CN108962415A - A kind of hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride - Google Patents
A kind of hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride Download PDFInfo
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- CN108962415A CN108962415A CN201710366458.2A CN201710366458A CN108962415A CN 108962415 A CN108962415 A CN 108962415A CN 201710366458 A CN201710366458 A CN 201710366458A CN 108962415 A CN108962415 A CN 108962415A
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- G—PHYSICS
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- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/007—Recovery of isotopes from radioactive waste, e.g. fission products
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- G—PHYSICS
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- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
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Abstract
The invention discloses a kind of hydrogen/deuterium methods in efficient depth recycling hydrogen/lithium deuteride, and this method comprises the following steps: 1) preparation of reaction system；2) the leak rate inspection of reaction unit；3) pretreatment of reactant；4) material mixes；5) hydrogen is released in heating；6) post-reaction treatment.The activator that wherein step 5) heating reaction step uses is selected from one of mesoporous silicon oxide SBA-15, mesoporous silica/aluminium oxide MCM-41, MCM-22, mesoporous TiO 2 or several for porous oxide.Method of the invention have it is easy to operate, it is low in cost, can be used for testing on a large scale, reaction temperature is lower, and the recovery efficiency of hydrogen isotope is high, and the residual quantity of hydrogen is small in product, and product composition is single and environmental-friendly, the advantages that convenient for processing.
Description
Technical field
The invention belongs to Application of Nuclear Technology fields, and in particular to hydrogen/deuterium side in a kind of efficient depth recycling hydrogen/lithium deuteride
Method.
Background technique
It is the important nuclear energy material of one kind and storage hydrogen (deuterium) material that hydrogen (deuterium), which changes lithium, is applied to nuclear chemistry and energy industry,
It needs to recycle hydrogen/deuterium therein under certain applications scene.But hydrogen (deuterium) change lithium thermal stability is very high, decomposition temperature reaches
To 850 DEG C, hydrogen/deuterium therein can not be recycled under mild conditions.The method that activator is added is generallyd use to hydrogen
(deuterium) is changed lithium and is activated, and decomposes it at a lower temperature and releases hydrogen/deuterium, achievees the purpose that recycling wherein hydrogen/deuterium gas.Mesh
Preceding to use two class materials as activator: one kind is another kind of for inorganic oxides such as silica for low-melting-point metal.Wherein eutectic
Point metal nearby can react with lithium hydride at 400 DEG C and release hydrogen, but its problem is that the product reacted is the conjunction of lithium
Gold, hydrogen are easily detained in a metal, cause difficulty to the depth recycling of hydrogen in this way.The inorganic oxides such as silica are common hydrogenation
The activator that lithium decomposes, remaining hydrogen amount is smaller in reaction product, but the temperature reacted completely is higher (690 DEG C or more).It compares
Two kinds of materials, for from hydrogen (deuterium) change lithium in depth recycle hydrogen/deuterium, inorganic oxide be preferably select, but how further
It reduces reaction temperature and improves the difficult point that the rate of recovery is this method.
Therefore, the present invention provides a kind of hydrogen/deuterium methods in efficient depth recycling hydrogen/lithium deuteride.Unexpectedly, should
Method can make hydrogen/lithium deuteride release hydrogen/deuterium at a lower temperature, and hydrogen/deuterium rate of recovery may be up to 99.5% with
On.
Summary of the invention
The problem of recycling hydrogen/deuterium in hydrogen/lithium deuteride for the prior art, the purpose of the present invention is to provide one
Kind efficiently depth can recycle hydrogen/deuterium method at a lower temperature.
The technical solution adopted by the invention is as follows:
A kind of hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride, including using porous oxide as activator and
The step of hydrogen/lithium deuteride reaction, recycling hydrogen/deuterium.
