CN113005389B - Method for treating packaging steel bottle of electronic grade chlorine trifluoride - Google Patents
Method for treating packaging steel bottle of electronic grade chlorine trifluoride Download PDFInfo
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- CN113005389B CN113005389B CN202110142238.8A CN202110142238A CN113005389B CN 113005389 B CN113005389 B CN 113005389B CN 202110142238 A CN202110142238 A CN 202110142238A CN 113005389 B CN113005389 B CN 113005389B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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Abstract
The invention provides a processing method of an electronic grade chlorine trifluoride packaging steel bottle, which comprises the following steps: s1, vacuumizing the gas in a packaging steel cylinder, and filling a certain amount of high-purity fluorine gas with the purity of more than 99% for fluorine gas passivation treatment; s2, analyzing the gas in the packaging steel cylinder without generating other impurity gases, entering a step S3, otherwise, entering a step S1, and repeating the treatment; s3, vacuumizing the gas in the packaging steel cylinder, and then filling a certain amount of high-purity chlorine trifluoride with purity of more than 99.9% for secondary passivation treatment; s4, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a layer of compact chlorine trifluoride passivation film is formed in the packaging steel cylinder qualified in treatment, and entering a step S5, otherwise, entering a step S3 to repeat treatment; and S5, detecting metal ions in the packaging steel cylinders, repeating the S3 for reprocessing if the metal ions exceed the standard, and evacuating for later use after the metal ions are analyzed to be qualified.
Description
Technical Field
The invention relates to a method for processing an electronic grade chlorine trifluoride packaging steel bottle.
Background
Chlorine trifluoride is currently a very strong oxidizing and fluorinating agent that reacts with most organic and inorganic materials, even plastics, and can cause severe combustion, and in some cases even explosion, of many materials without contact with a fire source. The requirements for the package are also extremely stringent due to the particular oxidizing nature of chlorine trifluoride. Although there is a preparation process of industrial grade chlorine trifluoride in China, the treatment method of the product packaging container is not suitable for sub-packaging and storage of electronic grade chlorine trifluoride, and the treatment method of the chlorine trifluoride package is not seen in China.
Disclosure of Invention
The invention provides a treatment method of an electronic grade chlorine trifluoride packaging steel bottle, which can effectively solve the problems.
The invention is realized in the following way:
a method for processing a packaging steel cylinder of electronic grade chlorine trifluoride, wherein the packaging steel cylinder is a stainless steel welding steel cylinder; the processing method comprises the following steps:
s1, vacuumizing the gas in a packaging steel cylinder, and then filling a certain amount of high-purity fluorine gas with the purity of more than 99% for passivation treatment of the fluorine gas;
s2, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a compact fluorinated passivation film is formed in the pretreatment qualified packaging steel cylinder, and entering a step S3, otherwise, entering a step S1 to repeat treatment;
s3, vacuumizing the gas in the packaging steel cylinder, and then filling a certain amount of high-purity chlorine trifluoride with purity of more than 99.9% for secondary passivation treatment;
s4, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a layer of compact chlorine trifluoride passivation film is formed in the packaging steel cylinder qualified in treatment, and entering a step S5, otherwise, entering a step S3 to repeat treatment;
and S5, detecting metal ions in the packaging steel cylinders, repeating the S3 for reprocessing if the metal ions exceed the standard, and evacuating for later use after the metal ions are analyzed to be qualified.
As a further improvement, the design pressure of the packaging steel cylinder is more than 1.6Mpa, an electric or pneumatic steel cylinder valve is selected as the packaging steel cylinder, the steel cylinder valve is connected with the bottle body by hard connection, the polishing of the inner surface of the valve is less than Rmax 0.8 mu m, and the leakage quantity is less than 2*E-11 Torr L/sec.
As a further improvement, in step S1, the step of evacuating the gas inside the packaging steel cylinder includes:
s11, vacuumizing the gas in the packaging steel cylinder to below 5 Pa.
As a further improvement, in step S1, the step of filling a certain amount of high-purity fluorine gas with a purity of 99% or more to perform the fluorine gas passivation treatment includes:
filling high-purity fluorine gas with purity of more than 99% of 1 kPa-5 kPa for 1-5 days, and carrying out fluorine gas passivation treatment inside the packaging steel cylinder.
As a further improvement, in step S3, the step of evacuating the gas inside the packaging steel cylinder includes:
s11, vacuumizing the gas in the packaging steel cylinder to below 5 Pa.
