CN106838549A - A kind of Combined getter of safe absorbable nitrogen - Google Patents
A kind of Combined getter of safe absorbable nitrogen Download PDFInfo
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- CN106838549A CN106838549A CN201611194966.9A CN201611194966A CN106838549A CN 106838549 A CN106838549 A CN 106838549A CN 201611194966 A CN201611194966 A CN 201611194966A CN 106838549 A CN106838549 A CN 106838549A
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- Prior art keywords
- nitrogen
- getter
- active material
- safe
- combined
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L59/00—Thermal insulation in general
- F16L59/06—Arrangements using an air layer or vacuum
- F16L59/065—Arrangements using an air layer or vacuum using vacuum
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- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Thermal Insulation (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention is a kind of Combined getter of safe absorbable nitrogen, it includes absorbent material, oxidant and is imbedded in the openable sealing container of the inside of absorbent material or absorbent material and oxidant mixture, being placed with inside the container can be with the active material of nitrogen reaction generation solid matter, the active material is present with≤10 microns of form of film, after vacuum insulation panel exhaust sealing terminates, container inside getter is opened by external force, you can trouble free service.Advantage：On the one hand because steam cannot be contacted with active material, thus the H for being substantially increased vacuum thermal insulation board heat conductivity coefficient is not had2Produce, absorbed N2Active material also will not with steam reaction release ammonia.On the other hand due to few for absorbing the active material quantity of nitrogen, and exist in very thin film form, when vacuum insulation panel seal failure, its be completely with enter inside air reaction finish and make the potential safety hazard of recovery cutting operation to be zero.
Description
Technical field
The present invention relates to a kind of Combined getter of safe absorbable nitrogen, for that can not be heated above
The getter composition of dimension vacuum, the more particularly to application such as refrigerator, electric heater, freezer are improved and maintained in 200 DEG C of device
Vacuum insulation panel.
Background technology
Vacuum insulation panel in oil, chemical industry, building, refrigerator, insulation cooker etc. due to good effect of heat insulation, being incubated
Field is progressively widely used.The heat-proof quality of vacuum insulation panel depends primarily on the vacuum of inside and leading for core
Hot coefficient.
Infiltration, the outlet of core backing material, the envelope of vacuum in vacuum insulation panel and outer sealing material to air
The several respects such as residual gas during mouth are relevant.Getter is according to various combination, in addition to remaining Ar cannot be absorbed, Ke Yi
Thermal insulation board absorbed inside H2、H2O、CO、N2、O2、CO2, one or more in the common gas such as CmHn, it is adiabatic in vacuum insulation panel
The aspects such as performance and used life have indispensable important function.In vacuum insulation panel using getter have one it is most main
The feature wanted：Its sealing shell is a kind of aluminium plastic composite material, and it is not amenable to the temperature more than more than 200 DEG C, therefore early stage
The use of the technology of getter is all that getter is high in advance in an openable vacuum plant in vacuum heat-insulation intralamellar part
After temperature activation, sealing device is then broken at normal temperatures makes getter work.
Vial will be enclosed as disclosed in United States Patent (USP) 4938667 in 1989 after the getter alloy high-temperature activation such as zirconium vanadium iron
In, vacuum heat-insulation intralamellar part again breaking glass bottle.And the Chinese patent 92109722 of 1992 is disclosed equipped with barium-lithium
The surface encapsulation heat-shrinkable film of alloy vessel, heat-shrinkable film is ruptured in the heating of vacuum insulation intralamellar part, exposes activation
Good barium-lithium alloy.Again by core after the disclosed barium metal film that evapotranspired to core in vacuum system of Chinese patent 201310280994
Material is put into aluminium plastic composite material inner seal, and postscript Chinese patent 200610122872 in 2006 is disclosed by evaporable barium air-breathing
Vial is enclosed in agent, and high frequency is baked after disappearing and sealed, then in vacuum heat-insulation intralamellar part breaking glass bottle.
These are operations using the major defect of traditional evaporable, nonevaporable getter method in vacuum insulation panel
Cumbersome, production efficiency is not high, absorptive capacity is extremely limited, it is unobvious to reduce vacuum thermal insulation board heat conductivity coefficient.
Chinese patent 94191152,96109371,200510040388,201110112501,201280067762 and U.S.
