CN113842753A - Treatment process of tail gas discharged from cathode of nitrogen trifluoride electrolytic cell - Google Patents
Treatment process of tail gas discharged from cathode of nitrogen trifluoride electrolytic cell Download PDFInfo
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- CN113842753A CN113842753A CN202111311673.5A CN202111311673A CN113842753A CN 113842753 A CN113842753 A CN 113842753A CN 202111311673 A CN202111311673 A CN 202111311673A CN 113842753 A CN113842753 A CN 113842753A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2047—Hydrofluoric acid
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Abstract
The invention provides a treatment process of tail gas discharged by a cathode of a nitrogen trifluoride electrolytic cell, which comprises the following operation steps: s1, preparing a mixed solution of ammonium bifluoride and hydrogen fluoride, and discharging the mixed solution into a three-stage absorption treatment system; s2, sending tail gas discharged by the cathode of the electrolytic cell into a three-stage absorption treatment system for absorption in sequence; and S3, guiding the solution in the primary absorption system to an electrolytic cell, guiding the solution in the secondary absorption system to a primary absorption storage tank, guiding the solution in the tertiary absorption system to a secondary absorption storage tank, supplementing a new mixed solution in the tertiary absorption system, and pouring the cathode waste gas again for absorption treatment. The process scheme of the invention has scientific and reasonable design, can ensure the high-efficiency standard-reaching treatment of the cathode tail gas, meets the requirement of environmental protection, and recycles the hydrogen fluoride for the second time, thereby improving the material utilization rate and reducing the production cost.
Description
Technical Field
The invention belongs to the technical field of nitrogen trifluoride production, and particularly relates to a treatment process of tail gas discharged by a cathode of a nitrogen trifluoride electrolytic cell.
Background
The chemical formula of nitrogen trifluoride is NF3It is a colorless, odorless and stable gas at normal temperature, and is a strong oxidant. Nitrogen trifluoride is an excellent plasma etching gas in the microelectronic industry, has higher etching rate and selectivity for etching silicon and silicon nitride compared with carbon tetrafluoride and mixed gas of carbon tetrafluoride and oxygen, has no pollution to the surface, has excellent etching rate and selectivity particularly in the etching of integrated circuit materials with the thickness of less than 1.5um, does not leave any residue on the surface of an etched object, and is a very good cleaning agent. With the development of nanotechnology and the large-scale development of technology in the electronics industry, the demand for it will increase.
At present, the waste gas generated by nitrogen trifluoride electrolysis is mainly treated by chemical neutralization reaction. The problem of whether the HF in the cathode tail gas is discharged after reaching the standard or not after being purified is also solved simultaneously in the HF treatment in the cathode tail gas generated by the electrolysis of nitrogen trifluoride.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a process for treating tail gas discharged from a cathode of a nitrogen trifluoride electrolytic cell, aiming at the defects of the prior art, the process has the advantages of scientific and reasonable design, simple and convenient operation, low application cost and good recovery effect, can meet the environmental-friendly discharge standard, can efficiently recycle hydrogen fluoride, can reduce the production cost, and has good economic benefit.
In order to solve the technical problems, the invention adopts the technical scheme that: a process for treating tail gas discharged from a cathode of a nitrogen trifluoride electrolysis cell, which is characterized by comprising the following operation steps:
s1, preparing a mixed solution composed of ammonium bifluoride and hydrogen fluoride, and introducing the prepared mixed solution into an absorption treatment system, wherein the absorption treatment system is composed of a primary absorption system, a secondary absorption system and a tertiary absorption system which are sequentially communicated, the primary absorption system is connected with a cathode tail gas discharge pipe of an electrolytic cell for producing nitrogen trifluoride, the tertiary absorption system is connected with an exhaust pipe for discharging cathode tail gas after absorption treatment, the secondary absorption system is arranged between the primary absorption system and the secondary absorption system, and the mixed solution is respectively introduced into the primary absorption system, the secondary absorption system and the tertiary absorption system;
s2, leading tail gas discharged by the cathode of the electrolytic cell during nitrogen trifluoride production into a primary absorption system through a cathode tail gas discharge pipe, and carrying out tertiary absorption treatment on the tail gas through a mixed solution sequentially through the primary absorption system, the secondary absorption system and a tertiary absorption system;
s3, discharging the tail gas subjected to the tertiary absorption treatment through an exhaust pipe, introducing the mixed solution in the primary absorption system into an electrolytic cell, introducing the mixed solution in the secondary absorption system into the primary absorption system, introducing the mixed solution in the tertiary absorption system into the secondary absorption system, and adding a new mixed solution into the tertiary absorption system;
and S4, repeating the steps S1-S3 to carry out tail gas absorption treatment again.