Hydrogen/deuterium method in above-mentioned efficient depth recycling hydrogen/lithium deuteride, is first heated to 400~500 for porous oxide
DEG C, 0.5~1h is roasted, is uniformly mixed after cooling with hydrogen/lithium deuteride, hydrogen/deuterium is released in heating, recycles hydrogen/deuterium.
First porous oxide heat pre-treatment is conducive to remove impurity therein, impurity content in the gas after making reaction
It reduces.
Hydrogen/deuterium method in above-mentioned efficient depth recycling hydrogen/lithium deuteride, the porous oxide and hydrogen/lithium deuteride heat
Releasing hydrogen/deuterium temperature is 300~620 DEG C.
Make the prior art of activator with oxide, the complete reaction temperature of oxide and lithium hydride typically at least needs height
Up to 690 DEG C or more, the present inventor has been surprisingly found that porous oxide can reduce reaction energy barrier, and then at a lower temperature
Start to react, especially in conjunction with the pretreatment of porous oxide, effect highly significant.The adoptable low temperature model of the method for the present invention
Enclosing art methods can not react completely, and at a high temperature of identical, the method for the present invention is reacted faster, time-consuming shorter and same
When ensure that the purity of gas reclaiming rate and gas, the rate of recovery are up to 99.5% or more.
Hydrogen/deuterium method in above-mentioned efficient depth recycling hydrogen/lithium deuteride, the porous oxide are selected from mesoporous silicon oxide
One or more of SBA-15, mesoporous silica/aluminium oxide MCM-41, MCM-22, mesoporous TiO 2, it is preferably mesoporous
Silica.
It is preferred that the density of the porous oxide is less than 1g/cm3。
Hydrogen/deuterium method in above-mentioned efficient depth recycling hydrogen/lithium deuteride, specifically includes the following steps:
1) design of reaction unit and integrated: reaction unit includes vacuum pump 1, high-purity argon gas device 2, flow through reactors
3, pressure sensor 4, uranium bed 5, gas standard tank 6 and gas-chromatography 7 pass through valve according to conventional connection type between each device
It is connected with stainless steel pipes；
2) leak rate of reaction unit is examined: after system is evacuated to 2Pa by vacuum pump 1, being filled helium to 1.5MPa and is protected
Press 1h；
3) material pre-treatment: porous oxide is heated to 400~500 DEG C, high-temperature roasting 0.5-1h；
4) material mixes: by 3) processing and porous oxide after cooling is uniformly mixed with lithium hydride, the lithium hydride
Content is 5%-85wt%；
5) hydrogen/deuterium is released in heating: the mixture in step 4) being placed in flow through reactors 3 simultaneously access system, will be reacted
After system pump down to 2Pa or less, reactor is heated to 300~620 DEG C；
6) post-reaction treatment: hydrogen/deuterium gas volume in meter gaseous standard can 6, and gas is analyzed using gas-chromatography 7
Gas, is then recycled in uranium bed 5 for use by composition.
The flow through reactors 3 are made of stainless steel outer envelope, dust filter unit, heater and temperature thermocouple, bed
Body is sealed using flange-type structure.The uranium bed 5 is made of outer envelope, dust filter unit, heater and temperature thermocouple, bed body
Using full soldering and sealing structure, uranium particle is encapsulated in bed, granularity is 20~80 mesh, the hydrogen isotope gas generated for absorbing reaction
Body.The gas standard tank 6 is integrated the cylindric rustless steel container that product is 2L, for carry out the temporary of hydrogen isotope gas and
Volume metering, when device is run, standard can one end is connected to pressure sensor, and tank internal pressure can be observed in real time by pressure sensor
Power situation of change, pressure sensor 4 records the pressure of gas, until when pressure value no longer changes, it is believed that reaction terminates.The height
Straight argon device of air 2 is used to provide carrier gas for gas-chromatography 7 and purging system is used.These above-mentioned equipment can pass through conventional commercial
Approach obtains.
