CN104147928B - A kind of containing the quick minimizing technology of protium in hydrogen tritide isotope gas - Google Patents
A kind of containing the quick minimizing technology of protium in hydrogen tritide isotope gas Download PDFInfo
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- CN104147928B CN104147928B CN201410354818.3A CN201410354818A CN104147928B CN 104147928 B CN104147928 B CN 104147928B CN 201410354818 A CN201410354818 A CN 201410354818A CN 104147928 B CN104147928 B CN 104147928B
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- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 title claims abstract description 101
- 241000720974 Protium Species 0.000 title claims abstract description 101
- 239000007789 gas Substances 0.000 title claims abstract description 76
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 52
- 239000001257 hydrogen Substances 0.000 title claims abstract description 52
- 150000002431 hydrogen Chemical class 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 title claims abstract description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 53
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 36
- 238000011282 treatment Methods 0.000 claims abstract description 9
- 238000007689 inspection Methods 0.000 claims abstract description 6
- 238000012805 post-processing Methods 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 21
- 238000003795 desorption Methods 0.000 claims description 2
- 229910052722 tritium Inorganic materials 0.000 description 32
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 31
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 27
- 229910052805 deuterium Inorganic materials 0.000 description 24
- 239000012071 phase Substances 0.000 description 13
- 238000012545 processing Methods 0.000 description 10
- 230000005445 isotope effect Effects 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000011221 initial treatment Methods 0.000 description 2
- 238000005372 isotope separation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910000946 Y alloy Inorganic materials 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 230000008717 functional decline Effects 0.000 description 1
- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- UBQALOXXVZQHGR-UHFFFAOYSA-N palladium yttrium Chemical compound [Y].[Pd] UBQALOXXVZQHGR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Separation Of Gases By Adsorption (AREA)
Abstract
The invention provides a kind of containing the quick minimizing technology of protium in hydrogen tritide isotope gas, comprise the following steps successively: a, palladium are detained the leak rate inspection of method fall protium device, fill He to 1.5MPa, pressurize 60min；Pretreatment before b, purification；C, purified treatment；D, post processing.Use the present invention containing the quick minimizing technology of protium in hydrogen tritide isotope gas, it is possible to obtain low protium content containing hydrogen tritide isotope gas.
Description
Technical field
The invention belongs to hydrogen isotope processing technology field, it is specifically related to a kind of containing the quick minimizing technology of protium in hydrogen tritide isotope gas, the present invention for by protium content higher than the protium in 1% deuterium tritium gas carry out efficient, quickly remove, to obtain the protium content deuterium tritium gas less than 1%.
Background technology
The energy, economy and environment are the three big problems that mankind nowadays social sustainable development faces, and wherein, the energy is the basis of economy and environment sustainable development.Nuclear fission energy is the emerging energy occurred the sixties in last century, through the development of nearly over half a century, has the most had suitable scale.To 20 end of the centurys, global installed capacity has reached 430GW, and disintegration energy is 7% to the contribution of total energy.As not having coal or natural gas to be impossible to the electric power output of traditional power plants, complete deuterium tritium fuel circulation is not had to be impossible to the electric power output of fusion reactor yet.
For deuterium-tritium fusion reactor, in deuterium tritium fuel, equally content to protium has strict restriction, it is desirable to carrying out ash discharge gas dropping after protium decontamination processes can injection ring shape room, it is achieved deuterium tritium fuel closed circulation.
Up to now, have been developed in multiple hydrogen isotope separation method both at home and abroad, mainly include Clusius-Dickel column method (TD-Thermal
Diffusion Column), stepwise adsorption method (FS-Fractional Sorption), batch-type membranes, cryogenic fractionation (CS-Batch Cryogenic Still) etc..Wherein CS method is the hydrogen isotope separation technology that the separating power generally acknowledged at present is maximum, but piece-rate system volume is relatively big, is difficult to carry out secondary seal, runs and controls to require height.FS method separation efficiency is low, is eliminated.It is that place, U.S. tritium factory Sa Fanna river (SRS) was in invention in 1980 that TCAP (thermal cycle absorption method) separates the technology of hydrogen isotope, there is the advantages such as operating condition is gentle, separation purity is high, separating power is big, can be not only used for separating it can also be used to contain the purification of tritium waste gas, the enrichment of low concentration tritium gas of hydrogen isotope gas；If multiple TCAP are unit cascaded, it is also possible to be directly separated ternary hydrogen isotope gas.
