CN110899248A - System and method for cleaning ultrahigh-purity gas steel cylinders in batch by using supercritical fluid - Google Patents
System and method for cleaning ultrahigh-purity gas steel cylinders in batch by using supercritical fluid Download PDFInfo
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- CN110899248A CN110899248A CN201910539750.9A CN201910539750A CN110899248A CN 110899248 A CN110899248 A CN 110899248A CN 201910539750 A CN201910539750 A CN 201910539750A CN 110899248 A CN110899248 A CN 110899248A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 201
- 239000010959 steel Substances 0.000 title claims abstract description 201
- 238000004140 cleaning Methods 0.000 title claims abstract description 37
- 239000012530 fluid Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 726
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 366
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 366
- 239000012535 impurity Substances 0.000 claims abstract description 61
- 239000013589 supplement Substances 0.000 claims abstract description 17
- 239000000498 cooling water Substances 0.000 claims description 40
- 239000002994 raw material Substances 0.000 claims description 29
- 230000001502 supplementing effect Effects 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 7
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000004806 packaging method and process Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0021—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/0804—Cleaning containers having tubular shape, e.g. casks, barrels, drums
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- Cleaning In General (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
The invention discloses a system for cleaning ultra-high purity gas steel cylinders in batches by using supercritical fluid, which comprises a supercritical carbon dioxide supplement pipeline, a high purity gas steel cylinder cleaning pipeline and an organic impurity analysis discharge pipeline which are sequentially communicated, wherein the supercritical carbon dioxide is provided by the carbon dioxide supplement pipeline and enters the high purity gas steel cylinder cleaning pipeline to realize batch cleaning of the gas steel cylinders, the carbon dioxide discharged from the high purity gas steel cylinder cleaning pipeline enters the organic impurity analysis discharge pipeline, organic impurities dissolved in the carbon dioxide are separated out through the organic impurity analysis discharge pipeline and are periodically discharged, the normal temperature and normal pressure carbon dioxide of the organic impurity analysis discharge pipeline is connected to the carbon dioxide supplement pipeline again to carry out circulation, the invention can rapidly remove the organic impurities attached to the inner wall surface of the steel cylinders, and has the characteristics of short treatment time, large quantity of steel cylinders treated at one time and low energy consumption, the technical characteristics of potential damage to the high-purity gas cylinder caused by conventional high-temperature baking and the like can be avoided.
Description
Technical Field
The present invention relates to a system and method for cleaning ultra-high purity gas cylinders, and more particularly, to a system and method for cleaning ultra-high purity gas cylinders in batch using supercritical fluid.
Background
At present, in the fields of ppm standard gas, high-purity electronic special gas and the like, the recovery treatment of the steel cylinder of the container is generally carried out by adopting a steel cylinder baking box and vacuumizing mode, the method needs to heat the steel cylinder to 200-250 ℃ and continuously vacuumize, then gasified organic impurities are pumped out to the atmosphere, in order to meet the filling requirement of the high-purity gas steel cylinder, the steel cylinder needs to be repeatedly heated and vacuumized for 3-5 times, and the method has the following defects: the treatment time is long, the single treatment of the steel cylinder is less, the energy consumption is high, organic impurities attached to the inner wall surface of the steel cylinder cannot be removed quickly, the treatment efficiency of the steel cylinder is poor, the equipment investment is high, and the practical requirement of treating the high-purity gas steel cylinder on an industrial scale cannot be met.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a system for cleaning ultrahigh-purity gas steel cylinders in batches by using supercritical fluid, which has the technical characteristics of high safety operability, low energy consumption, low investment, high steel cylinder treatment efficiency, capability of treating a large number of high-purity gas steel cylinders at one time and the like.
It is another object of the present invention to provide a method for batch cleaning ultra-high purity gas cylinders using supercritical fluids.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a system for cleaning ultra-high purity gas steel cylinders in batches by using supercritical fluid comprises a supercritical carbon dioxide supplement pipeline, a high purity gas steel cylinder cleaning pipeline and an organic impurity analysis discharge pipeline which are sequentially communicated;
the supercritical carbon dioxide supply pipeline is communicated with a carbon dioxide supply steel cylinder, the supercritical carbon dioxide supply pipeline is sequentially connected with a carbon dioxide supply stop valve, a carbon dioxide circulating compressor, a cooling water heat exchanger and a measurer, the high-purity gas steel cylinder cleaning pipeline comprises a first branch and a second branch, the tail ends of the first branch and the second branch are converged and communicated to form a third branch, the first branch is sequentially connected with a raw material gas steel cylinder and a supercritical carbon dioxide raw material gas steel cylinder stop valve, the second branch is connected with a supercritical carbon dioxide filling steel cylinder stop valve, the third branch is connected with a supercritical carbon dioxide filling steel cylinder check valve, the outlet of the supercritical carbon dioxide filling steel cylinder check valve extends and is respectively provided with a fourth branch and a fifth branch, and the fourth branch is connected with a supercritical carbon dioxide stop valve, the fifth branch is sequentially connected with a charging steel cylinder and a supercritical carbon dioxide discharging and charging steel cylinder stop valve, the tail ends of the fourth branch and the fifth branch are converged to form a sixth branch, and the sixth branch is communicated with an organic impurity analysis and discharge pipeline;
as an improvement, the analytic discharge line of organic impurity includes that the preface in proper order connects at the analytic discharge line's of organic impurity supercritical carbon dioxide buffer tank, supercritical carbon dioxide throttle valve, organic impurity collecting tank is connected with mutual independent normal atmospheric temperature and pressure carbon dioxide stop valve, organic impurity and excretes the stop valve, normal atmospheric temperature and pressure carbon dioxide stop valve export extends to be connected between carbon dioxide supplementary stop valve, carbon dioxide circulating compressor.