Some specific embodiments according to the present invention, above-mentioned steps 2) reaction unit leak rate examine, it is desirable that leak rate is less than
1.0×10-9·Pa·m3·s-1。
Some specific embodiments according to the present invention, above-mentioned steps 3) in air, nitrogen, argon atmosphere or vacuum condition
Under roasted, preferably roast in air.
Hydrogen/deuterium method in above-mentioned efficient depth recycling hydrogen/lithium deuteride, step 3) further includes being crushed to porous oxide
1nm-50μm。
Hydrogen/deuterium method in above-mentioned efficient depth recycling hydrogen/lithium deuteride, can be powder after the material mixing of step 4)
Shape, can also be with tabletting.Some embodiments of the present invention are packed into reactor after mixture is pressed into sheet.
The material of step (4) mixing as a preferred technical solution, the content of the hydrogen/lithium deuteride are 20%-
40wt.%.The effect and recovery efficiency of reaction can be combined under the content ratio.
Step (4) heating as a preferred technical solution, is released in hydrogen/deuterium, and reactor is heated to 400-610 DEG C.
Hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride provided by the invention, by rationally utilizing porous oxidation
Object, the specific surface area for increasing reactant, the particle size for reducing reactant significantly reduce reaction energy barrier, to reach reduction reaction
The effect of temperature makes lithium hydride release hydrogen at a lower temperature, and the initial temperature of reaction temperature even can be down to 300
DEG C, and art methods hardly happen reaction at such a temperature, need to start to react at 510 DEG C or more, such improvement
Effect is many-sided all with significant advantage in energy consumption, safety, cost etc..Specifically, method of the invention has with following
Beneficial effect:
1) operation of the present invention is simple, low in cost, can be used for testing on a large scale；
2) porous oxide density used in this method is suitable with hydrogen (deuterium) change lithium, and has very big specific surface area, has
Higher reactivity, reaction temperature is low, and hydrogen/deuterium recovery efficiency is high；
3) hydrogen/deuterium residual quantity is small in the product of this method, and composition is single and environmental-friendly, convenient for processing.
Detailed description of the invention
Fig. 1 is hydrogen/deuterium schematic device in depth recycling hydrogen/lithium deuteride of the present invention；Vacuum pump 1, high-purity argon gas device
2, flow through reactors 3, pressure sensor 4, uranium bed 5, gas standard tank 6, gas-chromatography 7, each device is by figure valve and not
The steel conduit that becomes rusty connects；
Fig. 2 is the XRD spectrum of raw mixture in the embodiment of the present invention 1；
Fig. 3 is the XRD spectrum of reaction product in the embodiment of the present invention 1；
Fig. 4 is the relational graph that raw material releases the deuterium pressure and reaction temperature that discharge during deuterium in the embodiment of the present invention 1；
1 is Temperature-time change curve, and 2 be deuterium pressure-time changing curve, and 300 DEG C or so mixtures start to react, and
The burst size of deuterium increases (deuterium pressure increase) as the temperature rises, and reaction rate is very fast, reaction to 600 DEG C nearby when, reaction
It is nearly completed.
Specific embodiment
Below it is only the present invention preferably some embodiments, this should not be interpreted as to the range of the above-mentioned theme of the present invention
It is only limitted to example below.All technologies realized based on above content of the present invention belong to the scope of protection of the invention.