Many metals or intermetallic compound (alloy) can occur reversible combination reaction with hydrogen, form metal hydride.One important feature is that these metal or alloy have isotope effect when forming hydride, and in the Hydrogen-metal system known to settled the present, the hydrogen isotope effect of palladium hydrogen system is the strongest.
The hydrogenation process of palladium is, hydrogen molecule, first by palladium surface adsorption, is dissociated into atom immediately, the atom Hydrogen Energy of palladium surface adsorption is dissolved in inside palladium metal as solute dissolves in solvent, forms so-called solid solution, when the hydrogen dissolved in is continuously increased, there will be phase transformation, form hydride phase.A phase therein is the face-centered cubic crystalline phase with different crystalline lattice parameter with β phase.Whether the formation of β phase, and one is relevant with H/Pd atomic ratio, and two is relevant with temperature.At a certain temperature, only H/Pd atomic ratio just there will be β phase after reaching certain value, and temperature is the lowest, occurs that the ratio of phase transformation is the least.When by a β inversion of phases in opposite directions, total H/Pd atomic ratio is changing, but gas phase pressure is basically unchanged, thus forms a pressure Ping Qu.
Different from hydrogen, deuterium tritium is after dissolving in palladium, and due to the difference of atomic mass, in lattice, residing energy state (ground state) is also different, and wherein the ground state level of tritium is the highest, next to that deuterium, hydrogen is minimum.The difference of energy state makes the macro-effect also difference of reaction: in terms of reaction heat, during hydrogenation, the heat of release is most, minimum time tritiated；In terms of inhaling/put hydrogen isothermal line, the pressure of tritium is the highest, and hydrogen is minimum.The These characteristics of palladium-hydrogen system is its hydrogen isotope effect.
The isotope effect of palladium-hydrogen system is also manifested by selective absorption and the release tendency of palladium.Palladium Preferential adsorption is hydrogen, next to that deuterium, is tritium again, and on the other hand, preferentially disengage when desorbing is tritium, next to that deuterium, is again only hydrogen.The hydrogen isotope effect of palladium-hydrogen system changes with temperature, and temperature is the highest, and isotope effect is the least, and the lowest isotope effect of temperature is the biggest.Such as, when temperature is relatively low, the relative difference of plateau pressure is very big, and rises high-temperature and will reduce this difference, i.e. existsβPhase time, separation factor along with temperature raise with exponential function decline, this conclusion be detained method fall protium device foundation provide theoretical basis.
When hydrogen isotope admixture of gas is absorbed by palladium, the hydrogen-absorption speed of palladium is not only fast than deuterium tritium, and the capacity that absorbs is the most slightly larger as a result, heavy hydrogen abundance ratio in the gas phase is original during adsorption equilibrium height, and absorption heavy hydrogen abundance in solid phase is then low than original.This means that heavy hydrogen (deuterium tritium) is concentrated in the gas phase, and light hydrogen (protium) is enriched with in solid phase, namely obtains a certain degree of separation between isotope.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of containing the quick minimizing technology of protium in hydrogen tritide isotope gas.
The present invention's is a kind of containing the quick minimizing technology of protium in hydrogen tritide isotope gas, comprises the following steps successively: a, palladium are detained the leak rate inspection of method fall protium device, fill He to 1.5MPa, pressurize 60min；Pretreatment before b, purification；C, purified treatment；D, post processing.
The leak rate value of the leak rate inspection in step a is less than 1.0 × 10- 9.Pa.m3.s-1。
The pretreatment before fall protium in step b comprises the following steps:
(1) method of being detained by palladium fall protium device is heated to 550 DEG C；
(2) with vacuum pump, fall protium device is evacuated to below 4Pa and maintains 60min；
(3) fall protium device is allowed to naturally cool to the various process valve of room temperature shutoff device.
Fall protium in step c processes and comprises the following steps:
(1) unstripped gas arrival end valve and the product gas receiving terminal valve of fall protium device are opened；
(2) at room temperature, allow and enter fall protium device containing hydrogen tritide isotope gas from unstripped gas arrival end；
(3) unstripped gas inlet port pressure controls between 0.2MPa-0.25MPa；
(4) product gas storage hydrogen bed absorbs；
(5), after fall protium is disposed, closes storage hydrogen bed valve and open storage hydrogen bed valve；
(6) adding heat drop protium device to 550 DEG C, the desorption gas being detained in fall protium device receives stores hydrogen bed；
(7), after desorbing, storage hydrogen bed valve is closed.
