CN202030525U - Ultrapure helium purification equipment - Google Patents

Ultrapure helium purification equipment Download PDF

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Publication number
CN202030525U
CN202030525U CN2011201109874U CN201120110987U CN202030525U CN 202030525 U CN202030525 U CN 202030525U CN 2011201109874 U CN2011201109874 U CN 2011201109874U CN 201120110987 U CN201120110987 U CN 201120110987U CN 202030525 U CN202030525 U CN 202030525U
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China
Prior art keywords
purifier
ultrapure helium
ultrapure
pipeline
liquid nitrogen
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Expired - Lifetime
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CN2011201109874U
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Chinese (zh)
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蔡体杰
刘炜炜
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SHANGHAI PUJIANG SPECIALTY GASES CO Ltd
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SHANGHAI PUJIANG SPECIALTY GASES CO Ltd
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Abstract

Ultrapure helium purification equipment comprises a feedstock pump, a buffer tank, a membrane type pressure machine, a purifier, an ultrapure helium filling unit, a pressure gauge and a reactivation and regeneration unit, wherein the feedstock pump, the buffer tank, the membrane type pressure machine, the purifier and the ultrapure helium filling unit are connected in sequence through a pipeline; and the pressure gauge is positioned between the purifier and the ultrapure helium filling unit. The utility model has the advantages that the pollution is reduced, and meanwhile, silica gel in an adsorbent cylinder body serves as a framework to reduce the pulverization speed of activated charcoal; the production cost is lowered through heat exchange of a heat exchange pipe coil; a nitrogen emptying pipe of the low-temperature purifier controls the liquid level height of liquid nitrogen in an absorber to control the liquid level of liquid nitrogen; and the insertion height of the nitrogen emptying pipe in a liquid nitrogen Dewar flask can be properly adjusted according to the purification result.