As a further improvement, in step S3, the step of charging a certain amount of high-purity chlorine trifluoride having a purity of 99.9% or more to perform the secondary passivation treatment includes:
filling high-purity chlorine trifluoride with the purity of more than 99.9 percent and 500 Pa-2 kPa for 1-5 days, and performing secondary passivation treatment on the inside of the packaging steel cylinder.
As a further improvement, after step S5, further comprising:
s6, charging a certain amount of electronic grade chlorine trifluoride for a period of time, detecting metal ions, if the analysis is unqualified, evacuating the steel cylinder, and repeating the step S6; and after the metal ions are analyzed to be qualified, the metal ions are used as a qualified circulation bottle to continue standby and wait for filling.
As a further improvement, in step S6, the step of charging an amount of electronic grade chlorine trifluoride for a period of time comprises:
s61, charging 5kPa to 10kPa electronic grade chlorine trifluoride for 1 to 5 hours.
The beneficial effects of the invention are as follows: firstly, the interior of the packaging steel cylinder and the interior channel of the valve are pretreated for multiple times, a fluoride film protective layer in a form of combining fluorine and chlorine trifluoride is formed in the bottle, and safer protection is provided for the gas in the packaging steel cylinder from corroding the bottle wall; secondly, stainless steel cylinders are selected, so that the cost is greatly reduced; thirdly, through analysis and detection, the integrality of the fluoride film inside the steel cylinder can be known at the straight end, and the leakage rate of the steel cylinder is greatly reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural view of a packaging device for electronic grade chlorine trifluoride according to an embodiment of the present invention.
Fig. 2 is a flowchart of a processing method of a packaging steel cylinder in a packaging device of electronic grade chlorine trifluoride provided by the embodiment of the invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Referring to fig. 1, an embodiment of the present invention provides a packaging apparatus for electronic grade chlorine trifluoride, including:
an inner tank 10 including a packing cylinder 101, a feed pipe 102 and a discharge pipe 103 provided at the top and bottom of the packing cylinder 101, and a pressure sensor 104 for measuring the pressure inside the packing cylinder 101;
a jacket sandwich 12 including a stainless steel outer layer 120 wrapped around the inner tank 10, and an inert gas inlet pipe 121 and an inert gas outlet pipe 122 communicating with the stainless steel outer layer 120;
the condensing assembly 11 is clamped between the jacket interlayer 12 and the inner tank 10, and comprises a condensing pipeline 111, and a liquid inlet pipeline 110 and a liquid outlet pipeline 112 which are respectively communicated with the condensing pipeline 111;
the system comprises an analysis component and an alarm component, wherein the analysis component is used for analyzing the content of chlorine trifluoride in inert gas, and the alarm component is used for alarming when detecting the chlorine trifluoride.
As a further improvement, the surface finish of the inner surface of the packing cylinder 101 is < Rmax 8 μm. The packaging steel cylinder can be a stainless steel welding steel cylinder. The design pressure of the packaging steel cylinder is more than 1.6Mpa, the packaging steel cylinder adopts an electric or pneumatic steel cylinder valve, the steel cylinder valve is connected with the bottle body by hard connection, the polishing of the inner surface of the valve is less than Rmax 0.8 mu m, and the leakage quantity is less than 2*E-11 Torr L/sec
As a further improvement, the temperature of the condensing unit 11 ranges from-30 ℃ to-50 ℃. More preferably, the temperature of the condensing unit 11 ranges from-35 ℃ to-40 ℃. The low temperature can provide a cold source for collecting the chlorine trifluoride, so that the chlorine trifluoride is rapidly cooled and liquefied to form negative pressure, and the negative pressure is stored in the packaging device (because in the actual operation process, the chlorine trifluoride has extremely strong corrosiveness, and the filling pressure or power cannot be provided by using devices such as a pump and the like).
As a further improvement, the electronic grade chlorine trifluoride packaging device further comprises a weighing assembly (not shown) for obtaining the actual storage amount of the chlorine trifluoride. Since the chlorine trifluoride has a high activity and is a gas-liquid two-phase coexisting material, it is necessary to strictly control the actual storage amount thereof to prevent occurrence of danger. Defining the volume of the packing cylinder 101 as ML, preferably, the maximum liquid storage amount of the chlorine trifluoride is 1/2ML, and the maximum storage amount of the chlorine trifluoride is about 1.42Mkg calculated according to the physical parameters thereof. In order to reduce the risk of the electronic grade chlorine trifluoride packing device, the packing cylinder 101 preferably has a volume ML of 5 to 10L. In one embodiment, the packing cylinder 101 has a volume ML of about 5L, so the maximum liquid storage amount of the chlorine trifluoride is 2.5L, thereby obtaining a maximum storage amount of the chlorine trifluoride of about 3.55kg.
