CN105271146B - High-purity krypton/xenon-133 gas purifier and manufacture method, the manufacture method of getter - Google Patents
High-purity krypton/xenon-133 gas purifier and manufacture method, the manufacture method of getter Download PDFInfo
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- CN105271146B CN105271146B CN201510671353.9A CN201510671353A CN105271146B CN 105271146 B CN105271146 B CN 105271146B CN 201510671353 A CN201510671353 A CN 201510671353A CN 105271146 B CN105271146 B CN 105271146B
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Abstract
The present invention discloses a kind of high-purity krypton/xenon-133 gas purifier, including：Reaction tube, hydrogen absorber, cooler, accurate filter, product storage device, the reaction tube, hydrogen absorber, cooler, accurate filter and product storage device are sequentially connected, the reaction tube is located in heater, gas reaction section is provided with the reaction tube, the both ends of the gas reaction section are equipped with stainless steel mesh layer, the stainless steel mesh interlayer is filled with getter, and the getter is in the hollow circular cylinder of one end closing.Present invention also offers a kind of method using the high-purity krypton/xenon-133 gas of above-mentioned purifier manufacture and the manufacture method of the getter for above-mentioned high-purity krypton/xenon-133 gas purifier.
Description
Technical field
The present invention relates to gas purification technique field, and in particular to a kind of high-purity krypton/xenon-133 gas purifier and utilization should
The method that purifier manufactures high-purity krypton/xenon-133 gas, has further related to a kind of getter for high-purity krypton/xenon gas purification device
Manufacture method.
Background technology
The problem of can not meeting high-end photovoltaic market and development of modern scientific technology for 1995 editions kryptons, xenon national standard,
Industry is to national standard《Krypton》(GB/T5829-2006) and《Xenon》(GB/T5828-2006) revised.2006 editions
Krypton, xenon new national standard are more strict to the quality requirement of product compared with 1995 editions kryptons, xenon former capital mark, have increased newly to nytron
The control standard of the impurity such as thing, carbon monoxide, carbon dioxide and fluorocarbon, and improve to oxynitrides, moisture etc.
The control standard of impurity.New national standard requirement is strict in and better than the external product standard gone together of the overwhelming majority, led in industrial gasses
Realizing Chinese gas products quality standard is higher than American-European standard for the first time in domain, improves the total quality water of Chinese rare gas
It is flat.
Although the krypton produced using original krypton/xenon purifier/xenon-133 gas product quality can reach 1995 editions national standards
It is required that it can not but reach the purity requirement of the high-purity krypton/xenon (99.999%) of 2006 editions new national standards.Meanwhile in the past 10 years, China is big
Gas environmental pollution aggravates, and space division system unstripped gas air quality declines, and fluorocarbon, oxynitrides content are in gradually liter
Height, 20~50ppm of fluorocarbon content the past rises in the poor krypton xenon material liquid required for high purity krypton/xenon production
To 150~220ppm, there is disposal ability deficiency in the device, loss is big, easily blocks, the problems of short life, the life-span from
1.5~2 years originally shorten to 3~6 months, and when the inlet side high temperature reaction zone getter failure of U-tube blocks, outlet
The getter of side Asia high temperature reaction zone does not fail also, but U-shaped reaction tube can only integral replacing, expensive getter utilizes
It is very insufficient.
For disadvantages mentioned above, enterprise's input great effort have developed new type purification device, though utilize the new type purification device
Purity can so be produced and reach 99.999% high purity krypton of 2006 editions new national standard requirements, xenon-133 gas product, still, in reality
In the running of border, above-mentioned new type purification device is after work 6 months, and just there occurs serious blocking for its reaction tube, it has to
Reaction tube is changed, does not reach the life expectancy of 1.5 years.
The content of the invention
Technical problem to be solved of the embodiment of the present invention is the provision of a kind of high-purity krypton/xenon-133 gas purifier and profit
The method that high-purity krypton/xenon-133 gas is manufactured with the purifier, additionally provide a kind of air-breathing for high-purity krypton/xenon gas purification device
The manufacture method of agent, it can effectively extend the service life of reaction tube.