As a modification, the measurer comprises a supercritical carbon dioxide thermometer, a supercritical carbon dioxide pressure gauge and a supercritical carbon dioxide flow meter which are arranged in sequence; the raw material gas steel cylinder and the filling steel cylinder are provided with a plurality of steel cylinders.
As an improvement, the outlet end of the supercritical carbon dioxide supplementing pipeline and the inlet end of the supercritical carbon dioxide buffer tank are communicated with supercritical carbon dioxide safety valves.
As an improvement, the cooling water heat exchanger is communicated with a cold source, the cold source is an industrial cooling water tank, and the cooling water heat exchanger is provided with an industrial cooling water outlet.
As an improvement, the first branch and the second branch are connected with a seventh branch in a gathering mode, a system vacuumizing stop valve, a vacuum resistance gauge and a vacuumizing rotary vane pump are sequentially connected onto the seventh branch, and the vacuumizing rotary vane pump is communicated with the outside.
As an improvement, the device also comprises a raw material gas steel cylinder packaging grid, wherein the raw material gas steel cylinder is placed in the raw material gas steel cylinder packaging grid.
As an improvement, the filling and distributing ring is provided with a channel, the filling and distributing ring is communicated with the fifth branch, and the filling steel cylinders are communicated with the filling and distributing ring at equal intervals.
As a modification, the organic impurity collecting tank is arranged close to the supercritical carbon dioxide throttling and adjusting valve; the supercritical carbon dioxide discharging and filling steel cylinder stop valve is arranged close to the filling distribution ring.
The invention discloses a method for cleaning ultrahigh pure gas steel cylinders in batch by using supercritical fluid, which comprises the following steps:
1) carbon dioxide in the carbon dioxide supplementing steel cylinder enters a carbon dioxide circulating compressor through a carbon dioxide supplementing stop valve and is compressed to the critical pressure of 7.4MPaA, when high-pressure carbon dioxide gas discharged from the carbon dioxide circulating compressor passes through a cooling water heat exchanger, the high-pressure carbon dioxide gas exchanges heat with industrial cooling water in the cooling water heat exchanger, the high-pressure carbon dioxide gas is cooled to the critical temperature of 31 ℃, and supercritical carbon dioxide discharged from the cooling water heat exchanger is sequentially monitored by a supercritical carbon dioxide thermometer and a supercritical carbon dioxide pressure gauge and then metered by a supercritical carbon dioxide flowmeter;
2) the supercritical carbon dioxide after the metering is divided into a first branch and a second branch for conveying: supercritical carbon dioxide in the first branch directly enters a feed gas steel cylinder, and then supercritical carbon dioxide is controlled by a stop valve 12 of the supercritical carbon dioxide feed gas steel cylinder to fill the steel cylinder; the supercritical carbon dioxide in the second branch firstly passes through the supercritical carbon dioxide to fill a steel cylinder stop valve and then fills a steel cylinder; if the feed gas steel cylinder is cleaned, the supercritical carbon dioxide is closed to fill the steel cylinder stop valve, the supercritical carbon dioxide enters the feed gas steel cylinder, the supercritical carbon dioxide is controlled by the supercritical carbon dioxide feed gas steel cylinder stop valve when exiting the feed gas steel cylinder, and the supercritical carbon dioxide flows to the third branch when passing through the passage; if the raw material gas steel cylinder does not need to be cleaned, the supercritical carbon dioxide directly passes through a stop valve of the supercritical carbon dioxide filling steel cylinder and flows to the third branch; the first branch and the second branch are connected with a seventh branch in a gathering manner, the seventh branch is sequentially connected with a system vacuumizing stop valve, a vacuum resistance gauge and a vacuumizing rotary vane pump, the vacuumizing rotary vane pump is communicated with the outside, and the vacuumizing rotary vane pump is started to realize vacuumizing;
3) the supercritical carbon dioxide in the third branch is divided into a fourth branch and a fifth branch for conveying: the supercritical carbon dioxide in the third branch is firstly filled into a steel cylinder check valve through the supercritical carbon dioxide, and then enters a supercritical carbon dioxide buffer tank through a supercritical carbon dioxide stop valve on the fourth branch; supercritical carbon dioxide in the third branch firstly passes through a supercritical carbon dioxide filling steel cylinder check valve, then enters a supercritical carbon dioxide filling steel cylinder in the fifth branch, and then passes through a supercritical carbon dioxide filling steel cylinder stop valve to enter a sixth branch and a supercritical carbon dioxide buffer tank; if the supercritical carbon dioxide needs to be cleaned to fill the steel cylinder, closing the supercritical carbon dioxide stop valve, and allowing the supercritical carbon dioxide to enter the filling steel cylinder through the filling distribution ring; if the supercritical carbon dioxide is not required to be cleaned to fill the steel cylinder, the supercritical carbon dioxide directly enters the sixth branch and the supercritical carbon dioxide buffer tank from the supercritical carbon dioxide stop valve, and a supercritical carbon dioxide safety valve is arranged at the inlet of the supercritical carbon dioxide buffer tank to prevent the overpressure of a system pipeline;
4) the supercritical carbon dioxide which is discharged from the supercritical carbon dioxide buffer tank is throttled and depressurized by the supercritical carbon dioxide throttling regulating valve to become normal-temperature normal-pressure carbon dioxide, organic impurities dissolved in the carbon dioxide are separated out, accumulated at the bottom of the organic impurity collecting tank and periodically discharged through the organic impurity discharge stop valve, the outlet of the normal-temperature normal-pressure carbon dioxide stop valve is extended and connected between the carbon dioxide supplement stop valve and the carbon dioxide circulating compressor, the normal-temperature normal-pressure carbon dioxide after the impurities are analyzed is converged with the carbon dioxide in the carbon dioxide supplement steel cylinder, and then the carbon dioxide sequentially enters each branch to enter circulation.
