CN104176717B - A kind of helium recovery method of purification and device - Google Patents
A kind of helium recovery method of purification and device Download PDFInfo
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- CN104176717B CN104176717B CN201410404048.9A CN201410404048A CN104176717B CN 104176717 B CN104176717 B CN 104176717B CN 201410404048 A CN201410404048 A CN 201410404048A CN 104176717 B CN104176717 B CN 104176717B
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- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The present invention is open provides a kind of helium recovery method of purification, and it step included is followed successively by: filter；Chemisorbed；Distribution；Heating；Catalysis；Cooling；Primary purification；Cooling；Rectification；Double purification.The invention also discloses a kind of helium recovery purifying plant, this device includes: filter；Chemisorption apparatus；Component analysis device；Add gas tank；Heater；Catalysis system；Cooler；First cleaning system；Raw helium cooler；Rectifying column；Second cleaning system；And helium storage tank.Use helium recovery method of purification and the device of the present invention, it is possible to for reclaiming the industrial waste gas containing helium, the purity of helium improved, it is also possible to go deep into purification and obtain pure helium, high-pure helium and ultrapure helium product.Relative to prior art, use the helium recovery method of purification of the present invention and device reclaim purify helium have that technique is simple, have that technique is simple, cost is relatively low, environment-friendly high-efficiency and the wider advantage of the scope of application.
Description
Technical field
The present invention relates to a kind of purification helium that reclaims from industrial exhaust gas and prepare the method and device of high-purity helium product.
Background technology
Helium is colorless and odorless, non-combustible gas, and the content in air is about 5.2/1000000ths.The complete torpescence of chemical property, is not combined with other element or compound under usual state.
Helium is widely used in the fields such as such as military project, scientific research, petrochemical industry, refrigeration, medical treatment, quasiconductor, pipeline leak detection, superconducting experiment, metal manufacture, deep sea diving, precision welding, O-E Products production.Its main uses has: utilize the low boiling of helium-268.9 DEG C, and liquid helium may be used for ultralow temperature cooling；In superconductor applications the most concerned in the fields such as aerotrain, helium is indispensable；Additionally, due to chemical property torpescence and be lighter than the features such as air, helium is usually used in the insufflation gas in airship or advertising balloon, and this purposes is also well-known；In the breathing mixture body in ocean development field, and in the purposes of the superconducting electromagnet cooling of the magnetic resonance imaging device of medical field, helium is widely used；Helium also is used as the protection gas of the metal solder such as leak-checking agent and magnesium, zirconium, aluminum, the titanium of high-vacuum installation, the nuclear reactor, spacecraft etc.；Rocket, spacecraft are used as the gas-pressurized of the conveying liquid propellant such as liquid hydrogen, liquid oxygen；Also serve as the abluent of atomic pile, the carrier gas of gas chromatographic analysis analysis, balloon inflation, arc welding protection gas, diving gaseous mixture and the filling gas of gas thermometer；The feature good, non-flammable additionally, due to helium permeability, it is also applied to vacuum leak hunting industry, such as helium mass spectrometer leak detector etc..
Helium can separate extraction in theory from air, but because its content is excessive rarefied, industrial separates from the natural gas of helium content about 0.5%, is refining to obtain helium.But owing to separating, being refining to obtain the complex process of helium, relatively costly, therefore, it is difficult to be widely used from natural gas.On the other hand, helium is finally all discharged along with industrial waste gas in making application together, causes the substantial amounts of wasting of resources, does not meets the energy-conserving and environment-protective demand that people are growing.But at present, although have some helium recovery system can reclaim helium, but after reclaiming, the purity of helium cannot ensure.Helium after recovery also needs to be purified and just can reuse, and the purification of helium bothers the most very much, relatively costly.
Therefore, a kind of technique helium recovery method of purification simple, lower-cost and device in prior art, it is possible to reclaim from the gas of industrial and mining establishment's discharge and purify helium, obtaining highly purified helium product.
Summary of the invention
In order to overcome the defect of prior art, first purpose of the present invention is to provide the helium recovery method of purification that a kind of technique is simple, cost is relatively low, can prepare high-purity helium product.
