CN111111387A - Method for removing water in hydrogen fluoride steel cylinder - Google Patents
Method for removing water in hydrogen fluoride steel cylinder Download PDFInfo
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- CN111111387A CN111111387A CN201911353376.XA CN201911353376A CN111111387A CN 111111387 A CN111111387 A CN 111111387A CN 201911353376 A CN201911353376 A CN 201911353376A CN 111111387 A CN111111387 A CN 111111387A
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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
- B01D53/26—Drying gases or vapours
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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
- B01D2257/80—Water
Abstract
The invention discloses a method for removing water in a hydrogen fluoride steel cylinder, and belongs to the technical field of hydrogen fluoride gas purification. The method comprises the following steps: (1) setting the temperature of a cylinder body of a hydrogen fluoride steel cylinder at 50-60 ℃, introducing mixed gas of fluorine gas and nitrogen gas from the upper part of the steel cylinder, and removing water in the steel cylinder after the fluorine gas entering the steel cylinder contacts with the water in the steel cylinder to obtain a product 1; (2) the steel cylinder after the reaction is processed by 'vacuumizing-nitrogen pumping-vacuumizing' in turn, and the processed gas is collected to a tail gas recovery device, so that the water removal of the hydrogen fluoride steel cylinder is completed. The invention has the advantages of high efficiency of treating the hydrogen fluoride steel cylinder, thorough water treatment, simple process and no pollution.
Description
Technical Field
The invention belongs to the technical field of hydrogen fluoride gas purification, and relates to a method for removing water in a hydrogen fluoride steel cylinder.
Background
With the continuous development of the integrated circuit industry, the market demands for the purity of electronic gas and the quantity of the electronic gas are increasing, and higher demands are also made on steel cylinders for containing products. A large amount of water remains in the steel cylinder after the use by the customer. The steel bottle inner wall after the customer uses for a long time is coarse, and moisture adsorbs the steel bottle inner wall more easily, increases the steel bottle moisture processing degree of difficulty. Residual water in the steel cylinder not only can seriously affect the product quality, but also can greatly shorten the service life of the steel cylinder. Therefore, the water treatment of the steel cylinder is a very critical link in the production process.
The water removal mode of the steel cylinder commonly used at present is to heat the steel cylinder to raise the temperature, fill nitrogen or other inert gases into the steel cylinder, evacuate the steel cylinder, and repeatedly carry out the 'inflation-evacuation' treatment for many times. The CN108687574A patent of Suzhou gold Macro gas GmbH adopts a heating and evacuating mode to remove water in a steel cylinder; the CN 109838686A of Limited liability company of Riming chemical research and design institute also adopts a heating and vacuumizing mode to remove water in the steel cylinder. The method has low treatment efficiency, long period and poor treatment effect, and is difficult to treat the water content of the steel cylinder to a good level. Especially, after the steel cylinder containing corrosive media is used for a long time, the inner wall of the steel cylinder becomes rough, water is easy to store, and the water treatment difficulty of the steel cylinder is increased.
Disclosure of Invention
The invention aims to provide a method for removing water from a hydrogen fluoride steel cylinder, which has the advantages of high efficiency of treating the hydrogen fluoride steel cylinder, thorough water treatment, simple process and no pollution.
The purpose of the invention is realized by the following technical scheme:
a method for removing water from a hydrogen fluoride steel cylinder comprises the following steps:
(1) setting the temperature of a cylinder body of a hydrogen fluoride steel cylinder at 50-60 ℃, introducing a fluorine gas and nitrogen gas mixture from the upper part of the steel cylinder, allowing the fluorine gas entering the steel cylinder to contact with water in the steel cylinder, and then performing a reaction shown in the formula I, removing the water in the steel cylinder to obtain a product 1:
2F2+2H2O→4HF+O2I
(2) the steel cylinder after the reaction is processed by 'vacuumizing-nitrogen pumping-vacuumizing' in turn, and the processed gas is collected to a tail gas recovery device, so that the water removal of the hydrogen fluoride steel cylinder is completed.
Preferably, the pressure of the mixed gas of fluorine gas and nitrogen gas in the step (1) is 0.2-0.3 MPa, and the volume of the fluorine gas accounts for 20-40% of the total volume of the mixed gas; the reaction time is 5-10 min; the purity of fluorine gas is 99% or more.