Has the advantages that: the supercritical carbon dioxide fluid is used as a cleaning medium of the high-purity gas steel cylinder, organic impurities attached to the inner wall surface of the steel cylinder can be quickly removed, and the method has the characteristics of short treatment time, large steel cylinder treatment amount at one time and low energy consumption, and can be used as an ideal mode for industrial treatment of the high-purity gas steel cylinder; the cleaning effect of the inner wall surface of the high-purity gas steel cylinder can be achieved, the cleaning agent has the characteristic of strong grease dissolving capacity, organic impurities attached to the inner wall surface of the high-purity gas steel cylinder can be removed efficiently, and compared with conventional heating vacuumizing steel cylinder treatment equipment, the cleaning agent has the characteristics of high steel cylinder treatment efficiency, low equipment investment and capability of treating the high-purity gas steel cylinder in a large batch, and can meet the practical requirement of treating the high-purity gas steel cylinder in an industrial scale; by utilizing the characteristic that the critical temperature of carbon dioxide is 31 ℃ in a normal temperature range, organic impurities attached to the inner wall surface of the high-purity gas steel cylinder can be efficiently removed at normal temperature, and compared with the conventional method that the treatment temperature of the steel cylinder is treated by utilizing a baking oven and a vacuumizing mode, the energy consumption of a system is reduced; can process a large amount of recovered steel cylinders at one time, and has higher treatment efficiency to the steel cylinders because the supercritical carbon dioxide has stronger organic matter dissolving capacity. Because the steel cylinder is cleaned at normal temperature, the potential damage of the conventional high-temperature baking to the high-purity gas cylinder is avoided.
Drawings
Fig. 1 is a schematic structural diagram of the principle of the invention.
In the figure: 1-a supercritical carbon dioxide make-up line; 2-cleaning the pipeline of the high-purity gas cylinder; 3-organic impurity analysis discharge pipeline; 4-carbon dioxide replenishing cylinder; 5-carbon dioxide supplement stop valve; 6-carbon dioxide recycle compressor; 7-cooling water heat exchanger; 8-a first branch; 9-a second branch; 10-a third branch; 11-raw gas cylinder; 12-supercritical carbon dioxide raw gas cylinder stop valve; 13-filling a steel cylinder stop valve with supercritical carbon dioxide; 14-filling a check valve of a steel cylinder by supercritical carbon dioxide; 15-a fourth branch; 16-the fifth branch; 17-supercritical carbon dioxide stop valve; 18-filling a steel cylinder; 19-a stop valve for filling the steel cylinder with supercritical carbon dioxide; 20-a sixth branch; 21-filling a distribution ring; 22-supercritical carbon dioxide buffer tank; 23-a supercritical carbon dioxide throttling and regulating valve; 24-an organic impurity collection tank; 25-normal temperature and pressure carbon dioxide stop valve; 26-organic impurity discharge stop valve; 27-supercritical carbon dioxide thermometer; 28-supercritical carbon dioxide manometer; 29-supercritical carbon dioxide flow meter; 30-supercritical carbon dioxide relief valve; 31-industrial cooling water tank; 32-industrial cooling water outlet; 33-a seventh branch; 34-a system vacuumizing stop valve; 35-vacuum resistance gauge; 36-vacuum-pumping rotary vane pump.
Detailed Description
The present invention will be further described with reference to the drawings attached to the specification, but the present invention is not limited to the following examples.
