drawings illustrate:

110. a dust filter; 120. a compressor; 130. a cold dryer; 140. a heat regenerator; 150. a first catalytic reactor; 160. a heater; 170. a second catalytic reactor; 180. a cooler; 190. a normal temperature absorber; 210. a heat exchanger; 220. a first rectifying tower; 230. a first condenser; 240. a second rectifying tower; 250. a second condenser; 260. an argon gas recovery tube; 270. a liquid argon delivery pipe; 280. an emptying pipe; 290. an oxygen supply pipe; 310. a regeneration gas line.

Detailed Description

In order to facilitate understanding of the invention, the invention will be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which can be embodied in many different forms and are not limited to the embodiments described herein, but which are provided so as to render the disclosure of the invention more thorough and complete.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present; when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present; the terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention; as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

Example 1

Referring to the attached drawing 1, the device for recovering argon tail gas in monocrystalline silicon production according to the embodiment includes a dust filter 110, a compressor 120, a cold dryer 130, a heat regenerator 140, a second catalytic reactor 170, a cooler 180, and a normal temperature adsorber 190, which are sequentially communicated, the heat regenerator 140 is further communicated with a heater 160 and the first catalytic reactor 150, an outlet of the normal temperature adsorber 190 is communicated with a heat exchanger 210, and an outlet of the heat exchanger 210 is communicated with a rectifying tower. The dust in the recycled mixed argon is removed through a dust filter 110, then the mixed argon is compressed and cooled through a cooling dryer 130 for water removal, the mixed argon after water removal is conveyed into a heat regenerator 140, the content of oxidative impurities such as methane, carbon monoxide and the like and the content of oxygen in the mixed argon are calculated, oxygen is supplemented after calculation is completed, the temperature of the mixed argon is increased, impurity gases in the mixed argon are removed through a first catalytic reactor 150 and a second catalytic reactor 170, rough filtered argon is obtained, the rough filtered argon is sequentially subjected to a cooler 180 and a normal temperature adsorber 190 to obtain fine filtered argon, the fine filtered argon is cooled through a heat exchanger 210 and then conveyed to a rectifying tower for fractionation to obtain pure liquid argon and rectified waste gas, and the recovery of the argon is completed. Under the condition that hydrogen is not introduced as intermediate reaction gas, the efficiency of argon recovery is improved, the flow of argon recovery is simplified, and the cost of argon recovery is reduced.

The normal temperature adsorber 190 includes at least two adsorption cylinders, and the outlet of each adsorption cylinder is communicated with the heat exchanger 210, and a plurality of adsorption cylinders can promote the whole adsorption efficiency of the normal temperature adsorber 190, further promote the efficiency of argon gas recovery.

The heat exchanger 210 is provided with A, B, C three warming pipelines and a cooling pipeline, the normal temperature absorber 190 is communicated with the inlet of the cooling pipeline of the heat exchanger 210, the outlet of the cooling pipeline of the heat exchanger 210 is communicated with a first rectifying tower 220, the outlet of the lower layer of the first rectifying tower 220 is communicated with a first condenser 230, and the outlet of the first condenser 230 is communicated with the inlet of the warming pipeline C. The heat exchanger 210 saves overall heat consumption and saves heat exchange cost by exchanging heat between gases inside the system.

An upper outlet of the first rectifying tower 220 is communicated with a second rectifying tower 240, an upper outlet of the second rectifying tower 240 is communicated with an inlet of a warming pipeline B, an outlet of the warming pipeline B is communicated with a replacement gas inlet of the normal-temperature adsorber 190, an upper outlet of the second rectifying tower 240 is communicated with a second condenser 250, an outlet of the second condenser 250 is communicated with an inlet of a warming pipeline A, and an outlet of the warming pipeline A is communicated with an inlet of the compressor 120.

An outlet of the warming pipeline C is connected with an argon gas recycling pipe 260, and inlets of the first condenser 230 and the second condenser 250 are both communicated with a liquid argon conveying pipe 270.

The heat exchanger 210 can not only cool down the refined filtered argon gas after being processed by the normal temperature adsorber 190, but also warm up the rectified waste gas output by the second rectifying tower 240, so that the heat can be recycled, and the rectified waste gas is reheated by the heat exchanger 210 to be used as the replacement gas of the normal temperature adsorber 190, thereby further improving the efficiency of the system and reducing the cost.