Preferably, the ratio of ammonium bifluoride in the mixed solution prepared in S1 is: the mass ratio of the hydrogen fluoride is (3-4): 1, after the absorption treatment in S2, the ratio of ammonium bifluoride in the mixed solution in the primary absorption system: the mass ratio of hydrogen fluoride is 1: 1.
Preferably, the primary absorption system comprises a primary absorption container, a primary circulating pump and a primary solution storage tank which are sequentially communicated through a pipeline, the secondary absorption system comprises a secondary absorption container, a secondary circulating pump and a secondary solution storage tank which are sequentially communicated through a pipeline, the tertiary absorption system comprises a tertiary absorption container, a tertiary circulating pump and a tertiary solution storage tank which are sequentially communicated through a pipeline, the primary absorption container is connected with the cathode tail gas discharge pipe, the tertiary absorption container is connected with the exhaust pipe, the primary absorption container, the secondary absorption container and the tertiary absorption container are communicated through a pipeline, the primary solution storage tank, the secondary solution storage tank and the tertiary solution storage tank are filled with the mixed solution, the mixed solution in the three solution storage tanks is pumped out through the three circulating pumps to form a liquid circulating loop in the three absorption systems to absorb the cathode discharge tail gas in the absorption container, carry out the high-efficient recovery with the hydrogen fluoride in the tail gas, design three absorption system and can carry out the cubic to retrieve the hydrogen fluoride in the tail gas, improve the recovery effect.
Preferably, the working pressure of the first-stage circulating pump, the second-stage circulating pump and the third-stage circulating pump is 0.1-0.3MPa, the working temperature is normal temperature, and the working flow is 5-253And h, the primary absorption system, the secondary absorption system and the tertiary absorption system all work at normal temperature.
Compared with the prior art, the invention has the following advantages:
1. the method has the advantages of scientific and reasonable design, simple operation and good treatment effect on the cathode tail gas, and can recycle the hydrogen fluoride in the tail gas, improve the resource utilization rate and reduce the production cost.
2. According to the invention, the hydrogen fluoride in the tail gas is absorbed by the mixed solution composed of the ammonium bifluoride and the hydrogen fluoride, the characteristic that the ammonium bifluoride and the hydrogen fluoride are dissolved in different mass ratios (the mass ratio of the ammonium bifluoride to the hydrogen fluoride is liquid when being less than 3: 1, and the mass ratio of the ammonium bifluoride to the hydrogen fluoride can be changed into 1:1 by absorbing the hydrogen fluoride) is utilized, the recovery effect of the hydrogen fluoride in the tail gas is improved by three-stage absorption treatment, the tail gas discharged by the cathode reaches the environment-friendly discharge standard, the mixed solution after single recovery is returned to the electrolytic cell, the hydrogen fluoride recovered in the waste gas is put into the electrolytic cell again for electrolytic reaction, the resource utilization efficiency is improved, and the production cost is reduced.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic view showing a connection structure of a primary absorption system, a secondary absorption system and a tertiary absorption system in the present invention.
Description of reference numerals:
1-first stage absorption vessel; 2-first-stage solution storage tank; 3-first stage circulating pump;
4-cathode tail gas discharge pipe; 5-a secondary absorption vessel; 6-a secondary solution storage tank;
7-two-stage circulating pump; 8-three-stage absorption container; 9-a third-level solution storage tank;
10-three-stage circulating pump; 11-exhaust pipe.
Detailed Description
As shown in figure 1, the invention is realized by an absorption treatment system which comprises a primary absorption system, a secondary absorption system and a tertiary absorption system which are communicated in sequence, wherein the primary absorption system is connected with a cathode tail gas discharge pipe 4 of an electrolytic cell for producing nitrogen trifluoride, the tertiary absorption system is connected with an exhaust pipe 11 for discharging cathode tail gas after absorption treatment, the secondary absorption system is arranged between the primary absorption system and the secondary absorption system, the mixed solution is respectively introduced into the primary absorption system, the secondary absorption system and the tertiary absorption system, ammonium bifluoride and hydrogen fluoride are mainly contained in the mixed solution, and the water content of the mixed solution is not more than 500 ppm.
In this embodiment, one-level absorption system includes one-level absorption container 1, one-level circulating pump 3 and one-level solution storage tank 2 that communicate in proper order through the pipeline, two-level absorption system includes second grade absorption container 5, second grade circulating pump 7 and second grade solution storage tank 6 that communicate in proper order through the pipeline, three-level absorption system includes tertiary absorption container 8, tertiary circulating pump 10 and tertiary solution storage tank 9 that communicate in proper order through the pipeline, one-level absorption container 1 connects negative pole tail gas delivery pipe 4, tertiary absorption container 8 connects blast pipe 11, communicate through the pipeline between one-level absorption container 1, second grade absorption container 5 and the tertiary absorption container 8, one-level solution storage tank 2, second grade solution storage tank 6 and tertiary solution storage tank 9 pass through liquid guiding pipe connection.