State patent US2008/0272333 discloses another method, and it uses the water absorbing agents such as calcium oxide and metal oxide containing precious metals, mistake
The composition of metal oxide is crossed as Combined getter.The wherein water absorbing agent such as calcium oxide can absorb CO2、H2O, such as PdO
Metal oxide containing precious metals can be with CO, H2Reaction, and generate CO2And H2O, then absorbed by CaO.This kind of method substantially increases vacuum
Middle H2, CO infiltration rate and absorptive capacity.
As vacuum insulation panel getter technology develops, the selection of internal core and handling process are gradually improved, and core
Material selection and the improvement of handling process, core insulation effect in itself are become better and better, and at this moment, the heat conduction of vacuum insulation panel epidermis is just
A relatively important factor as influence vacuum insulation panel heat-insulating property, this is referred to as " Kelvin effect " in thermal insulation board field.
The epidermis of vacuum insulation panel is typically made of the composite for covering aluminium, and aluminum membranous layer is thicker, prevents the performance of gas infiltration better,
But Kelvin effect is more obvious.To reduce Kelvin effect, it is desirable to reduce the thickness of aluminium barrier layer so that vacuum insulation panel epidermis is to sky
The permeability of gas increases, and which increases the load of getter.On the other hand, the increasingly lower price of vacuum insulation panel, also forces
Vast thermal insulation board manufacturer improve production efficiency, shortens evacuation time, and this is also caused, remains in the N inside thermal insulation board2、O2
Increase.Therefore, it is effective to absorb N remaining in vacuum insulation panel2、O2It is a main target of getter development.Due to O2Tool
There is high activity, can easily by the absorption of prior art safety.
But because nitrogen has a very big inertia, thus to absorb nitrogen must could be by it using activity material very high
Absorb.The method that nitrogen is removed is mainly using barium-lithium alloy powder or evaporable barium getter at present.Such as China in 2006 specially
The method of the use evaporable barium getter disclosed in sharp Chinese patent 201310280994 in 200610122872,2013.This
Although a little methods can absorb nitrogen, there is a defect for maximum, barium metal can be with the generation hydrogen of the steam in thermal insulation board, and hydrogen
The thermal conductivity factor of gas is 8 times of nitrogen, does not play a part of not only so to reduce vacuum thermal insulation board heat conductivity coefficient, is improved on the contrary
The thermal conductivity factor of vacuum insulation panel, though in vacuum insulation panel the initial stage be not much moisture, barium metal and nitrogen, oxygen whole
Reaction is generated and nitrogenizes barium, barium monoxide, but gradually infiltration, release with steam, and nitridation barium will be with steam reaction generation ammonia
Gas, the effect that it reduces vacuum thermal insulation board heat conductivity coefficient is not obvious.
And these methods also have safety problem, since being come into force from European Union directive on WEEE, the electrical equipment of vacuum insulation panel has been used
It is that depositing dust needs to spray water smoke, it is necessary to electrical equipment is crushed when reclaiming operation.The method of above-mentioned use evaporable barium getter is produced
Even when exposed to also being difficult to all be finished with air reaction at once in air, such barium metal reacts raw excessive barium metal with water
The hydrogen of danger can be discharged.Although and the method for the use barium-lithium alloy that Chinese patent 92121883 is announced can eliminate water
The influence of vapour, but the aerial reaction speed of barium-lithium alloy powder that on the one hand it is used is slower, on the other hand because it compares
Surface area is smaller, it is necessary to using excessive barium-lithium alloy, so that its potential safety hazard existed when operation is reclaimed is more huge.
The content of the invention
Proposed by the present invention is a kind of Combined getter of safe absorbable nitrogen, and its purpose is intended to overcome existing skill
Drawbacks described above existing for art, can improve production efficiency, preferable absorptive capacity, substantially reduce vacuum thermal insulation board heat conductivity coefficient,
With obvious security performance.
Technical solution of the invention：A kind of Combined getter of safe absorbable nitrogen, it includes water-absorption material
Material, oxidant and be imbedded in absorbent material or absorbent material and oxidant mixture inside openable sealing container,
And being placed with inside the container can generate the active material of solid matter with nitrogen reaction, it is characterized in that：Can be anti-with nitrogen
The active material that solid matter should be generated is present with≤10 microns of form of film, when vacuum insulation panel exhaust sealing terminates
Afterwards, the container inside getter is opened by external force, you can trouble free service.