For reaching above-mentioned purpose, the present invention provides a kind of helium recovery method of purification, it is characterised in that comprise the following steps:
1. raw helium gas is collected and pressurized storage, then the raw helium gas after pressurization is filtered, remove the granule foreign such as oil removing, dust；
2. the raw helium gas after filtering, through chemisorbed, removes poisonous and hazardous corrosive impurity；
3. the raw helium gas after chemisorbed adds oxygen after component analysis and carries out distribution；
4. the raw helium gas after completing distribution heats, and the raw helium gas after heating enters catalysis system and carries out catalytic treatment；
5. cooling down the raw helium gas after catalysis, the raw helium gas after cooling enters low temperature purification system and carries out primary purification process；
6. the raw helium gas after primary purification is cooled down by raw helium cooler, and the raw helium gas entrance rectifying column being cooled to set point of temperature carries out cryogenic rectification, improves the concentrations of helium in gas；
7. the helium after concentration improves enters low temperature purification system and carries out double purification process, obtains highly purified helium product after purification.
Wherein, described primary purification processes and double purification processes and all includes gas is carried out adsorption treatment.
It is preferred that step 3. in, all components in gas is analyzed by the raw helium gas after filtration through chromatograph, then adds oxygen and carries out distribution by adding gas tank 3.For ensure safety and prevent from being catalyzed overheated, oxygenation distribution can aerating several times and repeatedly catalysis carry out, it is ensured that catalytic temperature is all in safety range every time.
It is preferred that step 4. in, the detailed process heating raw helium gas is: the raw helium gas after distribution completes first preheats, and raw helium gas after preheating enters heater and carries out post bake, and raw helium gas gradually rises through preheating and post bake temperature.
It is preferred that step 5. in, the detailed process cooling down raw helium gas is: the raw helium gas after catalysis first carries out pre-cooling, and raw helium gas after pre-cooling enters cooler and carries out cooling twice, and raw helium gas gradually lowers through pre-cooling and cooling twice temperature.
It is preferred that the 1. described raw helium gas of step is from the industrial discharged waste gas containing helium.
Wherein, including but not limited to the one or more of which of following impurity in described industrial discharged waste gas: nitrogen, hydrogen, argon, neon, oxygen, carbon monoxide, carbon dioxide, water, methane, chlorine, chloride, fluoride, bromide, hydro carbons, dust, oil.
The present invention also provides for a kind of helium recovery purifying plant, it is characterised in that include successively:
Raw helium gas is filtered the filter of the granule foreign such as oil removing and dust；
The chemisorption apparatus of the poisonous and harmful corrosive impurity in removal raw helium gas；
The component analysis device that all components in raw helium gas after filtering is analyzed；
That adds oxygen in the raw helium gas after filtering adds gas tank；
The heater that raw helium gas is heated；
Raw helium gas after heating is catalyzed the catalysis system of impurity such as making carbon monoxide therein, hydro carbons, hydrogen and oxygen generation redox reaction；
For the cooler carrying out cooling down by the raw helium gas after catalysis；
For the raw helium gas after cooling being carried out the first cleaning system of cold drying and adsorption treatment；
For the raw helium cooler that the raw helium gas through purifying is cooled down；
For the raw helium gas after cooling being carried out the rectifying column of rectification；
For the raw helium gas through rectification being carried out again the second cleaning system of cold drying and adsorption treatment；
For storing the helium storage tank of the helium product of described second cleaning system output.
Wherein, described first lowization system and described second cleaning system are all the circulating purification systems being made up of multiple absorbing cylinders.
It is preferred that described helium recovery purifying plant also includes for preheating the raw helium gas after adding oxygen and the raw helium gas after catalysis system is catalyzed carrying out the heat recovery system of pre-cooling.
In one embodiment, described heat recovery system is heat exchanger, described heat exchanger includes heat passage and cold flow passage, described heat passage adds in the conveyance conduit between gas tank and described heater described in being connected to, and described cold flow passage is connected in the conveyance conduit of described catalysis system and described cooler.