A kind of high-purity krypton/xenon-133 gas purifier provided by the present invention, including：Reaction tube, hydrogen absorber, cooler,
Accurate filter, product storage device, the reaction tube, hydrogen absorber, cooler, accurate filter and product storage device according to
Secondary connection, the reaction tube are located in heater, and gas reaction section, the both ends of the gas reaction section are provided with the reaction tube
Stainless steel mesh layer is equipped with, the stainless steel mesh interlayer is filled with getter, and the getter is hollow in one end closing
Cylinder.
Wherein, the conversion zone includes one section of conversion zone and second-stage reaction section, one section of reaction tube and second-stage reaction pipe
Between utilize steel pipe carry out bite type connection.
Further, the high-purity krypton/xenon-133 gas purifier also includes cooling water water return tank and cooling water enters water pot, institute
State cooling water water return tank and cooling water enters water pot and is connected with cooler.
Wherein, the heater is semi-open type circular shape heater, and the semi-open type circular shape heater includes two through hinge
The semicircle cartridge heater with heater strip of connection.
Wherein, the internal diameter of the hollow circular cylinder is set to R1, external diameter is set to R2, length is set to L, and wherein external diameter R2 is equal to length
L is spent, internal diameter R1 is less than external diameter R2.
Present invention also offers a kind of method that high-purity krypton/xenon-133 gas is manufactured using above-mentioned purifier, including：
The manufactured getter in hollow circular cylinder is filled with reaction tube, the entrance of the gas reaction section and outlet filling
Stainless steel mesh layer is to fix getter；
High-purity Krypton or argon gas are filled with, and vacuumizes displacement；
In gas reaction section high-purity Krypton or argon pressure be 0.1~0.2Mpa and gas flowing in the state of, start
Semi-open type circular shape heater progressively makes gas reaction section heat up, and opened after the first temperature is reached to be heated to gas reaction section
Beginning persistently vacuumizes；And carry out gas reaction section to be cooled to second temperature, and the Krypton or xenon that need to be purified gradually are passed through,
With the Krypton or xenon after being purified.
Wherein, first temperature is 980 degrees Celsius.
Wherein, the second temperature is 960 degrees Celsius.
Present invention also offers a kind of manufacture method of the getter for above-mentioned high-purity krypton/xenon-133 gas purifier, bag
Include：
The polynary getter alloys particle of melting under vacuum condition is clayed into power；And use metal jet powder for molding
It is Φ 3.0mm~Φ 3.2mm that internal diameter, which is made, in getter power by metallurgical method, and external diameter is Φ 5.0mm~Φ 5.2mm, and length is
The hollow circular cylinder of 5.0mm~5.2mm one end closing.
Wherein, the polynary getter alloys particle of melting under vacuum condition is clayed into power using fluidized bed jet mill.
In the present invention, it can be held using space between the annulus internal voids and annulus of the getter in hollow circular cylinder shape
Receive the advantages of ZRF4 crystalline particles, and the design feature that circular ring structure can rupture under stress extruding ensure that inside reaction tube
Flow area is not blocked by ZRF4 crystalline particles, effectively extends the service life of reaction tube, at present through life-cycle pilot experiment
The data of acquisition, theoretical calculation reaction tube life longer was to more than 2 years.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings；
Fig. 1 is a kind of plane structure chart of the better embodiment of high-purity krypton/xenon-133 gas purifier of the present invention.
Fig. 2 is the structural representation of getter in Fig. 1.
Fig. 3 is the flow chart of the better embodiment of the manufacture method of getter in Fig. 1.
Fig. 4-Fig. 6 is a kind of preferable implementation for the method that high-purity krypton/xenon-133 gas is manufactured using purifier in Fig. 1 of the present invention
The flow chart of mode.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
First, before embodiment is described, it is necessary to which some herein presented terms are explained.Example
Such as：
If occur describing various elements using the term such as " first ", " second " herein, but these elements should not
Limited by these terms.These terms are only used for distinguishing an element and another element.Therefore, " first " element can also
It is referred to as " second " element without departing from the teachings of the present invention.
In addition, it is to be understood that when referring to an element " connection " or " coupled " to another element, it can be direct
Ground connects or is directly coupled to another element or there may also be intermediary element.An element is referred on the contrary, working as " directly
When connection " or " directly coupling " arrive another element, then in the absence of intermediary element.
The various terms occurred herein are used only for describing the purpose of specific embodiment and being not intended as to this
The restriction of invention.Unless context clearly dictates otherwise, then singulative is intended to also include plural form.