Advantages of the present invention：It is embodied in
1) oxidant can will diffuse into the H of getter in vacuum insulation panel2、O2, the gas such as CO, CmHn be oxidized to H2O、CO2；
CaO water absorbing agents are by H2O、CO2Absorb, only remaining N2Just further infiltrate through inside getter, it is anti-with active material therein
Should；
2) due in vacuum insulation panel residual gas first pass around the oxidant of outer layer, drier filtering, only N2And Ar can enter
One step is infiltrated through inside getter；
3) due to can be with N2The active material of reaction has huge specific surface area, N2Absorbed by active material immediately, and generated
Corresponding metal nitride；
4) Ar cannot be absorbed and be remained in vacuum insulation panel；
5) because steam cannot be contacted with active material, thus the H for being substantially increased vacuum thermal insulation board heat conductivity coefficient is not had2Produce
It is raw, absorb N2Active material also will not with steam reaction release ammonia；
6) reclaim cutting using vacuum insulation panel electric equipment when, due to few for absorbing the active material quantity of nitrogen, and
And exist in very thin film form, when vacuum insulation panel seal failure, air enters in 10 seconds of thermal insulation board, its be completely with
Finished into internal nitrogen, oxygen reaction and make the potential safety hazard of recovery cutting operation to be zero；
7) different from Chinese patent 200610122872, its presence for not requiring water absorbing agent and oxidant is so directly exposed to
The H of thermal insulation board internal residual2、H2O、CO、N2、O2、CO2, barium metal in CmHn, on the one hand due to by CO, CO2Deng gaseous contamination
And make the gulp capacity reduction to nitrogen, on the other hand it can produce substantial amounts of hydrogen and make the heat conduction of thermal insulation board with steam reaction
Coefficient is raised extremely.Also, substantial amounts of barium metal is evaporated in narrow glass tube, causes the film layer of barium very thick, even if big
Breaking glass pipe in gas, its barium film be also required to for quite a long time could completely with air reaction and disappear.Use such suction
After the vacuum insulation panel of gas agent runs into water when disassembling, the risk that there is generation hydrogen and explode；
8) also different from Chinese patent 201310280994, its presence for not requiring water absorbing agent and oxidant equally is equally existed
Security risk when the abnormal elevated problem of vacuum thermal insulation board heat conductivity coefficient meeting and Dismantlement, and when producing vacuum insulation panel
It requires to use special exhaust sealing equipment, it is impossible to which continuous production, production efficiency is low；
9) it is also different from Chinese patent 95193987, although its presence for requiring water absorbing agent and oxidant and having used absorption nitrogen
Active material, but the active material barium-lithium alloy of its absorption nitrogen for using exists in powder form.Such suction
Gas agent, even when exposed to 24h in air, barium-lithium alloy therein cannot also be finished with atmospheric reaction completely, be at this moment put into water
Also have substantial amounts of hydrogen to produce, therefore there is huge security risk in Dismantlement.On the other hand, the barium-lithium that it is used
Alloy is that in an open containers, it is taken out from original vacuum packaging bag, is fitted into vacuum insulation panel again to vacuum
Thermal insulation board vacuumizes and finishes, seals and terminate, the process in having to be chronically exposed to air, and its barium-lithium alloy surface is by air
In nitrogen, oxygen polluted, its pumping property has been lost a lot.And the barium-lithium alloy of the absorption nitrogen in the present invention be with≤
10 microns of form of film is present, and remains stored in vacuum environment, until vacuum insulation panel exhaust, sealing terminate just cruelly
It is exposed in nitrogen.Therefore huge, cleaning the surface of the barium-lithium alloy in the present invention, makes the present invention have much bigger absorption
The ability of nitrogen, to absorb the nitrogen of equal number, the amount of barium-lithium alloy used in the present invention only has the percent of its consumption
Two.Because amount less, surface area it is big, in 10 seconds of vacuum insulation panel seal failure, its can rapidly with nitrogen, oxygen in air
Reaction is complete, so as to avoid the generation of hydrogen.Therefore the present invention is safer in use, removal process.
Specific embodiment
A kind of Combined getter of safe absorbable nitrogen, it includes absorbent material, oxidant and is imbedded in suction
The openable sealing container of the inside of water material or absorbent material and oxidant mixture, and be placed with inside the container
Can be with the active material of nitrogen reaction generation solid matter.It is characterized in that：Can be with the active material of nitrogen reaction generation solid matter
Material is present with≤10 microns of form of film.