An emptying pipe 280 is communicated with a pipeline between the outlet of the temperature rising pipeline B and the replacement gas inlet of the normal-temperature adsorber 190, a regeneration gas pipeline (310) is also communicated with the normal-temperature adsorber 190 and the emptying pipe 280, and an oxygen supplementing pipe 290 is communicated between the cold dryer 130 and the heat regenerator 140.

The operation method of the embodiment includes removing dust in the recycled mixed argon through a dust filter 110, compressing the removed dust, cooling and dewatering the dust through a cold dryer 130, conveying the cooled and dewatered mixed argon into a heat regenerator 140, calculating the content of oxidative impurities such as methane, carbon monoxide and the like and the content of oxygen in the mixed argon, supplementing oxygen after calculation, increasing the temperature of the mixed argon, removing the impurity gases in the mixed argon through a first catalytic reactor 150 and a second catalytic reactor 170 to obtain rough-filtered argon, sequentially passing the rough-filtered argon through a cooler 180 and a normal-temperature adsorber 190 to obtain fine-filtered argon, cooling the fine-filtered argon through a heat exchanger 210, conveying the fine-filtered argon to a rectifying tower for fractionation to obtain pure liquid argon and rectified waste gas, and completing the recovery of the argon.

The rectification waste gas is reheated by the heat exchanger 210 and then used as replacement gas of the normal temperature adsorber 190, so that the utilization rate of the rectification waste gas is improved, and meanwhile, the cost is saved.

Pure liquid argon is changed into a normal-temperature pure argon product after heat exchange between the first condenser 230 and the heat exchanger 210, and the subsequent monocrystalline silicon production process can be directly carried out.

The above-mentioned embodiments only express a certain implementation manner of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention; it should be noted that, for those skilled in the art, without departing from the concept of the present invention, several variations and modifications can be made, which all fall within the protection scope of the present invention; therefore, the protection scope of the present invention should be subject to the appended claims.

Claims

1. The utility model provides a retrieve device of argon gas tail gas in monocrystalline silicon production which characterized in that: the device comprises a dust filter (110), a compressor (120), a cold dryer (130), a heat regenerator (140), a catalytic reactor II (170), a cooler (180) and a normal-temperature adsorber (190) which are sequentially communicated, wherein the heat regenerator (140) is also communicated with a heater (160) and a catalytic reactor I (150), the outlet of the normal-temperature adsorber (190) is communicated with a heat exchanger (210), and the outlet of the heat exchanger (210) is communicated with a rectifying tower.

2. The device for recovering the argon tail gas in the monocrystalline silicon production as claimed in claim 1, characterized in that: the normal-temperature adsorber (190) comprises at least two adsorption cylinders, and the outlet of each adsorption cylinder is communicated with the heat exchanger (210).

3. The device for recovering the argon tail gas in the monocrystalline silicon production as claimed in claim 1, characterized in that: heat exchanger (210) are equipped with A, B, C three intensification pipelines and a cooling pipeline, normal atmospheric temperature adsorber (190) are linked together with the cooling pipeline import of heat exchanger (210), the cooling pipeline export intercommunication of heat exchanger (210) has rectifying column one (220), the lower floor export intercommunication of rectifying column one (220) has condenser one (230), the export of condenser one (230) and intensification pipeline C's import intercommunication.

4. The device for recovering argon tail gas in monocrystalline silicon production according to claim 3, characterized in that: the upper exit intercommunication of rectifying column one (220) has rectifying column two (240), the upper exit of rectifying column two (240) and the import intercommunication of intensification pipeline B, the export of intensification pipeline B and the replacement gas entry intercommunication of normal atmospheric temperature adsorber (190), the upper exit intercommunication of rectifying column two (240) has condenser two (250), the export and the import intercommunication of intensification pipeline A of condenser two (250), the import intercommunication of intensification pipeline A export and compressor (120).

5. The device for recovering argon tail gas in monocrystalline silicon production according to claim 3, characterized in that: the outlet of the warming pipeline C is connected with an argon gas recovery pipe (260), and the inlets of the first condenser (230) and the second condenser (250) are both communicated with a liquid argon delivery pipe (270).

6. The device for recovering the argon tail gas in the monocrystalline silicon production as claimed in claim 4, characterized in that: and a vent pipe (280) is communicated with a pipeline between the outlet of the temperature rising pipeline B and the replacement gas inlet of the normal-temperature adsorber (190), and an oxygen supplementing pipe (290) is communicated between the cold dryer (130) and the heat regenerator (140).