When using term " comprising " and/or " including " in this manual, these terms specify the feature, whole
Body, step, operation, the presence of element and/or part, but be also not excluded for more than one other feature, entirety, step, operation,
Element, part and/or the presence of its group and/or additional.
On embodiment：
, below will be simply to high-purity krypton, xenon-133 gas purification dress in order to better illustrate getter described in the invention
Put and illustrate：
It refer to shown in Fig. 1, the high-purity krypton of the present invention, the better embodiment of xenon-133 gas purifier include cooling water backwater
Tank 1, cooling water enter 2, one sections of reaction tubes 9 of water pot, second-stage reaction pipe 10, hydrogen absorber 11, cooler 12, accurate filter 13,
Product storage device 5.Raw material gas bottle 6 passes sequentially through one section of reaction tube 9, second-stage reaction pipe 10, hydrogen absorber 11, cooler
12nd, accurate filter 13 and product storage device 5 are connected, and steel pipe is utilized between one section of reaction tube 9 and second-stage reaction pipe 10
14 carry out bite type connection.The cooling water water return tank 1 and cooling water enter water pot 2 and are connected with cooler 12.
A semi-open type circular shape heater 15 is respectively provided with outside one section of reaction tube 9 and second-stage reaction pipe 10, it is described half-open
Formula circular shape heater 15 is formed by two through the hinged semicircle cartridge heater 8 with heater strip.One section of reaction tube 9
With gas reaction section 16 is equipped with second-stage reaction pipe 10, the both ends of the gas reaction section 16 are equipped with stainless steel mesh layer 4,
Getter 20 is filled with therebetween.
In present embodiment, because steel pipe 14 and one section of reaction tube 9 and second-stage reaction pipe 10 are removable connection, therefore
The reaction tube can be removed after wherein any one reaction tube failure, then a new reaction tube is installed again as replacement, and
Without two reaction tubes are abandoned together, purpose is reused to greatest extent so as to reach, and reduces operating cost.Meanwhile when
The hinge between semicircle cartridge heater 8 can be untied after heater strip damage, changes heater strip, it is convenient and swift.In addition, present embodiment
Stainless steel mesh layer 4 is provided with the inlet and outlet of gas reaction section 16, does not influence to use so as to truly realize
Increase the purpose of the permeability of getter on the premise of function, can effectively avoid blocking the generation of etching problem, greatly improve suction
Gas agent and the service life of conversion zone.
It refer to shown in Fig. 2, the getter 20 is in the hollow circular cylinder of one end closing, and it includes annulus internal voids 22
And space 26 between annulus.The internal diameter of the hollow circular cylinder is set to R1, external diameter is set to R2, length is set to L.Present embodiment
In, the external diameter R2 of the hollow circular cylinder is equal to length L, and internal diameter R1 is less than external diameter R2.Specifically, internal diameter is Φ 3.0mm~Φ
3.2mm, external diameter are Φ 5.0mm~Φ 5.2mm, and length is 5.0mm~5.2mm.
In the present invention, ZRF4 crystallizations can be accommodated using space 26 between the annulus internal voids 22 and annulus of getter 20
The advantage of particle, and the design feature that circular ring structure can rupture under stress extruding ensure that reaction tube internal circulation section not
Blocked by ZRF4 crystalline particles, effectively extend the service life of reaction tube, the data obtained at present through life-cycle pilot experiment,
Theoretical calculation reaction tube life longer was to more than 2 years.
Please continue to refer to shown in Fig. 3, the better embodiment of the manufacture method of getter 20 includes following step in the present invention
Suddenly：
Step S1：Using fluidized bed jet mill by the polynary getter alloys particle of melting under vacuum condition (particle diameter 3~
6mm) clay into power (10~20um of particle diameter).
Step S2：Use metal jet powder for molding metallurgical method that getter power is made into internal diameter for Φ 3.0mm~Φ
3.2mm, external diameter are Φ 5.0mm~Φ 5.2mm, and length is 5.0mm~5.2mm hollow ring.