Preferably, the initial water content of the hydrogen fluoride cylinder in the step (1) is 1 x 10-6～100×10-6。
Preferably, in the step (1), before the mixed gas of fluorine gas and nitrogen gas is introduced, the hydrogen fluoride steel cylinder is subjected to vacuum pumping pretreatment, and the vacuum degree is less than or equal to 1KPa
Preferably, the vacuum degree of each vacuumizing in the vacuumizing-nitrogen injecting-vacuumizing treatment in the step (2) is less than or equal to 1KPa, and the nitrogen pressure in the steel cylinder after each nitrogen injecting is 0.2-0.3 MPa.
Preferably, the times of the vacuum-pumping-nitrogen-pumping-vacuum treatment in the step (2) are 3 times.
The purity of the nitrogen used in the step (1) and the step (2) is more than 99.999 percent.
The hydrogen fluoride steel cylinder is an old steel cylinder filled with hydrogen fluoride.
The method for removing water from the hydrogen fluoride steel cylinder can be realized by adopting the following devices:
a device for removing water from a hydrogen fluoride steel cylinder comprises: the system comprises a vacuum pipeline, a nitrogen pipeline, a fluorine and nitrogen mixed gas pipeline, an analysis pipeline, a hydrogen fluoride steel cylinder, a public pipeline, a tail gas absorption device and a steel cylinder heating system;
wherein, one end of the public pipeline is connected with the hydrogen fluoride steel cylinder, and the other end is connected with the analysis pipeline; the fluorine gas and nitrogen gas mixed gas pipeline is connected to a common pipeline, the nitrogen gas pipeline is connected to the common pipeline between the hydrogen fluoride steel cylinder and the fluorine gas and nitrogen gas mixed gas pipeline, and the vacuum pipeline is connected to the common pipeline between the hydrogen fluoride steel cylinder and the nitrogen gas pipeline; the tail gas recovery device is connected to the vacuum pipeline; the outer side of the hydrogen fluoride steel cylinder body is provided with a steel cylinder heating system.
Preferably, the pipelines are all stainless steel pipes.
Preferably, the steel cylinder heating system adopts an electric heating bag, and the electric heating bag is wrapped outside the hydrogen fluoride steel cylinder body.
Preferably, the hydrogen fluoride steel cylinder is a cylinder group consisting of more than two steel cylinders.
Advantageous effects
(1) The water removal method for the hydrogen fluoride steel cylinder has the advantages of simple process, small equipment investment and low energy consumption.
(2) The invention has high efficiency of treating the hydrogen fluoride steel cylinder and thorough water treatment, and reduces the water content of the steel cylinder to 0.2 multiplied by 10 within 50min after long-term use by customers-6The steel cylinder treatment qualification index requirements are met below.
(3) The water removal method for the hydrogen fluoride steel cylinder utilizes the characteristic of reaction of fluorine gas and water to remove water in the steel cylinder, reaction products are easy to remove, and the reaction products are discharged to a tail gas recovery device through vacuum pumping, so that the pollution is avoided.
Drawings
FIG. 1 is a schematic view of the apparatus used in the method for removing water from a hydrogen fluoride cylinder according to the present invention.
Wherein, 1-vacuum pipeline, 2-nitrogen pipeline, 3-fluorine gas and nitrogen gas mixed gas pipeline, 4-analysis pipeline, 5-hydrogen fluoride steel cylinder, 6-common pipeline, 7-tail gas recovery device.
Detailed Description
The invention is described in detail below by way of example with reference to the accompanying drawings.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents, materials and equipment are commercially available, unless otherwise specified.
The standard for measuring the water content in the following examples was carried out according to the national Standard GB/T5832.1-2003 "determination of gas humidity part 1 electrolytic method".
The purity of nitrogen gas used in the following examples was 99.999% or more, and the purity of fluorine gas was 99% or more.