As shown in fig. 1, the system for batch cleaning ultra-high purity gas cylinders by using supercritical fluid according to the embodiment includes a supercritical carbon dioxide supply line 1, a high purity gas cylinder cleaning line 2, and an organic impurity desorption/discharge line 3, which are connected in sequence;
an inlet of the supercritical carbon dioxide supplementing pipeline 1 is communicated with a carbon dioxide supplementing steel cylinder 4, the supercritical carbon dioxide supplementing pipeline 1 is sequentially connected with a carbon dioxide supplementing stop valve 5, a carbon dioxide circulating compressor 6, a cooling water heat exchanger 7 and a measurer, the high-purity gas steel cylinder cleaning pipeline 2 comprises a first branch 8 and a second branch 9, the tail ends of the first branch 8 and the second branch 9 are converged and communicated to form a third branch 10, the first branch 8 is sequentially connected with a raw material gas steel cylinder 11 and a supercritical carbon dioxide raw material gas steel cylinder stop valve 12, the second branch 9 is connected with a supercritical carbon dioxide charging steel cylinder stop valve 13, the third branch 10 is connected with a supercritical carbon dioxide charging steel cylinder check valve 14, an outlet of the supercritical carbon dioxide charging steel cylinder check valve 14 extends and is respectively provided with a fourth branch 15 and a fifth branch 16, a supercritical carbon dioxide stop valve 17 is connected to the fourth branch 15, a charging steel cylinder 18 and a supercritical carbon dioxide discharging and charging steel cylinder stop valve 19 are sequentially connected to the fifth branch 16, a sixth branch 20 is formed by converging the tail ends of the fourth branch 15 and the fifth branch 16, and the sixth branch 20 is communicated with the organic impurity analysis and discharge pipeline 3;
the process of cleaning ultrahigh-purity gas steel cylinders in batches comprises the following steps:
1) carbon dioxide in the carbon dioxide supplementing steel cylinder 4 enters a carbon dioxide circulating compressor 6 through a carbon dioxide supplementing stop valve 5 and is compressed to the critical pressure of 7.4MPaA, when high-pressure carbon dioxide gas from the carbon dioxide circulating compressor 6 passes through a cooling water heat exchanger 7, the high-pressure carbon dioxide gas exchanges heat with industrial cooling water in the cooling water heat exchanger 7, the high-pressure carbon dioxide gas is cooled to the critical temperature of 31 ℃, and supercritical carbon dioxide from the cooling water heat exchanger 7 is measured by a measurer;
2) the supercritical carbon dioxide measured by the measurer is divided into a first branch 8 and a second branch 9 for conveying: the supercritical carbon dioxide in the first branch 8 directly enters a raw material gas steel cylinder 11, and then the supercritical carbon dioxide is controlled by a stop valve 12 of the supercritical carbon dioxide raw material gas steel cylinder to fill a steel cylinder 18; the supercritical carbon dioxide in the second branch 9 firstly passes through the supercritical carbon dioxide to fill the steel cylinder stop valve 13 and then fills the steel cylinder 18; if the feed gas steel cylinder 11 is cleaned, the supercritical carbon dioxide is firstly closed to fill the steel cylinder stop valve 13, the supercritical carbon dioxide enters the feed gas steel cylinder 11, the supercritical carbon dioxide is controlled by the supercritical carbon dioxide feed gas steel cylinder stop valve 12 when exiting the feed gas steel cylinder 11, and the supercritical carbon dioxide flows to the third branch 10 when being communicated; if the raw gas steel cylinder 11 does not need to be cleaned, the supercritical carbon dioxide directly passes through the supercritical carbon dioxide filling steel cylinder stop valve 13 and flows to the third branch 10;
3) the supercritical carbon dioxide in the third branch 10 is divided into a fourth branch 15 and a fifth branch 16 for conveying: the supercritical carbon dioxide in the third branch 10 firstly passes through the supercritical carbon dioxide to fill the steel cylinder check valve 14, and then enters the sixth branch 20 and the organic impurity analysis discharge pipeline 3 through the supercritical carbon dioxide stop valve 17 on the fourth branch 15, so that the organic impurities dissolved in the carbon dioxide are separated out; supercritical carbon dioxide in the third branch 10 firstly passes through the supercritical carbon dioxide to fill a steel cylinder check valve 14, then enters the fifth branch 16, firstly passes through the supercritical carbon dioxide to fill a steel cylinder 18, then passes through a supercritical carbon dioxide discharging and filling steel cylinder stop valve 19, enters the sixth branch 20 and the organic impurity analysis and discharge pipeline 3, and separation of organic impurities dissolved in the carbon dioxide is realized; if the supercritical carbon dioxide needs to be cleaned to fill the steel cylinder 18, the supercritical carbon dioxide stop valve 17 is closed, and the supercritical carbon dioxide enters the filling steel cylinder 18 through the filling distribution ring 21; if the supercritical carbon dioxide is not needed to be cleaned to fill the steel cylinder 18, the supercritical carbon dioxide directly enters the sixth branch 20 and the organic impurity analysis discharge pipeline 3 from the supercritical carbon dioxide stop valve 17, so that the organic impurities dissolved in the carbon dioxide are separated out.