Owing to using technique scheme, use helium recovery method of purification and the device of the present invention, can be using the waste gas containing helium that discharges from any industrial and mining establishment as raw helium gas, through filtration, distribution, heat, be catalyzed, cool down, the step such as primary purification, liquid nitrogen washing and double purification, helium purity is improved, it might even be possible to go deep into pure helium, high-pure helium and ultrapure helium product (helium gas volume concentrations >=99.9999%) that purification obtains meeting in National Standard of the People's Republic of China GB/T4844-2011 " pure helium, high-pure helium, ultrapure helium ".The helium recovery method of purification of the present invention and device are applicable to helium gas volume concentrations and are 1% to 99% but are not limited to the recovery of the raw helium gas of this volume concentration range and purify, and raw helium gas can have pressure can also not have pressure, and range of application is wider.Compared to prior art, use the method and device of the present invention reclaim purify helium have that technique is simple, cost is relatively low, environment-friendly high-efficiency and the wider advantage of the scope of application.
Accompanying drawing explanation
Fig. 1 is the process chart of the helium recovery method of purification of the present invention.
Fig. 2 is the structural representation of the helium recovery purifying plant of the present invention.
In accompanying drawing: 1-filter；2-chemisorption apparatus；3-adds gas tank；4-heat exchanger；5-electric heater；6-is catalyzed cylinder；7-cooler；8-the first absorbing cylinder；9-rectifying column；10-raw helium cooler；11-the second absorbing cylinder；12-helium storage tank；The electric heater of 13-the first cleaning system；The electric heater of 14-the second cleaning system.
Detailed description of the invention
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described in detail.
Referring to Fig. 1 and Fig. 2, the helium recovery purifying plant of the present invention includes successively: raw helium gas filters filter 1 and the chemisorption apparatus 2 of the granule foreigns such as oil removing, dust and chlorine；To the component analysis device that is analyzed of all components in the raw helium gas after filtering, being chromatograph (not shown) in the present embodiment, it is arranged on chemisorption apparatus 2 and the conveyance conduit that adds between gas tank 3；That adds oxygen in the raw helium gas after filtering adds gas tank 3；Raw helium gas is carried out the heat exchanger 4 of pre-warmed heat recovery, raw helium gas is carried out the electric heater 5 of post bake；Raw helium gas after heating is catalyzed the catalysis system of impurity such as making carbon monoxide therein, hydro carbons, hydrogen and oxygen generation redox reaction, and this catalysis system is catalysis cylinder 6；Raw helium gas after catalysis carries out the heat recovery system precooled, and raw helium gas carries out the cooler 7 of cooling twice；For the raw helium gas after cooling is dried the first cleaning system with adsorption treatment, in the present embodiment, this first cleaning system is the system that the circulation being made up of two the first absorbing cylinders 8 can be carried out continuously purification；For the raw helium cooler 10 that the raw helium gas through primary purification is cooled down；For the raw helium gas after cooling being carried out the rectifying column 9 of rectification；For the raw helium gas through rectification carries out the second cleaning system of cryogenic absorption process, in the present embodiment, this second cleaning system is the circulating purification system being made up of two the second absorbing cylinders 11；For storing the helium storage tank 12 of the product helium of described second cleaning system output.
In the present embodiment, described heat recovery system is heat exchanger 4, heat exchanger 4 includes heat passage and cold flow passage, and described heat passage is connected to be catalyzed in the conveyance conduit of cylinder 6 and cooler 7, and described cold flow passage is connected to add in the conveyance conduit between gas tank 3 and electric heater 5.
Helium recovery purifying technique comprises the following steps:
Filter
Industrial discharged waste gas containing helium is collected and pressurized storage, then the raw helium gas after pressurization is filtered through filter 1, by removing the granule foreign such as oil removing, dust after accurate filter 1.
Chemisorbed
After removing the granule foreign such as oil removing, dust, enter chemisorption apparatus 2, carry out removing poisonous and harmful corrosive impurity, such as carbide, chloride and arsenide etc..
Distribution
All components in gas is analyzed by the raw helium gas after filtration through chromatograph, then adds oxygen and carries out distribution by adding gas tank 3.For ensure safety and prevent from being catalyzed overheated, oxygenation distribution can aerating several times and repeatedly catalysis carry out, it is ensured that catalytic temperature is all in safety range every time.
Raw helium gas after completing distribution carries out heat exchange through the cold flow passage of heat exchanger 4 with the high-temperature gas going out to be catalyzed cylinder, reach certain preheating temperature, so can reduce the heating load of heater below, thus reduce the power consumption of heater, raw helium gas after preheating gradually rises through preheating and post bake temperature through electric heater 5 post bake, raw helium gas.