After above-mentioned getter is completed in manufacture, the present invention manufactures high-purity krypton/xenon using above-mentioned high-purity krypton, xenon-133 gas purifier
The method of gas is following (refer to shown in Fig. 4)：
Step S10：The manufactured getter 20 in hollow circular cylinder is filled with to the one section of reaction tube 9 and second-stage reaction of series connection
Pipe 10, the entrance of the gas reaction section 16 and outlet fill stainless steel mesh layer 4 to fix getter 20.
Step S11：One section of reaction tube 9 and second-stage reaction pipe 10 are installed in cartridge heater 8, pass through connecting sleeve and raw material
Gas bottle 6, hydrogen absorber 11, cooler 12 and product storage device 5 are connected.
Step S12：Cooling water water return tank 1 and cooling water are entered into water pot 2 by connecting tube with cooler 12 to be connected.
Step S13：System vacuumizes displacement.It specifically refer to shown in Fig. 5, comprise the following steps：
Step S20：Working gas (Krypton) or high-purity argon gas are filled with to 0.1~0.2MPa, displacement is vacuumized, repeats 2~3
It is secondary, to whole device inside be replaced completely it is clean.
Step S21：High-purity argon gas is filled with whole device to 0.1~0.2MPa, is ready for activation manipulation.
Step S14：System heating activation.It specifically refer to shown in Fig. 6, comprise the following steps：
Step S30：High purity inert gas (argon gas) pressure is 0.1~0.2Mpa in gas reaction section 16 and gas flows
In the state of, start semi-open type circular shape heater 15 and run, to the heat activation of gas reaction section 16, progressively make gas reaction section 16
It is warming up to 100 DEG C, 300 DEG C, 500 DEG C, 700 DEG C, 980 DEG C.
Step S31：Start to vacuumize in temperature stabilization to startup vavuum pump after 980 DEG C, continue more than 6~8 hours, activate
Finish.
Step S32：The high purity inert gas that is passed through of low discharge is needed in activation, ensures what getter 20 desorbed
Gas is carried out gas reaction section 16.
Step S15：It is passed through the krypton/xenon-133 gas for needing to purify.
Step S16：Gas reaction section 16 is down to 960 DEG C, is gradually passed through working gas (Krypton/xenon), purifier
Put into commencement of commercial operation.
Step S17：Krypton/xenon of purifier outlet is analyzed in the process of running, after purity qualified,
Filled in subsequent technique Krypton/xenon product gas on bottle stand and carry out the freezing of high-purity krypton/xenon-133 gas product and fill bottle operation.
The purifier for including the getter in hollow circular cylinder shape described using the present invention, preparation contain 200ppm
The Krypton of CF4 impurity, carry out life-cycle experiment using pilot-plant, reaction temperature is controlled at 850~950 DEG C, until exit
Containing CF4 more than 1ppm in the Krypton measured, it was demonstrated that getter saturation fails.Monitored in experimentation when air-flow passes through reaction tube
Resistance drop, does not find significantly raised, and experiment cuts one section of reaction tube and second-stage reaction pipe after terminating, and does not find that flow area blocks
Situation.The purifier of the getter for including hollow circular cylinder shape of this patent exploitation is efficiently solved inside reaction tube
The problem of flow area is blocked by ZRF4 crystalline particles, the data obtained through life-cycle pilot experiment, theoretical calculation reaction tube longevity
Life can extend to more than 2 years, by effective service life for extending reaction tube.
Embodiments of the present invention are these are only, are not intended to limit the scope of the invention, it is every to utilize the present invention
The equivalent structure or equivalent flow conversion that specification and accompanying drawing content are made, or directly or indirectly it is used in other related technologies
Field, it is included within the scope of the present invention.
Claims (9)
- A kind of 1. high-purity krypton/xenon-133 gas purifier, it is characterised in that including：Reaction tube, hydrogen absorber, cooler, accurate mistake Filter, product storage device, the reaction tube, hydrogen absorber, cooler, accurate filter and product storage device connect successively Connect, the reaction tube is located in heater, is provided with gas reaction section in the reaction tube, the both ends of the gas reaction section are all provided with There is stainless steel mesh layer, the stainless steel mesh interlayer is filled with getter, and the getter is polynary getter alloys powder The manufactured hollow circular cylinder in one end closing；The internal diameter of the getter is Ф 3.0mm~Ф 3.2mm, and external diameter is Ф 5.0mm ~Ф 5.2mm, length are 5.0mm~5.2mm.