As an improved embodiment, as shown in fig. 1, the organic impurity analysis discharge pipeline 3 includes a supercritical carbon dioxide buffer tank 22, a supercritical carbon dioxide throttle valve 23, and an organic impurity collection tank 24 sequentially connected to the organic impurity analysis discharge pipeline 3, the organic impurity collection tank 24 is connected to an independent normal-temperature normal-pressure carbon dioxide stop valve 25 and an independent organic impurity discharge stop valve 26, and an outlet of the normal-temperature normal-pressure carbon dioxide stop valve 25 is connected between the carbon dioxide supplement stop valve 5 and the carbon dioxide recycle compressor 6 in an extending manner;
the process of cleaning ultrahigh-purity gas steel cylinders in batches comprises the following steps:
1) carbon dioxide in the carbon dioxide supplementing steel cylinder 4 enters a carbon dioxide circulating compressor 6 through a carbon dioxide supplementing stop valve 5 and is compressed to the critical pressure of 7.4MPaA, when high-pressure carbon dioxide gas from the carbon dioxide circulating compressor 6 passes through a cooling water heat exchanger 7, the high-pressure carbon dioxide gas exchanges heat with industrial cooling water in the cooling water heat exchanger 7, the high-pressure carbon dioxide gas is cooled to the critical temperature of 31 ℃, and supercritical carbon dioxide from the cooling water heat exchanger 7 is measured by a measurer;
2) after being measured by the measurer, the supercritical carbon dioxide is divided into a first branch 8 and a second branch 9 for conveying: the supercritical carbon dioxide in the first branch 8 directly enters a raw material gas steel cylinder 11, and then the supercritical carbon dioxide is controlled by a stop valve 12 of the supercritical carbon dioxide raw material gas steel cylinder to fill a steel cylinder 18; the supercritical carbon dioxide in the second branch 9 firstly passes through the supercritical carbon dioxide to fill the steel cylinder stop valve 13 and then fills the steel cylinder 18; if the feed gas steel cylinder 11 is cleaned, the supercritical carbon dioxide is firstly closed to fill the steel cylinder stop valve 13, the supercritical carbon dioxide enters the feed gas steel cylinder 11, the supercritical carbon dioxide is controlled by the supercritical carbon dioxide feed gas steel cylinder stop valve 12 when exiting the feed gas steel cylinder 11, and the supercritical carbon dioxide flows to the third branch 10 when being communicated; if the raw gas steel cylinder 11 does not need to be cleaned, the supercritical carbon dioxide directly passes through the supercritical carbon dioxide filling steel cylinder stop valve 13 and flows to the third branch 10; the first branch 8 and the second branch 9 are connected with a seventh branch 33 in a gathering manner, the seventh branch 33 is sequentially connected with a system vacuumizing stop valve 34, a vacuum resistance gauge 35 and a vacuumizing rotary vane pump 36, the vacuumizing rotary vane pump 37 is communicated with the outside, and the vacuumizing rotary vane pump 36 is started to realize vacuumizing;
3) the supercritical carbon dioxide in the third branch 10 is divided into a fourth branch 15 and a fifth branch 16 for conveying: the supercritical carbon dioxide in the third branch 10 firstly passes through the supercritical carbon dioxide to fill the steel cylinder check valve 14, and then enters the supercritical carbon dioxide buffer tank 22 through the supercritical carbon dioxide stop valve 17 on the fourth branch 15; supercritical carbon dioxide in the third branch 10 firstly passes through a supercritical carbon dioxide filling steel cylinder check valve 14, then enters a supercritical carbon dioxide filling steel cylinder 18 in the fifth branch 16, and then passes through a supercritical carbon dioxide discharging and filling steel cylinder stop valve 19 and enters a sixth branch 20 and a supercritical carbon dioxide buffer tank 22; if the supercritical carbon dioxide needs to be cleaned to fill the steel cylinder 18, the supercritical carbon dioxide stop valve 17 is closed, and the supercritical carbon dioxide enters the filling steel cylinder 18 through the filling distribution ring 21; if the supercritical carbon dioxide is not required to be cleaned to fill the steel cylinder 18, the supercritical carbon dioxide directly enters the sixth branch 20 and the supercritical carbon dioxide buffer tank 22 from the supercritical carbon dioxide stop valve 17, and a supercritical carbon dioxide safety valve 30 is arranged at an inlet of the supercritical carbon dioxide buffer tank 22 to prevent overpressure of a system pipeline; a supercritical carbon dioxide safety valve 30 is arranged at the inlet of the supercritical carbon dioxide buffer tank 22 to prevent the overpressure of the system pipeline;
4) the supercritical carbon dioxide which is discharged from the supercritical carbon dioxide buffer tank 22 is throttled and depressurized by the supercritical carbon dioxide throttle valve 23 to become normal-temperature normal-pressure carbon dioxide, organic impurities dissolved in the carbon dioxide are separated out and accumulated at the bottom of the organic impurity collecting tank 24, and is periodically discharged by the organic impurity discharge stop valve 26, the outlet of the normal-temperature normal-pressure carbon dioxide stop valve 25 is extended and connected between the carbon dioxide supplement stop valve 5 and the carbon dioxide circulating compressor 6, the normal-temperature normal-pressure carbon dioxide after the impurities are analyzed and the carbon dioxide in the carbon dioxide supplement steel cylinder 4 are converged, and then the carbon dioxide sequentially enters each branch to enter circulation.
As a modified example, the measurer comprises a supercritical carbon dioxide thermometer 27, a supercritical carbon dioxide pressure gauge 28 and a supercritical carbon dioxide flow meter 29 which are arranged in sequence, and the feed gas cylinder 11 and the charging cylinder 18 are respectively provided with a plurality of.
As an improved embodiment, the outlet end of the supercritical carbon dioxide supplementing pipeline 1 and the inlet end of the supercritical carbon dioxide buffer tank 22 are both communicated with a supercritical carbon dioxide safety valve 30, so that the rapid fluctuation of the system pressure caused by the flash evaporation of the supercritical carbon dioxide is prevented, and the system operation safety is protected.