Catalysis
The raw helium gas that will warm up uniform temperature carries out catalytic treatment through catalysis cylinder 6.After catalysis, the carbon monoxide in raw helium gas, carbon dioxide, hydrogen, hydrocarbon gas generate water and carbon dioxide with oxygen generation redox reaction.
Cooling
Through the cold flow passage of heat exchanger 4, the raw helium gas after catalysis is carried out pre-cooling, and the purpose of pre-cooling is cooler 7 load after reducing, and reduces cost.Raw helium gas after pre-cooling is again through subcooler 7 cooling twice, and raw helium gas is gradually lowered through pre-cooling and cooling twice temperature.
Primary purification
The raw helium gas that will be cooled to uniform temperature carries out primary purification process through the primary purification system being made up of an electric heater 13 and one or more first absorbing cylinder 8.Primary purification processes main being dried raw helium gas and decarburization absorption, removes the water in raw helium gas and carbon dioxide.It is for saturated absorbing cylinder is added Thermal desorption that first cleaning system is provided with electric heater 13, the most just makes absorbing cylinder to work the most continuously.
Cooling
Raw helium gas after primary purification is carried out degree of depth cooling by raw helium cooler 10, reaches extremely low temperature.
Rectification
The raw helium gas being cooled to set point of temperature being entered rectifying column 9 and carries out rectification, by high boiling point gaseous impurity, the such as gas such as micro CO, argon, nitrogen is separated by cryogenic rectification, to improve the concentrations of helium in gas.Rectifying column 9 has helium entrance, helium outlet, liquid nitrogen entrance and liquid nitrogen fraction output channel.Raw helium cooler 10 uses a heat exchanger that with the pipeline of input helium, the liquid nitrogen fraction output channel of rectifying column 9 is carried out heat exchange, thus is input to after raw helium air cooling in rectifying column 9.
Double purification
Helium concentration after rectification improved enters the second cleaning system being made up of an electric heater 14 and one or more second absorbing cylinder 11 and carries out double purification process, after the double purifications such as cryogenic absorption denitrogenation, obtain highly purified helium product, meet pure helium, high-pure helium and ultrapure helium product in GB/T4844-2011 " pure helium, high-pure helium and ultrapure helium ".
Claims (9)
1. a helium recovery method of purification, it is characterised in that comprise the following steps:
1. raw helium gas is collected and pressurized storage, then the raw helium gas after pressurization is filtered, remove oil removing, dust；
2. the raw helium gas after filtering, through chemisorbed, removes poisonous and hazardous corrosive impurity；
3. the raw helium gas after chemisorbed adds oxygen after component analysis and carries out distribution；
4. the raw helium gas after completing distribution heats, and the raw helium gas after heating enters catalysis system and carries out catalytic treatment；
5. cooling down the raw helium gas after catalysis, the raw helium gas after cooling enters low temperature purification system and carries out primary purification process；
6. the raw helium gas after primary purification is cooled down by raw helium cooler, and the raw helium gas entrance rectifying column being cooled to set point of temperature carries out cryogenic rectification, improves the concentrations of helium in gas；
7. the helium after concentration improves enters low temperature purification system and carries out double purification process, obtains highly purified helium product after purification；
Described primary purification processes and double purification processes and all includes gas is carried out adsorption treatment.
A kind of helium recovery method of purification the most according to claim 1, it is characterised in that: step 3. in, all components in gas is analyzed by the raw helium gas after chemisorbed through chromatograph, then adds oxygen and carries out distribution by adding gas tank.
A kind of helium recovery method of purification the most according to claim 1, it is characterized in that: step 4. in, the detailed process heating raw helium gas is: the raw helium gas after distribution completes first preheats, raw helium gas after preheating enters heater and carries out post bake, and raw helium gas gradually rises through preheating and post bake temperature.
A kind of helium recovery method of purification the most according to claim 1, it is characterized in that: step 5. in, the detailed process cooling down raw helium gas is: the raw helium gas after catalysis first carries out pre-cooling, raw helium gas after pre-cooling enters cooler and carries out cooling twice, and raw helium gas gradually lowers through pre-cooling and cooling twice temperature.