The method for removing water from the hydrogen fluoride steel cylinder can be realized by adopting the following devices:
as shown in fig. 1, a device for removing water from a hydrogen fluoride steel cylinder comprises: the device comprises a vacuum pipeline 1, a nitrogen pipeline 2, a fluorine and nitrogen mixed gas pipeline 3, an analysis pipeline 4, a hydrogen fluoride steel bottle 5, a common pipeline 6, a tail gas absorption device 7 and a steel bottle heating system;
wherein, one end of the public pipeline 6 is connected with the hydrogen fluoride steel cylinder 5, and the other end is connected with the analysis pipeline 4; the fluorine and nitrogen mixed gas pipeline 3 is connected with a common pipeline 6, the nitrogen pipeline 2 is connected with the common pipeline 6 between the hydrogen fluoride steel cylinder 5 and the fluorine and nitrogen mixed gas pipeline 3, and the vacuum pipeline 1 is connected with the common pipeline 6 between the hydrogen fluoride steel cylinder 5 and the nitrogen pipeline 2; the tail gas recovery device 7 is connected to the vacuum pipeline 1; and a steel cylinder heating system is arranged on the outer side of the 5-body of the hydrogen fluoride steel cylinder.
The pipelines are all stainless steel pipes.
The steel cylinder heating system adopts an electric heating bag, and the electric heating bag is wrapped outside the 5 bottle bodies of the hydrogen fluoride steel cylinders.
The hydrogen fluoride steel cylinder 5 is a cylinder group consisting of two steel cylinders.
Example 1
A water removal method for a hydrogen fluoride steel cylinder comprises the following specific steps:
firstly, a heating bag is wrapped on a hydrogen fluoride steel cylinder 5, and the water content of the hydrogen fluoride steel cylinder 5 is 100 multiplied by 10-6After the temperature of the cylinder body of the steel cylinder rises to 50 ℃, the hydrogen fluoride steel cylinder 5 is vacuumized and pretreated by a vacuum pipeline 1, and then fluorine gas and nitrogen gas are introduced from the valve port of the steel cylinder by a fluorine gas and nitrogen gas mixed pipeline 3And (2) nitrogen mixed gas, wherein the volume of the fluorine gas accounts for 20% of the total volume of the mixed gas, the pressure of the mixed gas of the fluorine gas and the nitrogen gas is 0.2MPa, the reaction time is 5min, the fluorine gas and the water are contacted and then react as shown in the formula I, the water in the steel cylinder is removed, and a product 1:
2F2+2H2O→4HF+O2I
evacuating the reacted product from the valve port of the steel cylinder by a vacuum pipeline 1, wherein the vacuum degree is 1Kpa, introducing nitrogen from the valve port of a hydrogen fluoride steel cylinder 5 by a nitrogen pipeline 2, the pressure of the nitrogen is 0.2MPa, and evacuating again after the pressure is stable, wherein the vacuum degree is 1 Kpa. The operations of vacuumizing, nitrogen gas injection and vacuumizing are repeated for 3 times.
The vacuumized tail gas is recycled to the tail gas recycling device 7, and pollution is avoided.
The operation steps take 38min in total.
After the treatment, the water content in the hydrogen fluoride steel cylinder 5 is detected to be 0.12 multiplied by 10-6Meet the qualification index of steel cylinder treatment of 0.75 multiplied by 10-6The requirements of (1).
Example 2
A water removal method for a hydrogen fluoride steel cylinder comprises the following specific steps:
firstly, the hydrogen fluoride steel cylinder 5 is wrapped with a heating bag, and the water content of the hydrogen fluoride steel cylinder 5 is 80 multiplied by 10-6After the temperature of the cylinder body of the steel cylinder rises to 55 ℃, a vacuum pipeline 1 is used for vacuumizing a hydrogen fluoride steel cylinder 5 for pretreatment, then a fluorine and nitrogen mixed gas is introduced from a valve port of the steel cylinder through a fluorine and nitrogen mixed gas pipeline 3, wherein the volume of the fluorine gas accounts for 20% of the total volume of the mixed gas, the pressure of the fluorine and nitrogen mixed gas is 0.2MPa, the reaction time is 7min, the fluorine gas contacts with water to perform a reaction shown in formula I, and the water in the steel cylinder is removed to obtain a product 1:
2F2+2H2O→4HF+O2I
evacuating the reacted product from the valve port of the steel cylinder by a vacuum pipeline 1, wherein the vacuum degree is 1Kpa, introducing nitrogen from the valve port of a hydrogen fluoride steel cylinder 5 by a nitrogen pipeline 2, the pressure of the nitrogen is 0.2MPa, and evacuating again after the pressure is stable, wherein the vacuum degree is 1 Kpa. The operations of vacuumizing, nitrogen gas injection and vacuumizing are repeated for 3 times.
