CN115744845A - Argon gas recovery purification efficiency increasing system - Google Patents

Argon gas recovery purification efficiency increasing system Download PDF

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Publication number
CN115744845A
CN115744845A CN202211291510.XA CN202211291510A CN115744845A CN 115744845 A CN115744845 A CN 115744845A CN 202211291510 A CN202211291510 A CN 202211291510A CN 115744845 A CN115744845 A CN 115744845A
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China
Prior art keywords
pipeline
argon
rich
communicated
adsorption tower
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CN202211291510.XA
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Chinese (zh)
Inventor
朱东赟
郝文炳
王世豪
贺明星
唐勤友
刘华琴
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Shanghai Lianfeng Energy Technology Co ltd
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Shanghai Lianfeng Energy Technology Co ltd
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Priority to CN202211291510.XA priority Critical patent/CN115744845A/en
Publication of CN115744845A publication Critical patent/CN115744845A/en
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Abstract

The invention provides an argon recovery, purification and efficiency enhancement system which comprises a compressor, a cold dryer, a first air pipeline, an adsorption device, a second air pipeline and a buffer tank, wherein the compressor, the cold dryer, the first air pipeline, the adsorption device, the second air pipeline and the buffer tank are sequentially connected; the adsorption device comprises a first adsorption tower, a second adsorption tower, a first air inlet pipeline, a second air inlet pipeline, a first air outlet pipeline, a second air outlet pipeline and a pressure equalizing pipeline, wherein the first argon-rich pipeline is communicated with an inlet of the first adsorption tower through the first air inlet pipeline, and an outlet of the first adsorption tower is communicated with the second argon-rich pipeline through the first air outlet pipeline; the first argon-rich pipeline is communicated with an inlet of a second adsorption tower through a second air inlet pipeline, and an outlet of the second adsorption tower is communicated with a second argon-rich pipeline through a second air outlet pipeline. The argon recovery and purification synergistic system provided by the invention removes the impurity N by using a normal-temperature physical adsorption method 2 And purifying to obtain argon gas with higher concentration, buffering, and delivering to an argon recovery system to improve the extraction rate.