Embodiment 1
Mounting device referring to Fig.1, will fill He to 1.5MPa and pressure maintaining 1h after system pump down to 2Pa, leak detection to leak rate is less than
1.0×10-9·Pa·m3·s-1It is stand-by afterwards.By mesoporous silicon oxide SBA-15, (density is less than 1g/cm3) add in air atmosphere
Heat is crushed to 100nm or less to 500 DEG C, high-temperature roasting 0.5h.By the mesoporous silicon oxide SBA-15 and lithium deuteride after roasting
It uniformly mixes, mixture is pressed by sheet with 25Mpa pressure under conditions of nitrogen protection and is packed into anti-according to 64:36 weight ratio
Answer device.2Pa, which is evacuated to, by reactor access system and by system starts to decompose to give off deuterium hereinafter, being heated to 300 DEG C of lithium deuterides
Gas.The deuterium of decomposition is stored to gas standard tank, using the pressure of pressure sensor record gas, until pressure value no longer becomes
When change (600 DEG C), it is believed that reaction terminates.It is using the composition of chromatography gas and gas collection is stand-by to uranium bed.It collects
Gas composition is as shown in table 1, and the deuterium of recycling is very pure.The XRD of reacting material mixture and product is respectively such as Fig. 2,3 institutes
Show, calculates the deuterium rate of recovery by theoretical value and be greater than 99.5%.Fig. 4 is the pass that raw material releases the deuterium pressure and reaction temperature that discharge during deuterium
System's figure.
Gas composition and content after the reaction of table 1
| Gas component | D2 | O2 | N2 | CH4 | CO |
| Content | 99.95% | <30ppm | <30ppm | <50ppm | <50ppm |
Using identical device, conventional spherical silicon dioxide is used to carry out according to a conventional method as activator, in above-mentioned temperature
The lower reaction of degree can not carry out.Initial reaction temperature is 510 DEG C, and at 600 DEG C, reaction is remained unfulfilled.Under the same terms, 600
DEG C when, spherical silicon dioxide is only 60% as the system deuterium rate of recovery of activator.
Embodiment 2
He to 1.5MPa and pressure maintaining 1h will be filled after system pump down to 2Pa, leak rate is less than 1.0 × 10-9·Pa·m3·s-1Afterwards
For use.By mesoporous silica/aluminium oxide MCM-41, (density is less than 1g/cm3) it is heated to 450 DEG C in air atmosphere, high temperature
0.5h is roasted, and is crushed to 100nm or less.By the mesoporous silica after roasting/aluminium oxide MCM-41 and lithium deuteride according to 79:
21 weight ratios uniformly mix, and mixture is pressed into sheet with 25Mpa pressure under conditions of nitrogen protection and is packed into reactor.It will
System is simultaneously evacuated to 2Pa hereinafter, being heated to 350 DEG C or more, lithium deuteride starts to decompose to give off deuterium by reactor access system.
The deuterium of decomposition is stored to gas standard tank, using the pressure of pressure sensor record gas, until pressure value no longer changes
When (600 DEG C), it is believed that reaction terminate.It is using the composition of chromatography gas and gas collection is stand-by to uranium bed.The gas of collection
As shown in table 2, the deuterium of recycling is very pure for body composition, calculates deuterium rate of recovery > 99.5% by theoretical value.
Gas composition and content after the reaction of table 2
| Gas component | D2 | O2 | N2 | CH4 | CO |
| Content | 99.95% | <30ppm | <30ppm | <50ppm | <50ppm |
Using identical device, under same reaction temperature, use conventional spherical silicon dioxide as activator routinely
Method carries out releasing deuterium alpha reaction, and the present embodiment method initial reaction temperature is lower, and reaction rate is fast, at 600 DEG C, spherical titanium dioxide
Silicon is 60% as the system deuterium rate of recovery of activator.
Embodiment 3
He to 1.5MPa and pressure maintaining 1h will be filled after system pump down to 2Pa, leak rate is less than 1.0 × 10-9·Pa·m3·s-1Afterwards
For use.By mesoporous silicon oxide SBA-15, (density is less than 1g/cm3) it is heated to 500 DEG C in air atmosphere, high-temperature roasting
0.5h, and it is crushed to 100nm or less.Mesoporous silicon oxide SBA-15 lithium hydride after roasting is uniform according to 60:40 weight ratio
Mixing, is pressed into sheet for mixture with 25Mpa pressure under conditions of nitrogen protection and is packed into reactor.Reactor is accessed and is
It unites and system is evacuated to 2Pa hereinafter, being heated to 330 DEG C or more, lithium hydride starts to decompose to give off hydrogen.By the hydrogen of decomposition
Storage is to gas standard tank, using the pressure of pressure sensor record gas, until recognizing when pressure value no longer changes (610 DEG C)
Terminate for reaction.It is using the composition of chromatography gas and gas collection is stand-by to uranium bed.The gas composition of collection such as 3 institute of table
Show, the hydrogen of recycling is very pure, calculates hydrogen retrieval rate > 99.5% by theoretical value.