The vacuum pumping tail gas is recycled to the tail gas recycling device, and pollution is avoided.
The operation steps take 40min in total.
After the treatment, the water content in the hydrogen fluoride steel cylinder 5 is detected to be 0.09 multiplied by 10-6Meet the qualification index of steel cylinder treatment of 0.75 multiplied by 10-6The requirements of (1).
Example 3
A water removal method for a hydrogen fluoride steel cylinder comprises the following specific steps:
firstly, a heating bag is wrapped on a hydrogen fluoride steel cylinder 5, and the water content of the hydrogen fluoride steel cylinder 5 is 100 multiplied by 10-6After the temperature of the cylinder body of the steel cylinder rises to 50 ℃, the hydrogen fluoride steel cylinder 5 is subjected to vacuumizing pretreatment through a vacuum pipeline 1, then mixed gas of fluorine gas and nitrogen gas is introduced from a valve port of the steel cylinder through a mixed gas pipeline 3 of fluorine gas and nitrogen gas, wherein the volume of the fluorine gas accounts for 30% of the total volume of the mixed gas, the pressure of the mixed gas of fluorine gas and nitrogen gas is 0.25MPa, the reaction time is 5min, the fluorine gas and water are contacted to generate a reaction shown in formula I, and the water in the steel cylinder is removed to obtain a product 1:
2F2+2H2O→4HF+O2I
evacuating the reacted product from the valve port of the steel cylinder by a vacuum pipeline 1, wherein the vacuum degree is 1Kpa, introducing nitrogen from the valve port of a hydrogen fluoride steel cylinder 5 by a nitrogen pipeline 2, the pressure of the nitrogen is 0.2MPa, and evacuating again after the pressure is stable, wherein the vacuum degree is 1 Kpa. The operations of vacuumizing, nitrogen gas injection and vacuumizing are repeated for 3 times.
The vacuumized tail gas is recycled to the tail gas recycling device 7, and pollution is avoided.
The operation steps take 38min in total.
After the treatment, the water content in the hydrogen fluoride steel cylinder 5 is detected to be 0.11 multiplied by 10-6Meet the qualification index of steel cylinder treatment of 0.75 multiplied by 10-6The requirements of (1).
Example 4
A water removal method for a hydrogen fluoride steel cylinder comprises the following specific steps:
firstly, a hydrogen fluoride steel cylinder 5 is wrapped with a heating bag, and the water content of the hydrogen fluoride steel cylinder 5 is 1 multiplied by 10-6After the temperature of the cylinder body of the steel cylinder rises to 60 ℃, a vacuum pipeline 1 is used for vacuumizing a hydrogen fluoride steel cylinder 5 for pretreatment, then a fluorine and nitrogen mixed gas is introduced from a valve port of the steel cylinder through a fluorine and nitrogen mixed gas pipeline 3, wherein the volume of the fluorine gas accounts for 40% of the total volume of the mixed gas, the pressure of the fluorine and nitrogen mixed gas is 0.3MPa, the reaction time is 10min, the fluorine gas contacts with water to perform a reaction shown in formula I, and the water in the steel cylinder is removed to obtain a product 1:
2F2+2H2O→4HF+O2I
evacuating the reacted product from the valve port of the steel cylinder by using a vacuum pipeline 1, wherein the vacuum degree is 1KPa, introducing nitrogen from the 5 ports of the hydrogen fluoride steel cylinder valve by using a nitrogen pipeline 2, the nitrogen pressure is 0.3MPa, and vacuumizing again after the pressure is stable, wherein the vacuum degree is 1 KPa. The operations of vacuumizing, nitrogen gas injection and vacuumizing are repeated for 3 times.
The vacuumized tail gas is recycled to the tail gas recycling device 7, and pollution is avoided.
The operation steps take 43min in total.
After the treatment, the water content in the hydrogen fluoride steel cylinder 5 is detected to be 0.05 multiplied by 10-6Meet the qualification index of steel cylinder treatment of 0.75 multiplied by 10-6The requirements of (1).