Fall protium in step d processes and comprises the following steps:
(1) under the constant temperature of 550 DEG C, fall protium device is evacuated to below 4Pa and maintains 60min；
(2) naturally cool to room temperature and close the various process valve of fall protium device.
The invention has the beneficial effects as follows the removal cycle shortening protium in deuterium tritium, simplify the removal technique of protium, reduce the running temperature of device, decrease seeping at high temperature and the Environment release of tritium, reduce the removal cost of protium in deuterium tritium gas, the fall protium easily realizing large-scale deuterium tritium gas processes, and the protium content in deuterium tritium gas can be reduced to less than 1% by fall protium technological parameter effectively that determine.
Detailed description of the invention
The present invention uses palladium to be detained method containing the quick minimizing technology of protium in hydrogen tritide isotope gas, and the main body of the method equipment therefor is provided with spiral helicine palladium yttrium alloys serpentine pipe.Its process system be mainly detained by palladium detached dowel, circulating tank, pressure transducer, valve, vacuum gauge, gas loop jump pump, vacuum pump, product receive bed, tail gas receive bed and data collecting system etc. constitute.Whole process system before use must be through helium mass spectrum leak detection, and leak rate is less than 1.0 10-9Pa.m3.s-1.Palladium be detained detached dowel be mainly used in deuterium tritium gas a small amount of protium reduction process；Circulating tank is mainly used in dropping the quantitatively calibrating processing tolerance in protium processing procedure；Pressure transducer is mainly used in dropping operating pressure in protium processing procedure and shows and control；Process system is mainly controlled by valve；Vacuum gauge is mainly used in the monitoring of process system vacuum；Gas loop jump pump is mainly used in dropping transfer and the supercharging of gas during protium；Vacuum pump is mainly used in the evacuation of process system and processes；Data collecting system is mainly used in dropping the Real-time Collection of data during protium.
The present invention containing the quick minimizing technology of protium in hydrogen tritide isotope gas, in turn include the following steps:
1), palladium is detained the method fall design of protium device and processing
The be detained main body of method fall protium device of palladium is that the palladiums of three cascades are detained separate palladium post, and each palladium separate palladium post of being detained is welded by stainless steel tube, all with palladium asbestos and the layering filling of pure palladium powder, makes each layer close with actual column length during filling as far as possible.Two ports of every post are all welded with sintered stainless steel filter, to prevent palladium powder from entering pipe-line system.The maximum compressive resistance of this device is 1.5MPa.Bed, tail gas reception bed is received including 1 raw material gas inlet, 1 product gas outlet, circulating tank, circulating pump, vacuum pump, product gas.
2) palladium be detained method fall protium device leak rate inspection
In order to be detained by the palladium made, method fall protium device accesses leak detection tool equipment, fills after He to 1.5MPa and pressurize 60min, and leak rate is less than 1.0 × 10- 9.Pa.m3.s-1。
3) palladium be detained method fall protium device fall protium before pretreatment
Method of being detained by palladium fall protium device is heated to 550 DEG C, after being evacuated to below 4Pa with vacuum pump and maintain 60min by fall protium device, allows fall protium device naturally cool to the various process valve of room temperature shutoff device, standby.
4) palladium is detained method fall protium device quickly processing protium a small amount of in deuterium tritium gas
At room temperature, by the deuterium tritium gas in surge tank from palladium be detained method fall protium device unstripped gas arrival end enter fall protium device, product gas receiving terminal absorbs with preactivated good storage hydrogen bed, when in product gas, protium is close to 1%, close product gas and receive bed valve, add heat drop protium device to 550 DEG C, allow and be trapped in the deuterium tritium gas (tail gas) that is enriched with of protium content in fall protium device and desorb and with other reception bed reception, higher driving force is had, it is necessary to use gas cycle supercharging device to maintain the gas-powered power of relative constancy in order to ensure fall protium device.
When in unstripped gas, protium content is higher than 2%, when initial treatment tolerance is 100L, after fall protium processes 6h, the protium content in product gas is 0.88%, and product gas is 54L, i.e. product gas extraction ratio is 54%；And when initial treatment tolerance is 75L, after purifying 6h, in product gas, protium content is 0.75%, and product gas is 49L, i.e. product gas extraction ratio is 65%.Result shows, at room temperature, the method has reducing effect fast and efficiently to protium a small amount of in deuterium tritium gas, and the protium content in product gas is less than 1%.Within the identical process time, the treatment scale the most general relatively existing palladium Hot swapping segregation apparatus of the fall protium processing means that the present invention obtains improves about 7 times, fall protium treatment temperature temperature is reduced to room temperature by 550 DEG C, the safety greatly improving plant running, the seeping at high temperature reducing tritium and Environment release.