The invention provides a treatment process of tail gas discharged by a cathode of a nitrogen trifluoride electrolytic cell, which comprises the following operation steps:
s1, preparing a mixed solution composed of ammonium bifluoride and hydrogen fluoride, and respectively introducing the prepared mixed solution into the primary solution storage tank 2, the secondary solution storage tank 6 and the tertiary solution storage tank 9;
s2, leading tail gas discharged by the cathode of the electrolytic cell during nitrogen trifluoride production into the primary absorption container 1 through the cathode tail gas discharge pipe 4, and carrying out tertiary absorption treatment on the tail gas through a mixed solution sequentially through the primary absorption container 1, the secondary absorption container 5 and the tertiary absorption container 8;
s3, discharging the tail gas subjected to the three-time absorption treatment through an exhaust pipe 11, introducing the mixed solution in the primary solution storage tank 2 into an electrolytic cell, introducing the mixed solution in the secondary solution storage tank 6 into the primary solution storage tank 2, introducing the mixed solution in the tertiary solution storage tank 9 into the secondary solution storage tank 6, and adding a new mixed solution into the tertiary solution storage tank 9;
and S4, repeating the steps S1-S3 to carry out tail gas absorption treatment again.
In this embodiment, the ammonium acid fluoride in the mixed solution prepared in S1: the mass ratio of the hydrogen fluoride is (3-4): 1, after the absorption treatment in S2, the ratio of ammonium bifluoride in the mixed solution in the primary absorption system: the mass ratio of the hydrogen fluoride is 1:1, and a new mixed solution of ammonium bifluoride added in the third-stage solution storage tank 9 in S3: the mass ratio of the hydrogen fluoride is (3-4): 1.
in this embodiment, set up the delivery pump that is used for deriving the mixed solution on the catheter, form the liquid circulation return circuit in three solution storage tanks pump in three absorption system through three circulating pump and absorb the processing to the negative pole emission tail gas in the absorption vessel, carry out high-efficient the retrieving with the hydrogen fluoride in the tail gas, design three absorption system and can carry out the cubic to the hydrogen fluoride in the tail gas and retrieve, improve the recovery effect.
In this embodiment, each pipeline is provided with a valve for circulating the tail gas and the mixed solution.
In this embodiment, the working pressure of the first-stage circulation pump 3, the second-stage circulation pump 7 and the third-stage circulation pump 10 is 0.1-0.3MPa, the working temperature is normal temperature, and the working flow rate is 5-253And h, the primary absorption system, the secondary absorption system and the tertiary absorption system all work at normal temperature.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (4)
1. A process for treating tail gas discharged from a cathode of a nitrogen trifluoride electrolysis cell, which is characterized by comprising the following operation steps:
s1, preparing a mixed solution composed of ammonium bifluoride and hydrogen fluoride, and introducing the prepared mixed solution into an absorption treatment system, wherein the absorption treatment system is composed of a primary absorption system, a secondary absorption system and a tertiary absorption system which are sequentially communicated, the primary absorption system is connected with a cathode tail gas discharge pipe of an electrolytic cell for producing nitrogen trifluoride, the tertiary absorption system is connected with an exhaust pipe for discharging cathode tail gas after absorption treatment, the secondary absorption system is arranged between the primary absorption system and the secondary absorption system, and the mixed solution is respectively introduced into the primary absorption system, the secondary absorption system and the tertiary absorption system;
s2, leading tail gas discharged by the cathode of the electrolytic cell during nitrogen trifluoride production into a primary absorption system through a cathode tail gas discharge pipe, and carrying out tertiary absorption treatment on the tail gas through a mixed solution sequentially through the primary absorption system, the secondary absorption system and a tertiary absorption system;
s3, discharging the tail gas subjected to the tertiary absorption treatment through an exhaust pipe, introducing the mixed solution in the primary absorption system into an electrolytic cell, introducing the mixed solution in the secondary absorption system into the primary absorption system, introducing the mixed solution in the tertiary absorption system into the secondary absorption system, and adding a new mixed solution into the tertiary absorption system;
and S4, repeating the steps S1-S3 to carry out tail gas absorption treatment again.
2. The process of claim 1, wherein the ratio of ammonium acid fluoride in the mixed solution prepared in S1 is as follows: the mass ratio of the hydrogen fluoride is (3-4): 1, after the absorption treatment in S2, the ratio of ammonium bifluoride in the mixed solution in the primary absorption system: the mass ratio of hydrogen fluoride is 1: 1.
