CN118326320A - Passivation treatment method for storage electronic grade corrosive liquefied gas steel cylinder - Google Patents
Passivation treatment method for storage electronic grade corrosive liquefied gas steel cylinder Download PDFInfo
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- CN118326320A CN118326320A CN202410355906.9A CN202410355906A CN118326320A CN 118326320 A CN118326320 A CN 118326320A CN 202410355906 A CN202410355906 A CN 202410355906A CN 118326320 A CN118326320 A CN 118326320A
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- steel cylinder
- liquefied gas
- electronic grade
- passivation
- vacuumizing
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 121
- 239000010959 steel Substances 0.000 title claims abstract description 121
- 238000002161 passivation Methods 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000003860 storage Methods 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 76
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- 238000010926 purge Methods 0.000 claims abstract description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 20
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 7
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 5
- 239000010962 carbon steel Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 16
- 239000012535 impurity Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 5
- 238000010408 sweeping Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
The application belongs to the field of passivation treatment of chemical equipment, and particularly relates to a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder; the method comprises the following steps: s1, vacuumizing a steel cylinder to be treated; s2, carrying out nitrogen replacement treatment on the steel cylinder; s3, vacuumizing the steel cylinder, and filling electronic grade corrosive liquefied gas; s4, horizontally placing the steel cylinder so that the axis of the steel cylinder is in a horizontal state, and rotating the steel cylinder around the axis for at least 2 days in an environment of not lower than 60 ℃ to form a passivation film; and S5, vacuumizing the electronic grade corrosive liquefied gas in the steel cylinder, then introducing argon to purge and replace, and vacuumizing the steel cylinder. The application adopts nitrogen to replace water, and carries out pivoting treatment on the steel cylinder, so that a uniform and compact passivation film is formed on the surface of the inner wall of the steel cylinder, and the corrosion rate of gas to the inner wall of the steel cylinder is slowed down. The steel cylinders treated by the method have stable gas indexes within 2 years.
Description
Technical Field
The application belongs to the field of passivation treatment of chemical equipment, relates to a passivation treatment method of a storage steel cylinder, and in particular relates to a passivation treatment method of a storage electronic grade corrosive liquefied gas steel cylinder.
Background
The special gas is a support material necessary for industries such as integrated circuits, display panels and the like, is widely used in the fields of photoetching, etching, film forming, cleaning and the like, and has extremely high requirements on the purity of the gas and the stability of products in each field. In order to prevent secondary pollution, the storage and transportation of the gas must be effectively controlled.
The cleanliness of the packaging container greatly influences the quality stability of the stored gas inside. In general, moisture, metal ions, and particulate impurities that are difficult to remove remain inside a newly purchased steel cylinder. Under certain conditions, electronic grade corrosive liquefied gases (such as hydrogen chloride, hydrogen bromide, hydrogen fluoride and the like) can react with the container to form chemical corrosion, so that the impurity content in the gases is unstable, and the quality of products is affected.
The Chinese patent with the application publication number of CN115574254A carries out electrolytic polishing on the steel cylinder to control the roughness of the steel cylinder, then carries out the processes of baking, passivation and the like, and improves the product quality stability of high-purity electronic gas contained in the steel cylinder, but the process takes longer time and has larger energy consumption. The invention patent with the application publication number of CN115029657A carries out the processes of preheating, heating and baking, vacuumizing, passivating, cooling, pressurizing and testing on the steel cylinder, improves the comprehensive performance of the steel cylinder, but has relatively complex flow. The invention patent with the application publication number of CN113005389A provides a treatment method for an electronic grade chlorine trifluoride packaging steel cylinder, namely, the chlorine trifluoride steel cylinder is subjected to passivation treatment twice by utilizing fluorine gas. In the steel cylinder treatment method in the related art, in the process of passivating the inner wall of the steel cylinder by using the product gas, the steel cylinder is in a static state, and uniform reaction between the gas and the inner wall of the steel cylinder cannot be ensured.
Therefore, developing a steel cylinder passivation treatment method with simple flow, short time consumption and good treatment effect is important for improving the quality stability of products.
Disclosure of Invention
In order to optimize and absorb various defects of the steel cylinder treatment method in the prior art and ensure the stability of the quality of electronic grade corrosive liquefied gas, the application provides a steel cylinder passivation treatment method which is used for pretreating the steel cylinder through nitrogen replacement and removing part of impurities on the inner wall of the steel cylinder. Then, the steel cylinder for storing the product gas is horizontally placed on a gas cylinder mixing device in a high-temperature environment, so that the steel cylinder continuously rotates around the shaft, and a uniform passivation film is formed on the inner wall. The steel cylinder treated by the method stores electronic grade corrosive liquefied gas, the purity of the gas can be kept for two years, and the quality stability of the product is improved.