Description

Ultrapure helium purification devices
Technical field
The utility model relates to a kind of fixed sorbent material of using with gas or the isolating device of steam, especially a kind of ultrapure helium purification devices.
Background technology
Helium is a kind of rare gas, and price is more expensive.Mainly be present in atmosphere, rock and the Sweet natural gas, industry system helium extracts from Sweet natural gas mostly.Helium content is not high in the China's natural gas, generally all below 0.3%, belongs to poor helium resource.
Helium has a wide range of applications in each field of national economy, departments such as leak detection, deep water breathing, welding, laser cutting, Metal smelting, low-temperature superconducting, semiconducter device production, nuclear power industry, aerospace, war production, medical science, scientific research and gas mixture configuration, stratographic analysis all need to use helium, along with science and technology development, the production of some high-end technology products, require the purity of helium to rise to 99.999% by 99.99%, even to 99.9999%, and the 6m of one bottle of import 3Purity is 99.9999% ultrapure helium, and city's price is about 2000 yuans.So consider the costliness of helium and rare, but the current domestic helium that produces, most of from the U.S. or Australian import liquid helium, by domestic packing factory liquid helium is vaporized, compression, filling bottle forms, because the pollution in the filling process, cause dashing helium in foreign matter content higher, often can only produce some purity and be 99.99% ~ 99.995% pure helium, and consumption is increasing year by year, specification of quality is being risen progressively gradually, for guaranteeing the utilization of helium resources effective, we try to pressurize with industrial helium or from the helium that applying unit reclaims, purifying, production purity are not less than 99.999% high-pure helium or ultrapure helium.
The utility model content
The purpose of this utility model is to design a kind of purification devices, becomes purity to be not less than 99.999% ultrapure helium by the series of steps purifying industrial helium.
The utility model is achieved in that a kind of ultrapure helium purification devices, it is characterized in that: comprise feedstock pump, surge tank, membrane type press, purifier, ultrapure helium filling element and tensimeter; Described feedstock pump, surge tank, membrane type press, purifier and ultrapure helium filling element are connected by pipeline successively, and tensimeter is between purifier and ultrapure helium filling element.
Described purifier comprises blind flange, induction part, purification part, escape pipe and purifier base; Described induction part comprises inlet pipe and heat exchange coil; Described purification part comprises sorbent material cylindrical shell, desuperheating coil, liquid nitrogen inlet, gas nitrogen blow-down pipe and leakage fluid dram; Described purifier profile is a vacuum jacketed flask, the top is fixed with a blind flange, described inlet pipe is inserted blind flange and is connected with heat exchange coil, the heat exchange coil tail end connects pneumatic tube and inserts in the sorbent material cylindrical shell, described sorbent material cylindrical shell both sides are fixed with desuperheating coil, described liquid nitrogen inlet is positioned at bottom, purifier side, one purifier base is arranged at the bottom of the described purifier bottle, and the bottle end, be connected with a leakage fluid dram, gas nitrogen blow-down pipe vertical direction is inserted purifier, and is fixing near the liquid nitrogen inlet, and gas nitrogen blow-down pipe and liquid nitrogen inlet all to be positioned at sorbent tube external, described escape pipe inserts purifier top flange lid, is fixed on purifier top.
Also have another root pipeline on the connecting pipeline of described membrane type press and purifier, lead to feedstock pump, and on this pipeline a recycle valve is arranged.
One purifying valve is arranged between described membrane type press and the purifier.
Described ultrapure helium purification devices also comprises an activating and regenerating unit, is made up of electrically heated rod, oil-sealed rotary pump, tensimeter and pumpout valve.Described oil-sealed rotary pump connects escape pipe by pipeline, and tensimeter and pumpout valve are installed on the described pipeline, and described electrically heated rod vertical direction is inserted purifier sorbent material cylindrical shell inside.
The beneficial effects of the utility model, adopt the high pressure low temperature purification technique, the absorption property of sorbent material is increased, and the ultrapure helium that produces can directly fill bottle, avoid filling bottle, reduce and pollute, simultaneously with the supercharger supercharging, the high pressure adsorption and purification also increases the loading capacity and the purifying degree of depth of adsorber, guarantees quality product.Adopt filling activated coco nut charcoal and enhancement type pore spherical silica gel blended sorbent material, wherein the performance of silica gel compressive resistance variation gas shock is stronger than traditional activated carbon of sorbent, in fact silica gel has played the effect of skeleton in the absorption cylindrical shell, thereby can reduce gac efflorescence speed, in addition, the regeneration temperature of silica gel and gac is roughly the same, very coupling.Adopt the heat exchange coil heat exchange, pass to the raw material helium after the cold heat exchange that can take away the helium behind the purifying, thereby can reduce the consumption of liquid nitrogen in the production process, reduce production costs.Utilize the gas nitrogen blow-down pipe of low temperature purifier to control the liquid nitrogen liquid level of adsorber, calculate and determine the insertion height of gas nitrogen blow-down pipe in cryogenic absorption purifier Dewar container for liquefied nitrogen bottle, when liquid nitrogen surface surpasses the inlet of gas nitrogen blow-down pipe, mouth of pipe valve gushes out at that time is not gas nitrogen but liquid nitrogen, illustrate that liquid nitrogen surface has exceeded the entrance height of gas nitrogen blow-down pipe, therefore suitably regulate the add-on of liquid nitrogen, make it emit gas nitrogen and non-hydrojet nitrogen, thereby reach the purpose of control liquid nitrogen liquid level.Gas nitrogen blow-down pipe inserts the height in the Dewar container for liquefied nitrogen bottle, can do suitable lifting according to purification result.