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for removing water from a hydrogen fluoride steel cylinder is characterized by comprising the following steps:
(1) setting the temperature of a cylinder body of a hydrogen fluoride steel cylinder at 50-60 ℃, introducing a fluorine gas and nitrogen gas mixture from the upper part of the steel cylinder, allowing the fluorine gas entering the steel cylinder to contact with water in the steel cylinder, and then performing a reaction shown in the formula I, removing the water in the steel cylinder to obtain a product 1:
2F2+2H2O→4HF+O2I
(2) the steel cylinder after the reaction is processed by 'vacuumizing-nitrogen pumping-vacuumizing' in turn, and the processed gas is collected to a tail gas recovery device, so that the water removal of the hydrogen fluoride steel cylinder is completed.
2. The method for removing water in the hydrogen fluoride steel cylinder according to claim 1, wherein the pressure of the mixed gas of fluorine gas and nitrogen gas in the step (1) is 0.2 to 0.3MPa, and the volume of the fluorine gas accounts for 20 to 40 percent of the total volume of the mixed gas; the reaction time is 5-10 min.
3. The method for removing water from a hydrogen fluoride cylinder as claimed in claim 1, wherein the initial water content of the hydrogen fluoride cylinder in the step (1) is 1 x 10-6～100×10-6。
4. The method for removing water in the hydrogen fluoride steel cylinder according to claim 1, wherein in the step (1), before the mixed gas of fluorine gas and nitrogen gas is introduced, the hydrogen fluoride steel cylinder is subjected to vacuum-pumping pretreatment, and the vacuum degree is less than or equal to 1 KPa.
5. The method for removing water in the hydrogen fluoride steel cylinder according to claim 1, wherein the degree of vacuum in each vacuum pumping in the vacuum pumping-nitrogen pumping-vacuum pumping treatment in the step (2) is less than or equal to 1KPa, and the pressure of nitrogen in the steel cylinder after each nitrogen pumping is 0.2-0.3 MPa.
6. The method for removing water from a steel cylinder of hydrogen fluoride as claimed in claim 1, wherein the number of times of the "vacuuming-nitrogen-vacuuming" treatment in the step (2) is 3.
7. The method for removing water in the hydrogen fluoride steel cylinder as claimed in claim 1, which is implemented by adopting the following devices:
the device comprises: the device comprises a vacuum pipeline (1), a nitrogen pipeline (2), a fluorine and nitrogen mixed gas pipeline (3), an analysis pipeline (4), a hydrogen fluoride steel cylinder (5), a public pipeline (6), a tail gas absorption device (7) and a steel cylinder heating system;
wherein, one end of the public pipeline (6) is connected with the hydrogen fluoride steel cylinder (5), and the other end is connected with the analysis pipeline (4); the fluorine and nitrogen mixed gas pipeline (3) is connected to a common pipeline (6), the nitrogen pipeline (2) is connected to the common pipeline (6) between the hydrogen fluoride steel cylinder (5) and the fluorine and nitrogen mixed gas pipeline (3), and the vacuum pipeline (1) is connected to the common pipeline (6) between the hydrogen fluoride steel cylinder (5) and the nitrogen pipeline (2); the tail gas recovery device (7) is connected to the vacuum pipeline (1); the outer side of the body of the hydrogen fluoride steel cylinder (5) is provided with a steel cylinder heating system.
8. The method of claim 7, wherein the lines are stainless steel.
9. The method for removing water in the hydrogen fluoride steel cylinder is characterized in that the steel cylinder heating system adopts an electric heating bag, and the electric heating bag is wrapped outside the cylinder body of the hydrogen fluoride steel cylinder (5).
10. The method for removing water in a hydrogen fluoride cylinder according to claim 7, wherein the hydrogen fluoride cylinder (5) is a cylinder group consisting of two or more cylinders.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112337271A (en) * | 2020-09-30 | 2021-02-09 | 中船重工（邯郸）派瑞特种气体有限公司 | Water removal method and device for hydrogen chloride steel cylinder |
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| CN112337271A (en) * | 2020-09-30 | 2021-02-09 | 中船重工（邯郸）派瑞特种气体有限公司 | Water removal method and device for hydrogen chloride steel cylinder |
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