The application provides a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder, which adopts the following technical scheme:
a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder comprises the following steps:
S1, vacuumizing a steel cylinder to be treated;
S2, after the vacuumizing is finished, carrying out nitrogen replacement treatment on the steel cylinder;
S3, after nitrogen replacement treatment, vacuumizing the steel cylinder, and then filling electronic grade corrosive liquefied gas;
s4, horizontally placing the steel cylinder so that the axis of the steel cylinder is in a horizontal state, and then rotating the steel cylinder around the axis for at least 2 days in an environment of not lower than 60 ℃ to form a passivation film;
and S5, vacuumizing the electronic grade corrosive liquefied gas in the steel cylinder, then introducing argon to purge and replace the steel cylinder, and vacuumizing the steel cylinder to complete the passivation treatment of the steel cylinder for storing the electronic grade corrosive liquefied gas.
In a specific embodiment, the electronic grade corrosive liquefied gas comprises any one of hydrogen chloride, hydrogen fluoride, hydrogen bromide, silicon tetrafluoride, and boron trichloride.
In a specific embodiment, the steel cylinder is made of carbon steel or stainless steel.
In a specific embodiment, all the vacuum-pumping steps S1, S3, S5 are specifically: pumping the pressure in the steel cylinder to less than or equal to-0.095 MPa.
In a specific embodiment, in S4, the ambient temperature of the pivoting treatment is 60 ℃ to 80 ℃ and the high temperature treatment time is 2 to 4 days.
In a specific embodiment, the purity of nitrogen used for the replacement in S2 is more than or equal to 99.999%; the purity of argon for purging and replacement in S5 is more than or equal to 99.999 percent
The application has the following beneficial technical effects: compared with the prior art, the application firstly adopts nitrogen to replace treatment to remove the residual moisture in the steel cylinder, then fills high-purity electronic grade corrosive liquefied gas into the pretreated steel cylinder, carries out continuous pivoting treatment on the steel cylinder in a high-temperature environment, promotes the stable reaction of the gas and the inner wall of the steel cylinder, thereby forming a uniform and compact passivation film on the surface of the inner wall of the steel cylinder, playing a certain role in protecting the material of the inner wall and slowing down the corrosion rate of the gas on the inner wall of the steel cylinder. The method provided by the application is used for treating the steel cylinder, and the stored corrosive gas is stable in index within 2 years, so that the stability of the product quality is greatly improved.
Detailed Description
In the field of industrial gas storage, before gas is stored in a steel cylinder, a newly purchased steel cylinder needs to be subjected to passivation cleaning treatment, and the technical problems of long time consumption, high energy consumption and complex flow in the prior art exist, so that the applicant proposes the following process steps in combination with actual production experience: vacuumizing the steel cylinder to be treated to-0.095 MPa or below, then performing nitrogen replacement treatment on the steel cylinder to remove impurities such as water in the steel cylinder, vacuumizing to a pressure of less than or equal to-0.095 MPa, and then filling electronic grade corrosive liquefied gas to passivate the steel cylinder; the specific operation of passivation is: the cylinder is horizontally placed by using a cylinder mixing device manufactured by Ningjin Rongda mechanical manufacturing limited company, then the cylinder is subjected to shaft winding treatment in an environment of not lower than 60 ℃, the rotation speed is 10r/min at a positive and negative rotation interval, and the time is at least 2 days, so that a uniform passivation film is formed in the cylinder, and the inner wall material of the cylinder is protected; and then vacuumizing to-0.095 MPa or below, introducing argon gas for purging replacement, and vacuumizing the steel cylinder to complete passivation treatment of the steel cylinder.
When the steel cylinder passivated by the method stores corrosive gas, the gas stability is good, the purity is well preserved, the process is simple and easy to implement, the operations such as high-temperature baking and preheating are not needed, the steps are simple, the energy consumption is low, and the method is convenient and efficient.
The following describes the embodiments of the present application in further detail with reference to specific examples.
In the method provided by the application, the electronic grade corrosive liquefied gas can be hydrogen chloride, hydrogen fluoride, hydrogen bromide, silicon tetrafluoride or boron trichloride, and the following examples are only examples.