Description

Argon gas recovery purification efficiency increasing system
Technical Field
The invention relates to the technical field of argon recovery, in particular to an argon recovery, purification and synergism system.
Background
The Czochralski method is a main method for producing single crystal silicon, and 70-80% of the silicon single crystals are produced globally by the Czochralski method. The most common Czochralski process for producing single crystal silicon uses a reduced pressure crystal pulling process that is both a vacuum process and a flowing atmosphere process; the decompression process is characterized in that high-purity argon is continuously introduced into a hearth of a single crystal furnace at a constant speed 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 to be stabilized at about 20 torr. The vacuum pump for the reduced pressure crystal pulling process generally adopts a slide valve pump, and the slide valve pump is a mechanical vacuum pump which uses oil to maintain sealing. 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 alkanes such as oxygen, nitrogen, carbon monoxide, carbon dioxide, methane and the like; the recycling of the argon has great practical significance. Known techniques for argon recovery purification: carrying out coarse oil removal on argon recovered from a single crystal furnace, and then carrying out high-precision oil removal and dust removal after compression and cooling; 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 slight excess of oxygen (oxygen is added when impurity oxygen is insufficient) is ensured in the catalytic reaction; after cooling, enabling excessive oxygen to react with added hydrogen under the action of a catalyst to generate water, and ensuring excessive reaction hydrogen, wherein impurity components in the argon after treatment are water, carbon dioxide, hydrogen and nitrogen; and finally, adsorbing water and carbon dioxide by an argon normal-temperature adsorption unit to obtain crude argon only containing nitrogen and hydrogen as impurities. The argon normal-temperature adsorption unit consists of two adsorbers, adsorbents for adsorbing water and carbon dioxide are filled in the adsorbers, one adsorber performs adsorption work, and the other adsorber performs regeneration work including pressure relief, heating and cold blowing. The argon normal-temperature adsorption unit and the pressure swing adsorption unit automatically control the operation switching through the time program controller.
The extraction rate of the existing argon recovery system process flow reaches 90 percent, and the extraction rate cannot be further improved under the condition that the existing argon recovery system is not changed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an argon recovery and purification synergistic system.
The invention adopts the following technical scheme for solving the technical defects:
the argon recovery and purification device comprises a compressor, a cold dryer, a first argon-rich pipeline, an adsorption device, a second argon-rich pipeline and a buffer tank which are sequentially connected; the adsorption device comprises a first adsorption tower, a second adsorption tower, a first air inlet pipeline, a second air inlet pipeline, a first air outlet pipeline, a second air outlet pipeline and a pressure equalizing pipeline, wherein the first argon-rich pipeline is communicated with an inlet of the first adsorption tower through the first air inlet pipeline, and an outlet of the first adsorption tower is communicated with the second argon-rich pipeline through the first air outlet pipeline; the first argon-rich pipeline is communicated with an inlet of the second adsorption tower through a second air inlet pipeline, an outlet of the second adsorption tower is communicated with the second argon-rich pipeline through a second air outlet pipeline, and the second argon-rich pipeline is communicated with an air inlet of the buffer tank.
Further, raw material argon is introduced into an air inlet of the compressor, an air outlet of the compressor is connected with an air inlet of the cold dryer through an electromagnetic valve V4101, and the air outlet of the cold dryer is communicated with the first argon-rich pipeline; the raw argon comes from argon-rich waste gas which cannot be recovered by an argon recovery system.
Furthermore, the first argon-rich pipeline is also communicated with an emptying pipeline, an electromagnetic valve V4103 is arranged on the first argon-rich pipeline, and an emptying valve V4104 is arranged on the emptying pipeline.
Further, the first intake line and the second intake line are communicated with an evacuation line through a solenoid valve V4115 and a solenoid valve V4116, respectively.
Further, a flow meter FIC4101 and a regeneration air valve V4105 are arranged on the pressure equalizing pipeline.
Furthermore, the second argon-rich pipeline is also communicated with a third argon-rich pipeline, an analyzer is arranged on the second argon-rich pipeline, and an emptying valve V4106 is arranged on the third argon-rich pipeline.
Further, the system also comprises a PLC, wherein the PLC is used for controlling and connecting the electromagnetic valve and the flow meter FIC4101.
By adopting the technical scheme, compared with the prior art, the invention has the following technical advantages:
the argon recovery, purification and synergism system provided by the invention removes the impurity N by using a normal-temperature physical adsorption method 2 And purifying to obtain argon gas with higher concentration, buffering, and delivering to an argon recovery system to improve the extraction rate.
The invention adopts a normal-temperature physical adsorption method, does not need to add a catalyst to carry out chemical reaction, and does not need the condition of high temperature or low temperature deep cooling, thereby greatly saving energy consumption, simplifying the flow and further reducing the operation cost of equipment.
Drawings
FIG. 1 is a system schematic of an argon recovery purification enhancement system of the present invention;
wherein the reference numbers are:
a compressor 1; a cooling and drying machine 2; a first adsorption column 3; a second adsorption column 4; a first intake line 5; a second intake line 6; a first outlet line 7; a second outlet line 8; a pressure equalizing pipeline 9; a first argon-rich gas line 10; a second argon-rich gas line 11; a third argon-rich gas line 12; an emptying pipeline 13; an evacuation line 14; a buffer tank 15.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the embodiment provides an argon recovery, purification and efficiency enhancement system, which includes a compressor 1, a freeze dryer 2, a first argon-rich gas pipeline 10, an adsorption device, a second argon-rich gas pipeline 11 and a buffer tank 15, which are connected in sequence; the adsorption device comprises a first adsorption tower 3, a second adsorption tower 4, a first air inlet pipeline 5, a second air inlet pipeline 6, a first air outlet pipeline 7, a second air outlet pipeline 8 and a pressure equalizing pipeline 9, wherein a first argon-rich pipeline 10 is communicated with an inlet of the first adsorption tower 3 through the first air inlet pipeline 5, and an outlet of the first adsorption tower 3 is communicated with a second argon-rich pipeline 11 through the first air outlet pipeline 7; the first argon-rich gas pipeline 10 is communicated with an inlet of the second adsorption tower 4 through a second gas inlet pipeline 6, an outlet of the second adsorption tower 4 is communicated with the second argon-rich gas pipeline 11 through a second gas outlet pipeline 8, the second argon-rich gas pipeline 11 is communicated with a gas inlet of the buffer tank 15, and a gas outlet of the buffer tank 15 is connected with an argon recovery system.
In this embodiment, raw material argon is introduced into an air inlet of the compressor 1, an air outlet of the compressor 1 is connected to an air inlet of the freeze-drying machine 2 through an electromagnetic valve V4101, and an air outlet of the freeze-drying machine 2 is communicated with the first argon-rich pipeline 10. The raw material argon comes from argon-rich waste gas which cannot be recovered by an argon recovery system, the argon recovery system is the prior art, and details are not described in the invention.
In this embodiment, the first argon-rich pipeline 10 is further communicated with an evacuation pipeline 13, the first argon-rich pipeline 10 is provided with an electromagnetic valve V4103, and the evacuation pipeline 13 is provided with an evacuation valve V4104.
In this embodiment, the first intake conduit 5 and the second intake conduit 6 are respectively communicated with an evacuation conduit 14 through a solenoid valve V4115 and a solenoid valve V4116.
In this embodiment, the pressure equalizing pipe 9 is provided with a flow meter FIC4101 and a regeneration air valve V4105, and the regeneration air valve V4105 controls the flow rate to be 30Nm 3 /h。
In this example, the second argon-rich gas pipeline 11 is further communicated with a third argon-rich gas pipeline 12, an analyzer is arranged on the second argon-rich gas pipeline 11, an emptying valve V4106 is arranged on the third argon-rich gas pipeline 12, specifically, two analyzers are arranged on the second argon-rich gas pipeline 11, and the analyzers are respectively a crude argon N analyzer AI4111 and a crude argon H 2 AnalyzerAI4111。
In this embodiment, the system further comprises a PLC which controls and connects each electromagnetic valve and the flow meter FIC4101.
The working parameters of the equipment in the invention are shown in the table 1:
TABLE 1
Serial number Parameter(s) Unit of Working range
1 Compressor outlet pressure kPa 350~420
2 Compressor outlet temperature 35~50
3 Outlet temperature of cooling and drying machine 15~20
4 Inlet pressure of adsorption tower kPa 350~400
5 Pressure at the outlet of the adsorption column kPa 200~50
6 Crude argon N analyzer AI4111 0~5%
7 Crude argon H2 analyzer AI4111 0~10%
The working process of the argon recovery and purification device of the embodiment is as follows:
and (4) checking that each cooling water valve is normally opened, opening a condensate water drain valve to drain water, and then closing the condensate water drain valve to check that the pressure of an instrument air source is normal.
Confirming that the electromagnetic valve V4103 is closed, opening the atmospheric valve V4104, selecting the adsorption tower C403A or C403B which is well regenerated to be put into operation, and suspending the regeneration process.
The electromagnetic valve V4103 is opened step by step, and the emptying valve V4104 is closed step by step and the stabilization of the discharge pressure of the compressor 1 is controlled.
The cooling and drying machine 2 is started, the outlet temperature is controlled, and the automatic operation is controlled.
Open vent valve V4106, observe N in crude argon outlet analyzer AI4111 2 When the content value trend is close to 1%, the vent valve V4106 is closed, the suspension of the adsorber switching program is cancelled, and the automatic operation is carried out.
Switching and regenerating processes of the molecular sieve adsorption tower:
the initial state electromagnetic valves V4115, V4116 and V4105 are in closed states;
after the two adsorption towers operate for a period of time in parallel, the first adsorption tower 3 is switched to regeneration. At this time, the positive flow inlet and outlet solenoid valves V4111 and V4113 of the first adsorption tower 3 are closed, and the pressure relief solenoid valve V4115 is opened. After the pressure release is completed, the electromagnetic valve V4105 is opened to equalize the pressure in the first adsorption tower 3, and the adsorption process is performed.
The normal state of the adsorption device is one adsorption and the other regeneration, the switching is carried out within 1 hour, and the PLC program automatically controls the adsorption device to carry out the switching, if the first adsorption tower 3 works and the second adsorption tower 4 regenerates, all valves V4112 and V4114 at the inlet and the outlet of the adsorption tower B are closed at the set switching moment, and the pressure relief electromagnetic valve V4116 is opened. After the pressure relief is finished, the regeneration valve V4105 is opened to raise the pressure of the second adsorption tower 4, when the pressure of the second adsorption tower 4 is consistent with the pressure of the crude argon main pipe, the regeneration valve V4105 is closed, then the inlet and outlet electromagnetic valves V4112 and V4114 of the second adsorption tower 4 are opened, and the second adsorption tower 4 is switched to the adsorption process.
Purifying to obtain argon with higher concentration, buffering by a buffer tank 15, and sending to an argon recovery system to improve the extraction rate of the argon recovery system.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.