5) palladium be detained method fall protium device post processing
After a small amount of protium is quickly removed in deuterium tritium gas, under the constant temperature of 500 DEG C, after being evacuated to below 4Pa with vacuum pump and maintain 60min by fall protium device, fall protium device is allowed to naturally cool to the various process valve of room temperature shutoff device.
Technical process major technique condition:
(1) leak detection medium: He-4 gas, purity: more than 99.999%.
(2) leak detection pressure: 1.5MPa(absolute pressure).
(3) pretreatment: be heated to 550 DEG C, is evacuated to below 4Pa and keeps 60min.
(4) palladium is detained method fall protium device quickly processing protium a small amount of in deuterium tritium gas: operating temperature is room temperature, and gas-powered power is not less than 0.2MPa(absolute pressure).
(5) palladium be detained method fall protium device post processing: at 550 DEG C, be evacuated to below 4Pa and maintain 60min.
The clean-up effect of hydrogen isotope purifier:
In using the present invention after pressurize leakage detecting process, it is ensured that the safety in use of this device；Pretreating process before protium device fall protium drops in method of being detained palladium, can effectively remove micro-moisture, oxygen, nitrogen and surface adsorption thing etc., it is ensured that in the fall protium processing procedure of follow-up deuterium tritium gas, avoiding device is poisoned and is reduced protium treatment effeciency；The fall protium obtained processes technological parameter can be reduced to less than 1% fast and efficiently by the protium in the protium content deuterium tritium unstripped gas higher than 2%；The treatment scale the most general relatively existing palladium Hot swapping segregation apparatus of the fall protium processing means obtained improves about 7 times, fall protium treatment temperature temperature is reduced to room temperature by 550 DEG C, the safety greatly improving plant running, the seeping at high temperature reducing tritium and Environment release.
Claims (4)
1. one kind containing the quick minimizing technology of protium in hydrogen tritide isotope gas, it is characterised in that comprise the following steps successively: a, palladium are detained the leak rate inspection of method fall protium device, fill He to 1.5MPa, pressurize 60min；Pretreatment before b, purification；C, purified treatment；D, post processing；Purified treatment in step c comprises the following steps:
(1) unstripped gas arrival end valve and the product gas receiving terminal valve of fall protium device are opened；
(2) at room temperature, allow and enter fall protium device containing hydrogen tritide isotope gas from unstripped gas arrival end；
(3) unstripped gas inlet port pressure controls between 0.2MPa-0.25MPa；
(4) product gas storage hydrogen bed absorbs；
(5), after fall protium is disposed, closes product and receive storage hydrogen bed valve and open tail gas reception storage hydrogen bed valve；
(6) adding heat drop protium device to 550 DEG C, the desorption gas tail gas being detained in fall protium device receives storage hydrogen bed and absorbs；
(7), after desorbing, close tail gas and receive storage hydrogen bed valve.
It is the most according to claim 1 containing the quick minimizing technology of protium in hydrogen tritide isotope gas, it is characterised in that: the leak rate value of the leak rate inspection in step a is less than 1.0 × 10- 9.Pa.m3.s-1。
It is the most according to claim 1 containing the quick minimizing technology of protium in hydrogen tritide isotope gas, it is characterised in that: the pretreatment before fall protium in step b comprises the following steps:
(1) method of being detained by palladium fall protium device is heated to 550 DEG C；
(2) with vacuum pump, fall protium device is evacuated to below 4Pa and maintains 60min；
(3) fall protium device is allowed to naturally cool to the various process valve of room temperature shutoff device.
It is the most according to claim 1 containing the quick minimizing technology of protium in hydrogen tritide isotope gas, it is characterised in that: the post processing in step d comprises the following steps:
(1) under the constant temperature of 550 DEG C, fall protium device is evacuated to below 4Pa and maintains 60min；
(2) naturally cool to room temperature and close the various process valve of fall protium device.
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| CN108962415B (en) * | 2017-05-23 | 2021-10-26 | 中国工程物理研究院材料研究所 | Method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride |
| CN108479393B (en) * | 2018-04-18 | 2020-07-31 | 中国工程物理研究院核物理与化学研究所 | Method for removing protium in gas containing tritium hydrogen isotope |
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