Example 1
The embodiment of the application provides a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder, which comprises the following specific steps:
S1: vacuumizing the carbon steel cylinder to be treated to the pressure of-0.095 MPa;
s2: carrying out nitrogen replacement treatment on the steel cylinder, wherein the purity of the used nitrogen is more than or equal to 99.999%;
s3: vacuumizing the air placed in the steel cylinder to the pressure of-0.095 MPa, and filling high-purity hydrogen fluoride gas;
S4: the steel bottle treated by the S3 is horizontally placed on a rolling shaft of a gas bottle mixing device, the ambient temperature is set to be 60 ℃, and the steel bottle is subjected to shaft rotation treatment for 4 days to form a uniform passivation film;
S5: after the passivation gas in the steel cylinder is vacuumized, argon is introduced to carry out sweeping and replacement treatment, and the purity of the used argon is more than or equal to 99.999%;
s6: after the steel cylinder is vacuumized to the pressure of-0.095 MPa, 2kg of hydrogen fluoride gas with the purity of more than or equal to 99.999% is filled into the steel cylinder.
The gas index change in the steel bottle in 2 years is shown in table 1, and the purity detection period is one detection every half year, and three detection are carried out in parallel.
TABLE 1 index Change of high purity Hydrogen fluoride gas
The detection result shows that the content of each impurity is within the standard line of the product within 2 years of storage, and the quality of the product is stable.
Example 2
The application provides a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder, which comprises the following specific steps:
S1: vacuumizing the stainless steel cylinder to be treated until the pressure is minus 0.095MPa;
s2: carrying out nitrogen replacement treatment on the steel cylinder, wherein the purity of the used nitrogen is more than or equal to 99.999%;
s3: vacuumizing the air placed in the steel cylinder until the pressure is minus 0.095MPa, and filling high-purity hydrogen chloride gas;
S4: the steel bottle treated by the S3 is horizontally placed on a rolling shaft of a gas bottle mixing device, the ambient temperature is set to 80 ℃, and the steel bottle is subjected to axial rotation treatment for 2 days to form a uniform passivation film;
S5: after the passivation gas in the steel cylinder is vacuumized, argon is introduced to carry out sweeping and replacement treatment, and the purity of the used argon is more than or equal to 99.999%;
S6: after the steel cylinder is vacuumized until the pressure is minus 0.095MPa, 2kg of hydrogen chloride gas with the purity of more than or equal to 99.999 percent is filled into the steel cylinder.
The gas index change in the steel bottle in 2 years is shown in table 2, and the purity detection period is one detection every half year, and three detection are carried out in parallel.
TABLE 2 index Change of high purity Hydrogen chloride gas
The detection result shows that the content of each impurity is within the standard line of the product within 2 years of storage, and the quality of the product is stable.
Example 3
The application provides a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder, which comprises the following specific steps:
s1: vacuumizing the carbon steel cylinder to be treated until the pressure is minus 0.095MPa;
s2: carrying out nitrogen replacement treatment on the steel cylinder, wherein the purity of the used nitrogen is more than or equal to 99.999%;
S3: vacuumizing the air placed in the steel cylinder to the pressure of-0.095 MPa, and filling high-purity hydrogen bromide gas;
s4: the steel bottle treated by the S3 is horizontally placed on a rolling shaft of a gas bottle mixing device, the ambient temperature is set to be 70 ℃, and the steel bottle is subjected to shaft rotation treatment for 3 days to form a uniform passivation film;
S5: after the passivation gas in the steel cylinder is vacuumized, argon is introduced to carry out sweeping and replacement treatment, and the purity of the used argon is more than or equal to 99.999%;
S6: after the steel cylinder is vacuumized to the pressure of-0.095 MPa, 2kg of hydrogen bromide gas with the purity of more than or equal to 99.999% is filled into the steel cylinder.
The gas index change in the steel bottle in 2 years is shown in table 3, and the purity detection period is one detection every half year, and three detection are carried out in parallel.
TABLE 3 index Change of high purity Hydrogen bromide gas
The detection result shows that the content of each impurity is within the standard line of the product within 2 years of storage, and the quality of the product is stable.