As a further improvement, the alarm assembly is further used for alarming and stopping filling and collecting chlorine trifluoride when the actual storage amount is equal to the maximum storage amount.
Referring to fig. 2, the embodiment of the invention further provides a method for processing the packaging steel cylinder 101, which includes the following steps:
s1, vacuumizing the gas in a packaging steel cylinder, and then filling a certain amount of high-purity fluorine gas with the purity of more than 99% for passivation treatment of the fluorine gas;
s2, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a compact fluorinated passivation film is formed in the pretreatment qualified packaging steel cylinder, and entering a step S3, otherwise, entering a step S1 to repeat treatment;
s3, vacuumizing the gas in the packaging steel cylinder, and then filling a certain amount of high-purity chlorine trifluoride with purity of more than 99.9% for secondary passivation treatment;
s4, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a layer of compact chlorine trifluoride passivation film is formed in the packaging steel cylinder qualified in treatment, and entering a step S5, otherwise, entering a step S3 to repeat treatment;
and S5, detecting metal ions in the packaging steel cylinders, repeating the S3 for reprocessing if the metal ions exceed the standard, and evacuating for later use after the metal ions are analyzed to be qualified.
As a further improvement, in step S1, the step of evacuating the gas inside the packaging steel cylinder includes:
s11, vacuumizing the gas in the packaging steel cylinder to below 5 Pa.
As a further improvement, in step S1, the step of filling a certain amount of high-purity fluorine gas with a purity of 99% or more to perform the fluorine gas passivation treatment includes:
filling high-purity fluorine gas with purity of more than 99% of 1 kPa-5 kPa for 1-5 days, and carrying out fluorine gas passivation treatment inside the packaging steel cylinder. In one embodiment, the inside of the packaging steel cylinder is filled with high-purity fluorine gas with the purity of 2kPa and 99 percent for 2 days to carry out fluorine gas passivation treatment.
In step S2, the gas may be analyzed by infrared or other analysis methods.
As a further improvement, in step S3, the step of evacuating the gas inside the packaging steel cylinder includes:
s11, vacuumizing the gas in the packaging steel cylinder to below 5 Pa.
As a further improvement, in step S3, the step of charging a certain amount of high-purity chlorine trifluoride having a purity of 99.9% or more to perform the secondary passivation treatment includes:
filling high-purity chlorine trifluoride with the purity of more than 99.9 percent and 500 Pa-2 kPa for 1-5 days, and performing secondary passivation treatment on the inside of the packaging steel cylinder. In one example, the package cylinder interior is subjected to a secondary passivation treatment for 3 days filled with high purity chlorine trifluoride having a purity of 99.9% at 1 kPa.
As a further improvement, after step S5, further comprising:
s6, charging a certain amount of electronic grade chlorine trifluoride for a period of time, detecting metal ions, if the analysis is unqualified, evacuating the steel cylinder, and repeating the step S6; and after the metal ions are analyzed to be qualified, the metal ions are used as a qualified circulation bottle to continue standby and wait for filling. Detection of metal ions may be performed by infrared analysis or other methods.