As an improved embodiment, the cooling water heat exchanger 7 is communicated with a cold source, the cold source is an industrial cooling water tank 31, the cooling water heat exchanger 7 is provided with an industrial cooling water outlet 32, and an annular pipeline can be communicated between the industrial cooling water tank 31 and the industrial cooling water outlet 32 to realize recycling.
As an improved embodiment, the first branch 8 and the second branch 9 are connected to a seventh branch 33 in a converging manner, the seventh branch 33 is sequentially connected to a system vacuumizing stop valve 34, a vacuum resistance gauge 35 and a vacuumizing rotary vane pump 36, the vacuumizing rotary vane pump 36 is communicated with the outside, and the vacuumizing rotary vane pump 36 is started to realize vacuumizing.
As an improved embodiment, the device also comprises a raw material gas steel cylinder packaging grid, wherein the raw material gas steel cylinders 11 are arranged in the raw material gas steel cylinder packaging grid, so that the raw material gas steel cylinders 11 are intensively arranged, and the operation is convenient.
As a modified embodiment, it further comprises a filling and distributing ring 21 with a passage, the filling and distributing ring 21 is communicated with the fifth branch 16, and the filling cylinders 18 are communicated with the filling and distributing ring 21 at equal intervals.
As a modified example, the organic impurity collecting tank 24 is arranged close to the supercritical carbon dioxide throttle valve 23, which can prevent the organic impurity desorption discharge pipeline from being blocked by the organic impurities, and the supercritical carbon dioxide charging steel cylinder stop valve 19 is arranged close to the charging distribution ring 21.
The invention discloses a method for cleaning ultrahigh pure gas steel cylinders in batch by using supercritical fluid, which comprises the following steps:
1) carbon dioxide in the carbon dioxide supplementing steel cylinder 4 enters a carbon dioxide circulating compressor 6 through a carbon dioxide supplementing stop valve 5 and is compressed to the critical pressure of 7.4MPaA, when high-pressure carbon dioxide gas from the carbon dioxide circulating compressor 6 passes through a cooling water heat exchanger 7, the high-pressure carbon dioxide gas exchanges heat with industrial cooling water in the cooling water heat exchanger 7, the high-pressure carbon dioxide gas is cooled to the critical temperature of 31 ℃, supercritical carbon dioxide from the cooling water heat exchanger 7 is sequentially monitored by a supercritical carbon dioxide thermometer 27 and a supercritical carbon dioxide pressure gauge 28, and then is metered by a supercritical carbon dioxide flowmeter 29;
2) the metered supercritical carbon dioxide is divided into a first branch 8 and a second branch 9 for conveying: the supercritical carbon dioxide in the first branch 8 directly enters a raw material gas steel cylinder 11, and then the supercritical carbon dioxide is controlled by a stop valve 12 of the supercritical carbon dioxide raw material gas steel cylinder to fill a steel cylinder 18; the supercritical carbon dioxide in the second branch 9 firstly passes through the supercritical carbon dioxide to fill the steel cylinder stop valve 13 and then fills the steel cylinder 18; if the feed gas steel cylinder 11 is cleaned, the supercritical carbon dioxide is firstly closed to fill the steel cylinder stop valve 13, the supercritical carbon dioxide enters the feed gas steel cylinder 11, the supercritical carbon dioxide is controlled by the supercritical carbon dioxide feed gas steel cylinder stop valve 12 when exiting the feed gas steel cylinder 11, and the supercritical carbon dioxide flows to the third branch 10 when being communicated; if the raw gas steel cylinder 11 does not need to be cleaned, the supercritical carbon dioxide directly passes through the supercritical carbon dioxide filling steel cylinder stop valve 13 and flows to the third branch 10; the first branch 8 and the second branch 9 are connected with a seventh branch 33 in a gathering manner, the seventh branch 33 is sequentially connected with a system vacuumizing stop valve 34, a vacuum resistance gauge 35 and a vacuumizing rotary vane pump 36, the vacuumizing rotary vane pump 37 is communicated with the outside, and the vacuumizing rotary vane pump 36 is started to realize vacuumizing;
3) the supercritical carbon dioxide in the third branch 10 is divided into a fourth branch 15 and a fifth branch 16 for conveying: the supercritical carbon dioxide in the third branch 10 firstly passes through the supercritical carbon dioxide to fill the steel cylinder check valve 14, and then enters the supercritical carbon dioxide buffer tank 22 through the supercritical carbon dioxide stop valve 17 on the fourth branch 15; supercritical carbon dioxide in the third branch 10 firstly passes through a supercritical carbon dioxide filling steel cylinder check valve 14, then enters a supercritical carbon dioxide filling steel cylinder 18 in the fifth branch 16, and then passes through a supercritical carbon dioxide discharging and filling steel cylinder stop valve 19 and enters a sixth branch 20 and a supercritical carbon dioxide buffer tank 22; if the supercritical carbon dioxide needs to be cleaned to fill the steel cylinder 18, the supercritical carbon dioxide stop valve 17 is closed, and the supercritical carbon dioxide enters the filling steel cylinder 18 through the filling distribution ring 21; if the supercritical carbon dioxide is not required to be cleaned to fill the steel cylinder 18, the supercritical carbon dioxide directly enters the sixth branch 20 and the supercritical carbon dioxide buffer tank 22 from the supercritical carbon dioxide stop valve 17, and a supercritical carbon dioxide safety valve 30 is arranged at an inlet of the supercritical carbon dioxide buffer tank 22 to prevent overpressure of a system pipeline;
4) the supercritical carbon dioxide which is discharged from the supercritical carbon dioxide buffer tank 22 is throttled and depressurized by the supercritical carbon dioxide throttle valve 23 to become normal-temperature normal-pressure carbon dioxide, organic impurities dissolved in the carbon dioxide are separated out and accumulated at the bottom of the organic impurity collecting tank 24, and is periodically discharged by the organic impurity discharge stop valve 26 once every 1-3 weeks, the outlet of the normal-temperature normal-pressure carbon dioxide stop valve 25 is extended and connected between the carbon dioxide supplement stop valve 5 and the carbon dioxide circulating compressor 6, and the normal-temperature normal-pressure carbon dioxide after the impurities are resolved is converged with the carbon dioxide in the carbon dioxide supplement steel cylinder 4 and then sequentially enters each branch to enter circulation.