3. The process for treating tail gas discharged from the cathode of a nitrogen trifluoride electrolyzer as claimed in claim 1, it is characterized in that the primary absorption system comprises a primary absorption container, a primary circulating pump and a primary solution storage tank which are sequentially communicated through pipelines, the secondary absorption system comprises a secondary absorption container, a secondary circulating pump and a secondary solution storage tank which are sequentially communicated through pipelines, the three-stage absorption system comprises a three-stage absorption container, a three-stage circulating pump and a three-stage solution storage tank which are sequentially communicated through a pipeline, the primary absorption container is connected with the cathode tail gas discharge pipe, the tertiary absorption container is connected with the exhaust pipe, the primary absorption container, the secondary absorption container and the tertiary absorption container are communicated through pipelines, and the first-stage solution storage tank, the second-stage solution storage tank and the third-stage solution storage tank are filled with the mixed solution.
4. The process for treating tail gas discharged from the cathode of a nitrogen trifluoride electrolyzer as claimed in claim 3, characterized in that the working pressure of the primary circulating pump, the secondary circulating pump and the tertiary circulating pump is 0.1-0.3MPa, the working temperature is normal temperature, and the working flow rate is 5-253/h。
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111311673.5A CN113842753A (en) | 2021-11-08 | 2021-11-08 | Treatment process of tail gas discharged from cathode of nitrogen trifluoride electrolytic cell |
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| CN202111311673.5A CN113842753A (en) | 2021-11-08 | 2021-11-08 | Treatment process of tail gas discharged from cathode of nitrogen trifluoride electrolytic cell |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534453A (en) * | 2022-03-24 | 2022-05-27 | 中船(邯郸)派瑞特种气体股份有限公司 | Process for recovering HF (hydrogen fluoride) in cathode tail gas discharged from nitrogen trifluoride electrolytic cell |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3966877A (en) * | 1974-09-11 | 1976-06-29 | Vladimir Sergeevich Kalach | Method of processing of waste gases |
| CN206308012U (en) * | 2016-12-31 | 2017-07-07 | 山东飞源科技有限公司 | For the fluorination hydrogen recovery unit of Nitrogen trifluoride production technology |
| CN111085086A (en) * | 2019-12-31 | 2020-05-01 | 中船重工（邯郸）派瑞特种气体有限公司 | NF prepared by electrolysis3System and method for recovering HF in tail gas of electrolysis system |
| CN111875124A (en) * | 2020-06-05 | 2020-11-03 | 中船重工（邯郸）派瑞特种气体有限公司 | Treatment method of nickel-containing waste residue wastewater generated in nitrogen trifluoride preparation process |
| CN112191081A (en) * | 2020-09-01 | 2021-01-08 | 中船重工（邯郸）派瑞特种气体有限公司 | Method and system for treating hydrogen fluoride tail gas generated in nitrogen trifluoride preparation process |
-
2021
- 2021-11-08 CN CN202111311673.5A patent/CN113842753A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3966877A (en) * | 1974-09-11 | 1976-06-29 | Vladimir Sergeevich Kalach | Method of processing of waste gases |
| CN206308012U (en) * | 2016-12-31 | 2017-07-07 | 山东飞源科技有限公司 | For the fluorination hydrogen recovery unit of Nitrogen trifluoride production technology |
| CN111085086A (en) * | 2019-12-31 | 2020-05-01 | 中船重工（邯郸）派瑞特种气体有限公司 | NF prepared by electrolysis3System and method for recovering HF in tail gas of electrolysis system |
| CN111875124A (en) * | 2020-06-05 | 2020-11-03 | 中船重工（邯郸）派瑞特种气体有限公司 | Treatment method of nickel-containing waste residue wastewater generated in nitrogen trifluoride preparation process |
| CN112191081A (en) * | 2020-09-01 | 2021-01-08 | 中船重工（邯郸）派瑞特种气体有限公司 | Method and system for treating hydrogen fluoride tail gas generated in nitrogen trifluoride preparation process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534453A (en) * | 2022-03-24 | 2022-05-27 | 中船(邯郸)派瑞特种气体股份有限公司 | Process for recovering HF (hydrogen fluoride) in cathode tail gas discharged from nitrogen trifluoride electrolytic cell |
| CN114534453B (en) * | 2022-03-24 | 2023-05-02 | 中船(邯郸)派瑞特种气体股份有限公司 | Recovery process of HF in cathode tail gas discharged by nitrogen trifluoride electrolytic tank |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Applicant after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Applicant before: PERIC SPECIAL GASES Co.,Ltd. |