As a further improvement, in step S6, the step of charging an amount of electronic grade chlorine trifluoride for a period of time comprises:
s61, charging 5kPa to 10kPa electronic grade chlorine trifluoride for 1 to 5 hours. In one example, 8kPa electronic grade chlorine trifluoride is charged for 3 hours. In the latter stage, the passivation rate can be increased by introducing higher pressure chlorine trifluoride.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for processing a packaging steel cylinder in a packaging device of electronic grade chlorine trifluoride, wherein the packaging steel cylinder is a stainless steel welding steel cylinder; the packaging device is characterized by comprising an inner tank, wherein the inner tank comprises the packaging steel cylinder, a feeding pipe, a discharging pipe and a pressure sensor, the feeding pipe and the discharging pipe are arranged at the top and the bottom of the packaging steel cylinder, and the pressure sensor is used for measuring the internal pressure of the packaging steel cylinder; the jacket interlayer comprises a stainless steel outer layer wrapped on the inner tank, and an inert gas inlet pipeline and an inert gas outlet pipeline which are communicated with the stainless steel outer layer; the condensing assembly is clamped and arranged between the outer sleeve interlayer and the inner tank and comprises a condensing pipeline, and a liquid inlet pipeline and a liquid outlet pipeline which are respectively communicated with the condensing pipeline; the system comprises an analysis component and an alarm component, wherein the analysis component is used for analyzing the content of chlorine trifluoride in inert gas, and the alarm component is used for alarming when detecting the chlorine trifluoride; the volume of the packaging steel bottle is ML 5-10L, and the maximum liquid storage amount of the chlorine trifluoride is 1/2ML;
the processing method comprises the following steps:
s1, vacuumizing the gas in a packaging steel cylinder, and then filling a certain amount of high-purity fluorine gas with the purity of more than 99% for performing fluorine gas passivation treatment, wherein the method specifically comprises the following steps: filling high-purity fluorine gas with the purity of more than 99% of 1-5 kPa for 2 days, and carrying out fluorine gas passivation treatment inside the packaging steel cylinder;
s2, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a compact fluorinated passivation film is formed in the pretreatment qualified packaging steel cylinder, and entering a step S3, otherwise, entering a step S1 to repeat treatment;
s3, vacuumizing the gas in the packaging steel cylinder, and then filling a certain amount of high-purity chlorine trifluoride with purity of more than 99.9% for secondary passivation treatment, wherein the method specifically comprises the following steps: filling 500 Pa-2 kPa high-purity chlorine trifluoride with purity of more than 99.9% for 3 days, and performing secondary passivation treatment on the inside of the packaging steel cylinder;
s4, analyzing the gas in the packaging steel cylinder without generating other impurity gases, judging that a layer of compact chlorine trifluoride passivation film is formed in the packaging steel cylinder qualified in treatment, and entering a step S5, otherwise, entering a step S3 to repeat treatment;
and S5, detecting metal ions in the packaging steel cylinders, repeating the S3 for reprocessing if the metal ions exceed the standard, and evacuating for later use after the metal ions are analyzed to be qualified.
2. The method of claim 1, wherein the design pressure of the packing cylinder is greater than 1.6Mpa, the packing cylinder is an electric or pneumatic cylinder valve, the cylinder valve is connected with the cylinder body by hard connection, the polishing of the inner surface of the valve is less than Rmax 0.8 ㎛, and the leakage is less than 2*E-11 Torr L/sec.
3. The method for processing a packing steel cylinder in a packing apparatus for electronic grade chlorine trifluoride as claimed in claim 1, wherein in step S1, said step of evacuating the gas inside the packing steel cylinder comprises:
s11, vacuumizing the gas in the packaging steel cylinder to below 5 Pa.
4. The method for processing a packing steel cylinder in a packing apparatus for electronic grade chlorine trifluoride as claimed in claim 1, wherein in step S3, said step of evacuating the gas inside the packing steel cylinder comprises:
s11, vacuumizing the gas in the packaging steel cylinder to below 5 Pa.
5. The method of processing a packing steel cylinder in a packing apparatus for electronic grade chlorine trifluoride as recited in claim 1, further comprising, after step S5:
s6, charging a certain amount of electronic grade chlorine trifluoride for a period of time, detecting metal ions, if the analysis is unqualified, evacuating the steel cylinder, and repeating the step S6; and after the metal ions are analyzed to be qualified, the metal ions are used as a qualified circulation bottle to continue standby and wait for filling.
6. The method of claim 5, wherein in step S6, the step of charging the amount of electronic grade chlorine trifluoride for a period of time comprises:
and S61, charging 5-10 kPa of electronic grade chlorine trifluoride for 1-5 hours.
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| CN202110142238.8A CN113005389B (en) | 2021-02-02 | 2021-02-02 | Method for treating packaging steel bottle of electronic grade chlorine trifluoride |
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| CN108884548A (en) * | 2016-04-05 | 2018-11-23 | 关东电化工业株式会社 | Material, using the material preservation container, be installed on the application method of the valve of the preservation container and the store method of ClF, ClF container |
| CN110832106A (en) * | 2017-08-01 | 2020-02-21 | 中央硝子株式会社 | Method for producing filled container and filled container |
| CN111041403A (en) * | 2019-12-29 | 2020-04-21 | 中船重工（邯郸）派瑞特种气体有限公司 | Processing method of steel cylinder for electronic gas storage |
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