Example 4
The application provides a passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder, which comprises the following specific steps:
s1: vacuumizing the carbon steel cylinder to be treated until the pressure is minus 0.095MPa;
s2: carrying out nitrogen replacement treatment on the steel cylinder, wherein the purity of the used nitrogen is more than or equal to 99.999%;
S3: vacuumizing the air placed in the steel cylinder to the pressure of-0.095 MPa, and filling high-purity hydrogen bromide gas;
S4: performing horizontal standing treatment on the steel bottle subjected to the S3 treatment, setting the ambient temperature to 70 ℃, and performing standing treatment for 3 days to form a passivation film;
S5: after the passivation gas in the steel cylinder is vacuumized, argon is introduced to carry out sweeping and replacement treatment, and the purity of the used argon is more than or equal to 99.999%;
S6: after the steel cylinder is vacuumized to the pressure of-0.095 MPa, 2kg of hydrogen bromide gas with the purity of more than or equal to 99.999% is filled into the steel cylinder.
The gas index change in the steel bottle in 2 years is shown in table 4, and the purity detection period is one detection every half year, and three detection are carried out in parallel.
TABLE 4 index Change of high purity Hydrogen bromide gas
The detection result shows that the impurity content has an ascending trend within 2 years of storage, and the product quality exceeds the index range and is unstable.
Comparison of example 3 and example 4 shows that when the steel cylinder in S4 is kept horizontally stationary without taking any rotation measures, the passivation effect is relatively poor and the stability of the product is lowered under the condition that other conditions are unchanged.
The above; is only a preferred embodiment of the present application; the scope of the application is not limited in this respect; any person skilled in the art is within the technical scope of the present disclosure; equivalent substitutions or changes are made according to the technical proposal of the application and the improved conception thereof; are intended to be encompassed within the scope of the present application.
Claims (6)
1. A passivation treatment method for a storage electronic grade corrosive liquefied gas steel cylinder is characterized by comprising the following steps:
S1, vacuumizing a steel cylinder to be treated;
S2, after the vacuumizing is finished, carrying out nitrogen replacement treatment on the steel cylinder;
S3, after nitrogen replacement treatment, vacuumizing the steel cylinder, and then filling electronic grade corrosive liquefied gas;
s4, horizontally placing the steel cylinder so that the axis of the steel cylinder is in a horizontal state, and then rotating the steel cylinder around the axis for at least 2 days in an environment of not lower than 60 ℃ to form a passivation film;
and S5, vacuumizing the electronic grade corrosive liquefied gas in the steel cylinder, then introducing argon to purge and replace the steel cylinder, and vacuumizing the steel cylinder to complete the passivation treatment of the steel cylinder for storing the electronic grade corrosive liquefied gas.
2. The passivation method for the storage electronic grade corrosive liquefied gas steel cylinder according to claim 1, wherein the passivation method comprises the following steps: the electronic grade corrosive liquefied gas comprises any one of hydrogen chloride, hydrogen fluoride, hydrogen bromide, silicon tetrafluoride and boron trichloride.
3. The passivation method for the storage electronic grade corrosive liquefied gas steel cylinder according to claim 1, wherein the passivation method comprises the following steps: the steel cylinder is made of carbon steel or stainless steel.
4. The passivation method for the storage electronic grade corrosive liquefied gas steel cylinder according to claim 1, wherein the passivation method comprises the following steps: the vacuum pumping steps in the steps S1, S3 and S5 are specifically as follows: pumping the pressure in the steel cylinder to less than or equal to-0.095 MPa.
5. The passivation method for the storage electronic grade corrosive liquefied gas steel cylinder according to claim 1, wherein the passivation method comprises the following steps: s4, the environment temperature of the pivoting treatment is 60-80 ℃, and the high-temperature treatment time is 2-4 days.
6. The passivation method for the storage electronic grade corrosive liquefied gas steel cylinder according to claim 1, wherein the passivation method comprises the following steps: the purity of the nitrogen for replacement in S2 is more than or equal to 99.999%; and the purity of argon for purging and replacing in S5 is more than or equal to 99.999 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410355906.9A CN118326320A (en) | 2024-03-27 | 2024-03-27 | Passivation treatment method for storage electronic grade corrosive liquefied gas steel cylinder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410355906.9A CN118326320A (en) | 2024-03-27 | 2024-03-27 | Passivation treatment method for storage electronic grade corrosive liquefied gas steel cylinder |
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| CN118326320A true CN118326320A (en) | 2024-07-12 |
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| CN202410355906.9A Pending CN118326320A (en) | 2024-03-27 | 2024-03-27 | Passivation treatment method for storage electronic grade corrosive liquefied gas steel cylinder |
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