A kind of described Combined getter, absorbent material is selected or combined in calcium oxide, barium monoxide, molecular sieve.
A kind of described Combined getter, oxidant is transition metal oxide or their mixture, with particle chi
The very little powder type for being less than 500 μm is utilized.
A kind of described Combined getter is the weight ratio of oxidant, absorbent material from 100：1 to 1：100.
Described can select with the active material of nitrogen reaction generation solid matter from lithium metal, sodium, potassium, barium, calcium, strontium
Or combination, preferably barium-lithium alloy, barium is 1 with the atomic ratio of lithium：4.
Embodiment 1
Under the protection of high-purity argon gas, by the iron wire of 50 microns of diameter continuously across the liquation of barium-lithium alloy, make wire surface
Coat the barium-lithium alloy of about 6 microns of a layer thickness;The iron wire that barium-lithium alloy content is about 2mg is folded and fills in one and is easy to crush
A diameter of 6mm, length for 5cm glass tube and be evacuated to 1 × 10-3Pa is simultaneously sealed;In a length of 9cm, a width of 7cm
10g CaO and 1g Co are poured into breathable polyethylene bag film3O4Compound, be inserted into above-mentioned glass tube and seal.Finally
Sample is enclosed into Aluminum-plastic composite bag vacuum to preserve.
Embodiment 2
This example is the sample preparation for the existing public technology for contrasting.By barium-lithium alloy pig, ball milling is obtained average grain in argon gas
The powder that 150 microns of footpath;During above-mentioned 100mg powder is pressed into an opening diameter for the stainless steel disk of 12mm, separately in a diameter
1g Co first are pressed through in the stainless steel disk of 28mm3O4, the above-mentioned metal disk for having a 100mg barium-lithium alloys is then placed in, finally
4g CaO are added, and with 4 tons of pressure compacting, is finally enclosed Aluminum-plastic composite bag vacuum and is preserved.
Embodiment 3
This example is the suction nitrogen performance test of each getter after simulating vacuum insulation panel actual production process;By sample from plastic-aluminum
Taken out in complex pocket, be placed on 15min in atmospheric environment, be then sealing in constant volume method pumping property test system, it is evacuated to 1 ×
10-3Pa, and after keeping 30min, is filled with high pure nitrogen to 30Pa pressure, and observing system pressure declines and changes with time.Pressure
Decline about soon, illustrate that the speed of sample absorption nitrogen is about fast;Tested with embodiment 2 with embodiment 1 respectively, except that
Embodiment 1 just opens glass tube inside getter being filled with after high pure nitrogen.Acetonideexample 1 in 1min pressure just from
30Pa will be 0, and embodiment 2 arrives 1h, and pressure will be just 28Pa.
Embodiment 4
This example is simulation vacuum insulation panel removal process, to test the security performance of each getter.By sample from Aluminum-plastic composite bag
Middle taking-up, is placed on 30 seconds in atmospheric environment, is then placed in the beaker for fill 500ml running water.Respectively with embodiment 1 and in fact
The sample for applying example 2 is tested, except that embodiment 1 opens the glass tube inside getter in Aluminum-plastic composite bag,
Breathable polyethylene bag film is drawn with blade after taking out getter, so that the water energy in beaker is quickly entered inside getter.As a result
Embodiment 1 does not find the release of hydrogen in addition to observing the reaction of CaO and water, and embodiment 2 then observed barium-lithium alloy
With the vigorous reaction of water, substantial amounts of hydrogen is released.
Claims (7)
1. a kind of Combined getter of safe absorbable nitrogen, including absorbent material, oxidant and it is imbedded in water-absorption material
The sealing container of the unlatching of the inside of material or absorbent material and oxidant mixture, and be placed with inside the container can be with nitrogen
Solid/liquid/gas reactions generate the active material of solid matter, it is characterized in that：Can with nitrogen reaction generation solid matter active material be with
≤ 10 microns of form of film is present;After vacuum insulation panel exhaust sealing terminates, the appearance inside getter is opened by external force
Device, you can trouble free service.
2. the Combined getter of a kind of safe absorbable nitrogen according to claim 1, it is characterized in that absorbent material
Selected in calcium oxide, barium monoxide, molecular sieve or combined.