Claims (7)

1. An argon recovery, purification and synergism system is characterized by comprising a compressor (1), a cold dryer (2), a first argon-rich pipeline (10), an adsorption device, a second argon-rich pipeline (11) and a buffer tank (15) which are connected in sequence; the adsorption device comprises a first adsorption tower (3), a second adsorption tower (4), a first air inlet pipeline (5), a second air inlet pipeline (6), a first air outlet pipeline (7), a second air outlet pipeline (8) and a pressure equalizing pipeline (9), wherein the first argon-rich pipeline (10) is communicated with an inlet of the first adsorption tower (3) through the first air inlet pipeline (5), and an outlet of the first adsorption tower (3) is communicated with the second argon-rich pipeline (11) through the first air outlet pipeline (7); the first argon-rich pipeline (10) is communicated with an inlet of the second adsorption tower (4) through a second air inlet pipeline (6), an outlet of the second adsorption tower (4) is communicated with the second argon-rich pipeline (11) through a second air outlet pipeline (8), and the second argon-rich pipeline (11) is communicated with an air inlet of the buffer tank (15).
2. The argon recovery, purification and synergy system according to claim 1, wherein a gas inlet of the compressor (1) is filled with raw argon, a gas outlet of the compressor is connected with a gas inlet of the freeze-drying machine (2) through an electromagnetic valve V4101, and a gas outlet of the freeze-drying machine (2) is communicated with the first argon-rich pipeline (10); the raw argon gas comes from argon-rich waste gas which cannot be recovered by an argon recovery system.
3. The argon recovery, purification and synergy system according to claim 1, wherein the first argon-rich pipeline (10) is further communicated with a vent pipeline (13), an electromagnetic valve V4103 is arranged on the first argon-rich pipeline (10), and a vent valve V4104 is arranged on the vent pipeline (13).
4. The argon recovery purification enhancement system according to claim 1, wherein the first gas inlet line (5) and the second gas inlet line (6) are communicated with an evacuation line (14) through a solenoid valve V4115 and a solenoid valve V4116, respectively.
5. The argon recovery, purification and efficiency enhancement system according to claim 1, wherein the pressure equalizing pipeline (9) is provided with a flow meter FIC4101 and a regeneration gas valve V4105.
6. The argon recovery, purification and efficiency enhancement system according to claim 1, wherein the second argon-rich pipeline (11) is further communicated with a third argon-rich pipeline (12), an analyzer is arranged on the second argon-rich pipeline (11), and a vent valve V4106 is arranged on the third argon-rich pipeline (12).
7. The argon recovery purification enhancement system of any one of claims 1-6, further comprising a PLC to control connection of the valves and the flow meter FIC4101.
CN202211291510.XA 2022-10-20 2022-10-20 Argon gas recovery purification efficiency increasing system Pending CN115744845A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117504525A (en) * 2023-09-18 2024-02-06 上海联风气体有限公司 Dirty argon separation system and method capable of reducing cryogenic dirty argon discharge

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4816237A (en) * 1984-08-03 1989-03-28 Hitachi, Ltd. Process for purifying argon gas and apparatus used therefor
US20160325996A1 (en) * 2014-01-29 2016-11-10 Shin-Etsu Handotai Co., Ltd. Method for recovering and purifying argon gas from silicon single crystal manufacturing apparatus and apparatus for recovering and purifying argon gas
CN108557787A (en) * 2018-06-29 2018-09-21 上海联风能源科技有限公司 A kind of recycling crude argon method of purification again
CN208471537U (en) * 2018-06-29 2019-02-05 上海联风能源科技有限公司 A kind of recycling crude argon purifying plant again
CN110803689A (en) * 2019-12-10 2020-02-18 上海联风能源科技有限公司 Argon recovery method and device for removing carbon monoxide and integrating high-purity nitrogen by rectification method
CN111634896A (en) * 2020-05-19 2020-09-08 北京北大先锋科技有限公司 Argon purification and recovery method and system

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4816237A (en) * 1984-08-03 1989-03-28 Hitachi, Ltd. Process for purifying argon gas and apparatus used therefor
US20160325996A1 (en) * 2014-01-29 2016-11-10 Shin-Etsu Handotai Co., Ltd. Method for recovering and purifying argon gas from silicon single crystal manufacturing apparatus and apparatus for recovering and purifying argon gas
CN108557787A (en) * 2018-06-29 2018-09-21 上海联风能源科技有限公司 A kind of recycling crude argon method of purification again
CN208471537U (en) * 2018-06-29 2019-02-05 上海联风能源科技有限公司 A kind of recycling crude argon purifying plant again
CN110803689A (en) * 2019-12-10 2020-02-18 上海联风能源科技有限公司 Argon recovery method and device for removing carbon monoxide and integrating high-purity nitrogen by rectification method
CN111634896A (en) * 2020-05-19 2020-09-08 北京北大先锋科技有限公司 Argon purification and recovery method and system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117504525A (en) * 2023-09-18 2024-02-06 上海联风气体有限公司 Dirty argon separation system and method capable of reducing cryogenic dirty argon discharge
CN117504525B (en) * 2023-09-18 2024-04-12 上海联风气体有限公司 Dirty argon separation system and method capable of reducing cryogenic dirty argon discharge

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