Gas composition and content after the reaction of table 3
| Gas component | H2 | O2 | N2 | CH4 | CO |
| Content | 99.95% | <30ppm | <30ppm | <50ppm | <50ppm |
Using identical device, under same reaction temperature, use conventional spherical silicon dioxide as activator routinely
Method carries out releasing hydrogen reaction, and the present embodiment method initial reaction temperature is lower, and reaction rate is fast, at 610 DEG C, spherical titanium dioxide
Silicon is 57% as the system hydrogen retrieval rate of activator.
Claims (10)
1. a kind of hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride, which is characterized in that including using porous oxide as
The step of activator is reacted with hydrogen/lithium deuteride, recycles hydrogen/deuterium.
2. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 1, which is characterized in that first will be more
Orifice oxide is heated to 400~500 DEG C, roasts 0.5~1h, uniformly mixes after cooling with hydrogen/lithium deuteride, and hydrogen/deuterium is released in heating, is returned
Receive hydrogen/deuterium.
3. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 1, which is characterized in that described more
It is 300~620 DEG C that hydrogen/deuterium temperature is released in orifice oxide and hydrogen/lithium deuteride heating.
4. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 1, which is characterized in that described more
Orifice oxide is selected from mesoporous silicon oxide SBA-15, mesoporous silica/aluminium oxide MCM-41, MCM-22, mesoporous TiO 2
One or more of, preferably mesoporous silicon oxide.
5. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 1, which is characterized in that described more
The density of orifice oxide is less than 1g/cm3。
6. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 1, which is characterized in that specific packet
Include following steps:
1) design of reaction unit and integrated: reaction unit includes vacuum pump (1), high-purity argon gas device (2), flow through reactors
(3), pressure sensor (4), uranium bed (5), gas standard tank (6) and gas-chromatography (7), according to conventional connection side between each device
Formula is connected by valve with stainless steel pipes；
2) leak rate of reaction unit is examined: after system is evacuated to 2Pa by vacuum pump (1), filling helium to 1.5MPa and pressure maintaining
1h；
3) material pre-treatment: porous oxide is heated to 400~500 DEG C, high-temperature roasting 0.5-1h；
4) material mixes: by 3) processing and porous oxide after cooling is uniformly mixed with hydrogen/lithium deuteride, the hydrogen/lithium deuteride
Content be 5%-85wt%, preferably 20%-40wt.%；
5) heating release hydrogen/deuterium: the mixture in step 4) is placed in flow through reactors 3) in and access system, by reaction system
After being evacuated to 2Pa or less, reactor is heated to 300~620 DEG C, is preferably heated to 400-610 DEG C；
6) post-reaction treatment: hydrogen/deuterium gas volume in meter gaseous standard can (6), and gas is analyzed using gas-chromatography (7)
Gas, is then recycled in uranium bed (5) for use by composition.
7. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 6, which is characterized in that above-mentioned step
The leak rate of rapid 2) reaction unit is examined, it is desirable that leak rate is less than 1.0 × 10-9·Pa·m3·s-1。
8. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 6, which is characterized in that above-mentioned step
It is rapid 3) to be roasted under air, nitrogen, argon atmosphere or vacuum condition, preferably roast in air.
9. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 6, which is characterized in that step 3)
It further include that porous oxide is crushed to 1nm-50um.
10. hydrogen/deuterium method in efficient depth recycling hydrogen/lithium deuteride according to claim 6, which is characterized in that step
It 4) is powdered or tabletting after material mixing.
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