Description of drawings
The ultrapure helium purification devices of Fig. 1 schematic flow sheet.
The ultrapure helium purifier synoptic diagram of Fig. 2.
The ultrapure helium purifier regeneration unit of Fig. 3 schematic flow sheet.
Specific embodiment
The utility model is described in further detail below in conjunction with drawings and Examples:
As shown in Figure 1, a kind of ultrapure helium purification devices comprises feedstock pump 1, surge tank 2, membrane type press 3, purifier 4, ultrapure helium filling element 5 and tensimeter 6; Described feedstock pump 1, surge tank 2, membrane type press 3, purifier 4 and ultrapure helium filling element 5 are connected by pipeline successively, and tensimeter 6 is between purifier 4 and ultrapure helium filling element 5.
As shown in Figure 2, described purifier 4 comprises blind flange 41, induction part 42, purification part 43, escape pipe 44 and purifier base 45; Described induction part 42 comprises inlet pipe 421 and heat exchange coil 422; Described purification part 43 comprises sorbent material cylindrical shell 431, desuperheating coil 432, liquid nitrogen inlet 433, gas nitrogen blow-down pipe 434 and leakage fluid dram 435; Described purifier profile is a vacuum jacketed flask, the top is fixed with a blind flange 41, described inlet pipe 421 is inserted blind flange 41 and is connected with heat exchange coil 422, heat exchange coil 422 tail ends connect pneumatic tube and insert in the sorbent material cylindrical shell 431, described sorbent material cylindrical shell 431 outer both sides are fixed with desuperheating coil 432, described liquid nitrogen inlet 433 is positioned at bottom, purifier side, one purifier base 45 is arranged at the bottom of the described purifier bottle, and the bottle end, be connected with a leakage fluid dram 435, gas nitrogen blow-down pipe 434 vertical direction are inserted purifier, fixing near liquid nitrogen inlet 433, and gas nitrogen blow-down pipe 434 all is positioned at outside the sorbent material cylindrical shell 431 with liquid nitrogen inlet 433, described escape pipe 44 inserts purifier top flange lid 41, is fixed on purifier top.
Preferably, also be provided with another root pipeline on the connecting pipeline of described membrane type press 3 and purifier 4, lead to feedstock pump 1, and a recycle valve 7 is arranged on this pipeline.
Preferably, a purifying valve 46 is arranged between described membrane type press 3 and the purifier 4.
As shown in Figure 3, described ultrapure helium purification devices also comprises an activating and regenerating unit 8, is made up of electrically heated rod 81, oil-sealed rotary pump 82, tensimeter 6 and pumpout valve 83.Described oil-sealed rotary pump 82 connects escape pipe 44 by pipeline, and tensimeter 6 and pumpout valve 83 are installed on the described pipeline, and described electrically heated rod 81 vertical direction are inserted purifier sorbent material cylindrical shell 431 inside.
Process step of the present utility model, before filling, close purifying valve 46 earlier, open recycle valve 7 and feedstock pump 1, with high-pure helium pressurising repeatedly, put and press the displacement air delivering pipeline six times, after displacement finishes, close recycle valve 7 and open purifying valve 46, ultrapure helium tank is inserted in the ultrapure helium filling element 5, open 1 pair of whole pipeline of feedstock pump and carry out pressurising, observe pressure by tensimeter 6 and reach 6Mpa, stand-by.
Subsequently, in purifier 4 stainless steel vacuum jacketed flasks, add liquid nitrogen, when being added to the little hydrojet nitrogen in gas nitrogen blow-down pipe 434 mouth of pipe places, turn liquid nitrogen filling speed down, be advisable with hydrojet nitrogen no longer with 160 liters of portable liquid nitrogen vessels.When purifier 4 internal pressures are constant, open membrane type press 3 line pressure is pressurized to 10Mpa, open purifying valve 46, the liquid helium unstripped gas slowly enters purifier 4 and carries out purifying, when pressure exceeds 10Mpa, opens ultrapure helium tank air valve, begins to fill ultrapure helium.
Because in the product gas that the ultrapure helium of use this device purifying is produced, impurity is far below the permissible value of quality and technical index regulation, so when examination and test of products result occur one or more foreign matter contents near or when reaching the permissible value of quality and technical index regulation, show that the sorbent material in the adsorber has been tending towards adsorbing saturated, should in time stop production, carry out the activating and regenerating of purifier 4 and handle.
The activating and regenerating of purifier 4 is at first closed purifying valve 46 and is opened pumpout valve 83, and the oil-sealed rotary pump 82 that next opens the activating and regenerating system is evacuated to negative pressure with purifier 4, then starts temperature controller and heats by 81 pairs of purifiers 4 of electrically heated rod.Purifier 4 stops heating after 180 ℃ ± 30 ℃ heating was found time 4 ~ 6 hours down, continue to find time, and allows it lower the temperature naturally; when device 4 temperature to be purified are reduced to below 60 ℃, close pumpout valve 83, shut down tool vacuum pump 82; when opening purifying valve 46 and being pressurized to 5Mpa, allow purifier 4 naturally cooling, stand-by.