A kind of helium recovery method of purification the most according to claim 1, it is characterised in that: the 1. described raw helium gas of step is from the industrial discharged waste gas containing helium；Including but not limited to the one or more of which of following impurity in described industrial discharged waste gas: nitrogen, hydrogen, argon, neon, oxygen, carbon monoxide, carbon dioxide, water, chlorine, chloride, fluoride, bromide, hydro carbons, dust, oil.
6. a helium recovery purifying plant, it is characterised in that include successively:
Raw helium gas is filtered the filter of oil removing and dust；
Raw helium gas is carried out the device of chemisorbed；
The component analysis device that all components in raw helium gas after chemisorbed is analyzed；
That adds oxygen in the raw helium gas after chemisorbed adds gas tank；
The heater that raw helium gas is heated；
Raw helium gas after heating is catalyzed the catalysis system making carbon monoxide therein, hydro carbons, hydrogen with oxygen generation redox reaction；
For the cooler carrying out cooling down by the raw helium gas after catalysis；
For the raw helium gas after cooling being carried out the first cleaning system of cold drying and adsorption treatment；
For the raw helium cooler that the raw helium gas through purifying is cooled down；
For the raw helium gas after cooling being carried out the rectifying column of cryogenic rectification；
For the raw helium gas through rectification being carried out again the second cleaning system of cold drying and adsorption treatment；
For storing the helium storage tank of the helium product of described second cleaning system output.
A kind of helium recovery purifying plant the most according to claim 6, it is characterised in that: described first cleaning system and described second cleaning system are all the continuous type cleaning systems of circulation being made up of an electric heater and multiple absorbing cylinder.
A kind of helium recovery purifying plant the most according to claim 6, it is characterised in that: also include for the raw helium gas after adding oxygen being preheated and the raw helium gas after catalysis system is catalyzed being carried out the heat recovery system of pre-cooling.
A kind of helium recovery purifying plant the most according to claim 8, it is characterized in that: described heat recovery system is heat exchanger, described heat exchanger includes heat passage and cold flow passage, described heat passage adds in the conveyance conduit between gas tank and described heater described in being connected to, and described cold flow passage is connected in the conveyance conduit of described catalysis system and described cooler.
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| CN104596832B (en) * | 2015-01-14 | 2017-05-03 | 成都瑞芬思生物科技有限公司 | Atmospheric haze purification method |
| CN105654997B (en) * | 2016-01-15 | 2017-07-25 | 中国科学技术大学 | Off-gas oxidizing isolation of purified regeneration method and device is cleaned in a kind of fusion reactor hot cell |
| CN105632574B (en) * | 2016-01-15 | 2017-10-03 | 中国科学技术大学 | A kind of fusion reactor hot cell cleaning waste gas cryogenic rectification purifying regeneration Application way and device |
| CN106315527B (en) * | 2016-08-11 | 2019-04-30 | 四川空分设备(集团)有限责任公司 | High hydrogeneous raw helium extracts high-pure helium process for refining |
| CN108394878B (en) * | 2018-04-09 | 2019-03-05 | 西安保埃罗环保科技有限公司 | A kind of hydrogeneous helium tail gas purification Helium process |
| CN108355416A (en) * | 2018-04-19 | 2018-08-03 | 合肥硕朗自动化科技有限公司 | A kind of helium recovery purifier for vacuum tank leak detection system |
| CN111977622A (en) * | 2019-05-23 | 2020-11-24 | 香港城市大学深圳研究院 | Helium purification method and device |
| CN110498401A (en) * | 2019-09-02 | 2019-11-26 | 北京中科富海低温科技有限公司 | Helium recovery purification device |
| FR3104564B1 (en) * | 2019-12-12 | 2022-03-04 | Air Liquide | Gas purification method and device |
| CN114229810B (en) * | 2021-12-15 | 2023-11-03 | 华能核能技术研究院有限公司 | Helium purification system and method for thermal aging test of high-temperature gas cooled reactor internals |
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| US20100101410A1 (en) * | 2008-10-24 | 2010-04-29 | Ravi Prasad | Helium recovery process |
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| US20100101410A1 (en) * | 2008-10-24 | 2010-04-29 | Ravi Prasad | Helium recovery process |
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