3. the Combined getter of a kind of safe absorbable nitrogen according to claim 1, it is characterized in that oxidant is
Transition metal oxide or their mixture, the powder type with particle size less than 500 μm are utilized.
4. the Combined getter of a kind of safe absorbable nitrogen according to claim 1, it is characterized in that oxidant, suction
The weight ratio of water material is from 100：1 to 1：100.
5. the Combined getter of a kind of safe absorbable nitrogen according to claim 1, it is characterized in that can be with nitrogen
The active material of reaction generation solid matter is selected or combined from lithium metal, sodium, potassium, barium, calcium, strontium.
6. the Combined getter of a kind of safe absorbable nitrogen according to claim 3, it is characterized in that oxidant will
The H of getter is diffused into vacuum insulation panel2、O2, CO, CmHn gas be oxidized to H2O、CO2；CaO water absorbing agents are by H2O、CO2Inhale
Receive, remaining N2Infiltrate through inside getter, reacted with active material therein.
7. the Combined getter of a kind of safe absorbable nitrogen according to claim 6, it is characterized in that can be with nitrogen
It is few for absorbing the active material quantity of nitrogen in the active material of reaction generation solid matter, and in very thin film form
In the presence of, when vacuum insulation panel seal failure, air enters in 10 seconds of thermal insulation board, its be completely with enter inside nitrogen, oxygen
Solid/liquid/gas reactions are finished and make the potential safety hazard of recovery cutting operation to be zero.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611194966.9A CN106838549A (en) | 2016-12-22 | 2016-12-22 | A kind of Combined getter of safe absorbable nitrogen |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611194966.9A CN106838549A (en) | 2016-12-22 | 2016-12-22 | A kind of Combined getter of safe absorbable nitrogen |
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| CN106838549A true CN106838549A (en) | 2017-06-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611194966.9A Pending CN106838549A (en) | 2016-12-22 | 2016-12-22 | A kind of Combined getter of safe absorbable nitrogen |
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| CN1945092A (en) * | 2006-10-23 | 2007-04-11 | 厦门高特高新材料有限公司 | Method for producing vacuum heat insulation plate for high temperature degasser |
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| CN103759098A (en) * | 2014-01-23 | 2014-04-30 | 吴丹淼 | Composite getter device for vacuum insulated panel and method for manufacturing composite getter device |
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| US20150021515A1 (en) * | 2012-12-10 | 2015-01-22 | Saes Getters S.P.A. | Non-evaporable getter alloys reactivable after exposure to reactive gases |
| CN105051442A (en) * | 2013-04-23 | 2015-11-11 | 松下知识产权经营株式会社 | Insulator including gas adsorbing material |
| CN105536686A (en) * | 2014-10-24 | 2016-05-04 | 三星电子株式会社 | Gas-adsorbing material and vacuum insulation material including the same |
| CN105570618A (en) * | 2015-12-10 | 2016-05-11 | 南京华东电子真空材料有限公司 | Combined type getter for improving hydrogen absorption performance |
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2016
- 2016-12-22 CN CN201611194966.9A patent/CN106838549A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1945092A (en) * | 2006-10-23 | 2007-04-11 | 厦门高特高新材料有限公司 | Method for producing vacuum heat insulation plate for high temperature degasser |
| US20140248452A1 (en) * | 2011-12-27 | 2014-09-04 | Saes Getters S.P.A. | Getter devices containing a combination of getter materials |
| CN103182297A (en) * | 2011-12-28 | 2013-07-03 | 北京有色金属研究总院 | Thin-film getter with high gas absorption performance and preparation method thereof |
| US20150021515A1 (en) * | 2012-12-10 | 2015-01-22 | Saes Getters S.P.A. | Non-evaporable getter alloys reactivable after exposure to reactive gases |
| CN105051442A (en) * | 2013-04-23 | 2015-11-11 | 松下知识产权经营株式会社 | Insulator including gas adsorbing material |
| CN103759098A (en) * | 2014-01-23 | 2014-04-30 | 吴丹淼 | Composite getter device for vacuum insulated panel and method for manufacturing composite getter device |
| CN105536686A (en) * | 2014-10-24 | 2016-05-04 | 三星电子株式会社 | Gas-adsorbing material and vacuum insulation material including the same |
| CN105570618A (en) * | 2015-12-10 | 2016-05-11 | 南京华东电子真空材料有限公司 | Combined type getter for improving hydrogen absorption performance |
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Application publication date: 20170613 |