Finally, it should be noted that the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (10)
1. A system for cleaning ultra-high purity gas steel cylinders in batch by using supercritical fluid is characterized in that: comprises a supercritical carbon dioxide supplement pipeline (1), a high-purity gas steel cylinder cleaning pipeline (2) and an organic impurity analysis discharge pipeline (3) which are communicated in sequence;
the supercritical carbon dioxide cleaning device is characterized in that an inlet of the supercritical carbon dioxide supplementing pipeline (1) is communicated with a carbon dioxide supplementing steel cylinder (4), the supercritical carbon dioxide supplementing pipeline (1) is sequentially connected with a carbon dioxide supplementing stop valve (5), a carbon dioxide circulating compressor (6), a cooling water heat exchanger (7) and a measurer, the high-purity gas steel cylinder cleaning pipeline (2) comprises a first branch (8) and a second branch (9), the tail ends of the first branch (8) and the second branch (9) are converged and communicated to form a third branch (10), the first branch (8) is sequentially connected with a raw material gas steel cylinder (11) and a supercritical carbon dioxide raw material steel cylinder stop valve (12), the second branch (9) is connected with a supercritical carbon dioxide steel cylinder filling stop valve (13), and the third branch (10) is connected with a supercritical carbon dioxide steel cylinder filling check valve (14), supercritical carbon dioxide goes to fill a dress steel bottle check valve (14) export and extends and divide and be equipped with fourth branch road (15), fifth branch road (16), be connected with supercritical carbon dioxide stop valve (17) on fourth branch road (15), connect gradually on fifth branch road (16) and fill a dress steel bottle (18), supercritical carbon dioxide and go out and fill a dress steel bottle stop valve (19), fourth branch road (15), fifth branch road (16) end are collected and are formed with sixth branch road (20), sixth branch road (20) and organic impurity are analyzed and are discharged pipeline (3) intercommunication.
2. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 1, wherein: organic impurity analysis discharges pipeline (3) including in proper order connect supercritical carbon dioxide buffer tank (22), supercritical carbon dioxide throttle valve (23), organic impurity collection tank (24) on organic impurity analysis discharges pipeline (3), organic impurity collection tank (24) are connected with mutual independent normal atmospheric temperature and pressure carbon dioxide stop valve (25), organic impurity and excrete stop valve (26), normal atmospheric temperature and pressure carbon dioxide stop valve (25) export extension is connected between carbon dioxide supplement stop valve (5), carbon dioxide circulating compressor (6).
3. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 1, wherein: the measurer comprises a supercritical carbon dioxide thermometer (27), a supercritical carbon dioxide pressure gauge (28) and a supercritical carbon dioxide flow meter (29) which are arranged in sequence; the raw gas steel cylinders (11) and the filling steel cylinders (18) are respectively provided with a plurality of steel cylinders.
4. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 2, wherein: the outlet end of the supercritical carbon dioxide supplement pipeline (1) and the inlet end of the supercritical carbon dioxide buffer tank (22) are communicated with a supercritical carbon dioxide safety valve (30).
5. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 1, wherein: the cooling water heat exchanger (7) is communicated with a cold source, the cold source is an industrial cooling water tank (31), and the cooling water heat exchanger (7) is provided with an industrial cooling water outlet (32).
6. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 1 or 2 or 3 or 4 or 5, wherein: the vacuum pump is characterized in that a seventh branch (33) is connected to the first branch (8) and the second branch (9) in a gathering mode, a system vacuum stop valve (34), a vacuum resistance gauge (35) and a vacuum rotary vane pump (36) are sequentially connected to the seventh branch (33), and the vacuum rotary vane pump (36) is communicated with the outside.
7. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 2, 3 or 4, wherein: still include raw materials gas steel cylinder collection dress check, raw materials gas steel cylinder (11) are placed in raw materials gas steel cylinder collection dress check.
8. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 3, wherein: the filling and distributing ring (21) with a passage is further included, the filling and distributing ring (21) is communicated with the fifth branch (16), and the filling steel cylinders (18) are communicated with the filling and distributing ring (21) at equal intervals.