- 2. high-purity krypton/xenon-133 gas purifier as claimed in claim 1, it is characterised in that：The conversion zone includes one section instead Section and second-stage reaction section are answered, bite type connection is carried out by steel pipe between one section of reaction tube and second-stage reaction pipe.
- 3. high-purity krypton/xenon-133 gas purifier as claimed in claim 1, it is characterised in that：Also include cooling water water return tank and Cooling water enters water pot, and the cooling water water return tank and cooling water enter water pot and be connected with cooler.
- 4. high-purity krypton/xenon-133 gas purifier as claimed in claim 1, it is characterised in that：The heater is justified for semi-open type Shape heater, the semi-open type circular shape heater include two through the hinged semicircle cartridge heater with heater strip.
- 5. high-purity krypton/xenon-133 gas purifier as claimed in claim 1, it is characterised in that：The internal diameter of the hollow circular cylinder Be set to R1, external diameter is set to R2, length is set to L, wherein external diameter R2 is equal to length L, and internal diameter R1 is less than external diameter R2.
- A kind of 6. side that high-purity krypton/xenon-133 gas is manufactured using purifier according to any one of claims 1 to 5 Method, it is characterised in that including：The manufactured getter in hollow circular cylinder is filled with reaction tube, the entrance of the gas reaction section and outlet filling are stainless Steel screen layer is to fix getter；High-purity Krypton or argon gas are filled with, and vacuumizes displacement；In gas reaction section high-purity Krypton or argon pressure be 0.1~0.2Mpa and gas flowing in the state of, start half-open Formula circular shape heater progressively makes gas reaction section heat up, and start to hold after the first temperature is reached to be heated to gas reaction section It is continuous to vacuumize；And carry out gas reaction section to be cooled to second temperature, and the Krypton or xenon that need to be purified gradually are passed through, with Krypton or xenon after to purification.
- 7. the method for high-purity krypton/xenon-133 gas is manufactured as claimed in claim 6, it is characterised in that：First temperature is taken the photograph for 980 Family name's degree.
- 8. the method for high-purity krypton/xenon-133 gas is manufactured as claimed in claim 6, it is characterised in that：The second temperature is taken the photograph for 960 Family name's degree.
- 9. a kind of manufacture method for the getter for being used for high-purity krypton/xenon-133 gas purifier as claimed in claim 1, its feature It is, including：The polynary getter alloys particle of melting under vacuum condition is clayed into power using fluidized bed jet mill；And using metal It is Ф 3.0mm~Ф 3.2mm that internal diameter, which is made, in getter power by injection molding powder metallurgy process, and external diameter is Ф 5.0mm~Ф 5.2mm, the hollow circular cylinder that one end that length is 5.0mm~5.2mm is closed.
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| CN201510671353.9A CN105271146B (en) | 2015-10-15 | 2015-10-15 | High-purity krypton/xenon-133 gas purifier and manufacture method, the manufacture method of getter |
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| CN201510671353.9A CN105271146B (en) | 2015-10-15 | 2015-10-15 | High-purity krypton/xenon-133 gas purifier and manufacture method, the manufacture method of getter |
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| CN106672926B (en) * | 2016-12-22 | 2019-02-19 | 南京华东电子真空材料有限公司 | A kind of inert gas purification device using evaporable air-absorbing agent |
| CN108408701B (en) * | 2018-04-18 | 2019-10-01 | 衢州杭氧特种气体有限公司 | A kind of krypton, the xenon technological process of production and its production line |
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| JPH03247503A (en) * | 1990-02-27 | 1991-11-05 | Mitsubishi Heavy Ind Ltd | Production of sulfuric acid |
| EP1052018A4 (en) * | 1997-10-14 | 2002-03-27 | Japan Energy Corp | Catalyst support, catalyst, reactor for hydrogenation reaction, and catalytic reaction method |
| BR112015007390A2 (en) * | 2012-10-08 | 2017-12-12 | Shell Int Research | biomass conversion system and method |
| CA2887170A1 (en) * | 2012-10-08 | 2014-04-17 | Joseph Broun Powell | Lignocellulosic biomass conversion |
| CN104310325B (en) * | 2014-10-24 | 2016-06-29 | 武汉钢铁(集团)公司 | Krypton, xenon-133 gas purification method and device |
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