Claims (5)

1. a ultrapure helium purification devices is characterized in that: comprise feedstock pump (1), surge tank (2), membrane type press (3), purifier (4), ultrapure helium filling element (5) and tensimeter (6); Described feedstock pump (1), surge tank (2), membrane type press (3), purifier (4) and ultrapure helium filling element (5) are connected by pipeline successively, and tensimeter (6) is positioned between purifier (4) and the ultrapure helium filling element (5).
2. ultrapure helium purification devices according to claim 1 is characterized in that: described purifier (4) comprises blind flange (41), induction part (42), purification part (43), escape pipe (44) and purifier base (45); Described induction part (42) comprises inlet pipe (421) and heat exchange coil (422); Described purification part (43) comprises sorbent material cylindrical shell (431), desuperheating coil (432), liquid nitrogen inlet (433), gas nitrogen blow-down pipe (434) and leakage fluid dram (435); Described purifier profile is a vacuum jacketed flask, the top is fixed with a blind flange (41), described inlet pipe (421) is inserted blind flange (41) and is connected with heat exchange coil (422), heat exchange coil (422) tail end connects pneumatic tube and inserts in the sorbent material cylindrical shell (431), the outer both sides of described sorbent material cylindrical shell (431) are fixed with desuperheating coil (432), described liquid nitrogen inlet (433) is positioned at bottom, purifier side, one purifier base (45) is arranged at the bottom of the described purifier bottle, and the bottle end, be connected with a leakage fluid dram (435), a gas nitrogen blow-down pipe (434) vertical direction is inserted purifier, up to fixing near the liquid nitrogen inlet (433), and gas nitrogen blow-down pipe (434) all is positioned at outside the sorbent material cylindrical shell (431) with liquid nitrogen inlet (433), described escape pipe (44) inserts purifier top flange lid (41), is fixed on purifier top.
3. ultrapure helium purification devices according to claim 1 is characterized in that: also be provided with another root pipeline on the connecting pipeline of described membrane type press (3) and purifier (4), lead to feedstock pump (1), and a recycle valve (7) is arranged on this pipeline.
4. ultrapure helium purification devices according to claim 1 is characterized in that: a purifying valve (46) is arranged between described membrane type press (3) and the purifier (4).
5. ultrapure helium purification devices according to claim 1 is characterized in that: also comprise an activating and regenerating unit (8), be made up of electrically heated rod (81), oil-sealed rotary pump (82), tensimeter (6) and pumpout valve (83); Described oil-sealed rotary pump (82) connects escape pipe (44) by pipeline, and tensimeter (6) and pumpout valve (83) are installed on the described pipeline, and described electrically heated rod (81) vertical direction is inserted purifier sorbent material cylindrical shell (431) inside.
CN2011201109874U 2011-04-15 2011-04-15 Ultrapure helium purification equipment Expired - Lifetime CN202030525U (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102654243A (en) * 2012-05-12 2012-09-05 重庆瑞信气体有限公司 Hyperpure gas charging system
CN102718198A (en) * 2012-03-14 2012-10-10 上海启元空分技术发展股份有限公司 Method and apparatus for purifying helium by condensing method
CN107497243A (en) * 2017-09-22 2017-12-22 清华大学 Gas purification apparatus
CN109422253A (en) * 2017-08-25 2019-03-05 镇江严彦气体有限公司 A kind of helium recovery and purification device
CN112902555A (en) * 2021-01-28 2021-06-04 武汉钢铁集团气体有限责任公司 Helium low-temperature purification method and device and helium refrigeration cycle system
CN113883827A (en) * 2021-10-29 2022-01-04 四川空分设备(集团)有限责任公司 Helium purification and liquefaction system
CN114484267A (en) * 2022-01-29 2022-05-13 山东简森能源科技有限公司 Helium subpackaging, recovering and purifying process
CN114950063A (en) * 2022-05-30 2022-08-30 中国工程物理研究院核物理与化学研究所 Low-temperature adsorption bed and using method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102718198A (en) * 2012-03-14 2012-10-10 上海启元空分技术发展股份有限公司 Method and apparatus for purifying helium by condensing method
CN102718198B (en) * 2012-03-14 2014-01-29 上海启元空分技术发展股份有限公司 Method and apparatus for purifying helium by condensing method
CN102654243B (en) * 2012-05-12 2014-09-03 重庆瑞信气体有限公司 Hyperpure gas charging system
CN102654243A (en) * 2012-05-12 2012-09-05 重庆瑞信气体有限公司 Hyperpure gas charging system
CN109422253A (en) * 2017-08-25 2019-03-05 镇江严彦气体有限公司 A kind of helium recovery and purification device
CN107497243B (en) * 2017-09-22 2020-09-22 清华大学 Gas purification device
CN107497243A (en) * 2017-09-22 2017-12-22 清华大学 Gas purification apparatus
CN112902555A (en) * 2021-01-28 2021-06-04 武汉钢铁集团气体有限责任公司 Helium low-temperature purification method and device and helium refrigeration cycle system
CN113883827A (en) * 2021-10-29 2022-01-04 四川空分设备(集团)有限责任公司 Helium purification and liquefaction system
CN113883827B (en) * 2021-10-29 2023-03-03 四川空分设备(集团)有限责任公司 Helium purification and liquefaction system
CN114484267A (en) * 2022-01-29 2022-05-13 山东简森能源科技有限公司 Helium subpackaging, recovering and purifying process
CN114484267B (en) * 2022-01-29 2024-03-22 山东简森能源科技有限公司 Helium split charging recovery and purification process
CN114950063A (en) * 2022-05-30 2022-08-30 中国工程物理研究院核物理与化学研究所 Low-temperature adsorption bed and using method thereof

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Granted publication date: 20111109