9. A system for batch cleaning ultra-high purity gas cylinders using supercritical fluid according to claim 2 or 4, wherein: the organic impurity collecting tank (24) is arranged close to the supercritical carbon dioxide throttling and adjusting valve (23); the supercritical carbon dioxide discharging and filling steel cylinder stop valve (19) is arranged close to the filling distribution ring (21).
10. A method for cleaning ultrahigh pure gas steel cylinders in batch by using supercritical fluid is characterized by comprising the following steps:
1) carbon dioxide in the carbon dioxide supplementing steel cylinder (4) enters a carbon dioxide circulating compressor (6) through a carbon dioxide supplementing stop valve (5) and is compressed to the critical pressure of 7.4MPa (A), when high-pressure carbon dioxide gas coming out of the carbon dioxide circulating compressor (6) passes through a cooling water heat exchanger (7), the high-pressure carbon dioxide gas exchanges heat with industrial cooling water in the cooling water heat exchanger (7), the high-pressure carbon dioxide gas is cooled to the critical temperature of 31 ℃, and supercritical carbon dioxide coming out of the cooling water heat exchanger (7) is sequentially monitored by a supercritical carbon dioxide thermometer (27) and a supercritical carbon dioxide pressure gauge (28) and then metered by a supercritical carbon dioxide flowmeter (29);
2) the metered supercritical carbon dioxide is divided into a first branch (8) and a second branch (9) for conveying: supercritical carbon dioxide in the first branch (8) directly enters a feed gas steel cylinder (11), and then the supercritical carbon dioxide is controlled by a stop valve (12) of the feed gas steel cylinder to fill a steel cylinder (18); the supercritical carbon dioxide in the second branch (9) firstly passes through the supercritical carbon dioxide to fill a steel cylinder stop valve (13) and then fills a steel cylinder (18); if the raw material gas steel cylinder (11) is cleaned, the supercritical carbon dioxide is firstly closed to fill the steel cylinder stop valve (13), the supercritical carbon dioxide enters the raw material gas steel cylinder (11), the supercritical carbon dioxide is controlled by the supercritical carbon dioxide raw material gas steel cylinder stop valve (12) when exiting the raw material gas steel cylinder (11), and the supercritical carbon dioxide flows to the third branch (10) when passing through the channel; if the raw material gas steel cylinder (11) does not need to be cleaned, the supercritical carbon dioxide directly passes through a stop valve (13) for filling the steel cylinder from the supercritical carbon dioxide and flows to the third branch (10); the first branch (8) and the second branch (9) are connected with a seventh branch (33) in a gathering manner, the seventh branch (33) is sequentially connected with a system vacuumizing stop valve (34), a vacuum resistance gauge (35) and a vacuumizing rotary vane pump (36), the vacuumizing rotary vane pump (36) is communicated with the outside, and the vacuumizing rotary vane pump (36) is started to realize vacuumizing;
3) the supercritical carbon dioxide in the third branch (10) is divided into a fourth branch (15) and a fifth branch (16) for conveying: wherein, the supercritical carbon dioxide in the third branch (10) firstly passes through the supercritical carbon dioxide to fill a steel cylinder check valve (14), and then enters a supercritical carbon dioxide buffer tank (22) through a supercritical carbon dioxide stop valve (17) on the fourth branch (15); supercritical carbon dioxide in the third branch (10) firstly passes through a supercritical carbon dioxide filling steel cylinder check valve (14), then enters a fifth branch (16) to be filled with supercritical carbon dioxide filling steel cylinders (18), and then passes through a supercritical carbon dioxide filling steel cylinder stop valve (19) to enter a sixth branch (20) and a supercritical carbon dioxide buffer tank (22); if the supercritical carbon dioxide needs to be cleaned to fill the steel cylinder (18), the supercritical carbon dioxide stop valve (17) is closed, and the supercritical carbon dioxide enters the filling steel cylinder (18) through the filling distribution ring (21); if the supercritical carbon dioxide is not required to be cleaned to fill the steel cylinder (18), the supercritical carbon dioxide directly enters the sixth branch (20) and the supercritical carbon dioxide buffer tank (22) from the supercritical carbon dioxide stop valve (17), and a supercritical carbon dioxide safety valve (30) is arranged at the inlet of the supercritical carbon dioxide buffer tank (22) to prevent the overpressure of a system pipeline;
4) supercritical carbon dioxide which goes out of the supercritical carbon dioxide buffer tank (22) is throttled and depressurized through a supercritical carbon dioxide throttling valve (23) to become normal-temperature normal-pressure carbon dioxide, organic impurities dissolved in the carbon dioxide are separated out and accumulated at the bottom of an organic impurity collecting tank (24), and is periodically discharged through an organic impurity discharge stop valve (26), the outlet of the normal-temperature normal-pressure carbon dioxide stop valve (25) is extended and connected between a carbon dioxide supplement stop valve (5) and a carbon dioxide circulating compressor (6), the normal-temperature normal-pressure carbon dioxide after the impurities are resolved is converged with the carbon dioxide in a carbon dioxide supplement steel cylinder (4), and then the carbon dioxide sequentially enters each branch and enters circulation.
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