CN106957045B - A method of recycling hydrogen isotope from hydrogen isotope lithiumation object - Google Patents
A method of recycling hydrogen isotope from hydrogen isotope lithiumation object Download PDFInfo
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Abstract
The method that the invention discloses a kind of to recycle hydrogen isotope from hydrogen isotope lithiumation object, when purpose is to solve to extract from lithium tritide and recycle tritium, heat resolve need to be at 700 DEG C or more, and tritium is mentioned in the thermal decomposition for carrying out lithium tritide in lithium-aluminium alloy and then needs to control between 530 DEG C ~ 630 DEG C, and gas-solid exchange process detritiation then needs 580 DEG C or more of problem.It includes the following steps：Under protective atmosphere, hydrogen isotope lithiumation object, magnesium diboride are mixed, and mixture carried out hydrogen abstraction reaction, obtains inhaling hydrogen product；Hydrogen product will be inhaled again and carries out hydrogen release processing, and hydrogen isotope is realized by hydrogen discharge reaction and is recycled.Operation of the present invention temperature is low, the time is short; for durings the recycling of hydrogen isotope, extraction, removing etc.; reduce the seepage loss of hydrogen isotope; improve safety coefficient; and the protection for environment; promote the development and application of hydrogen isotope fuel technology, have important practical significance and improve meaning.
Description
Technical field
The present invention relates to the recycling of the extraction of hydrogen isotope and recycling field, especially hydrogen isotope, it is specially a kind of from
The method of hydrogen isotope is recycled in hydrogen isotope lithiumation object.The present invention can be used in time of hydrogen isotope in hydrogen isotope lithiumation object
It receives, is intended especially for6Li produces tritium（Elemental lithium can be broadly divided into6Li and7Li is general to use6Li produces tritium）It is realized from lithium tritide afterwards
Extraction, recycling and the removal for remaining tritium of tritium（Provide it is a kind of can under cryogenic, from lithium tritide extract, recycle tritium
Method）, have the advantages that simple process, effect are obvious, temperature is low.Hydrogen isotope therein is protium（H）, deuterium（D）, tritium（T）
It is one or more.
Background technique
With the worsening shortages of natural resources, the exacerbation of increase and the environmental pollution of energy consumption, cleaning is reliable, can
The regenerated energy has become whole world focus of attention.Based on fusion energy caused by deuterium, tritium fusion have release energy it is huge,
The advantages that fuel source is abundant and low-activity, has been considered as the major way of the human future acquisition energy.International Thermonuclear is real
Test reactor（ITER）As foremost fusion reaction device in the world, at present just by European Union, the U.S., Russia, China, day
Originally, South Korea and seven side of India carry out joint construction, are exactly based on burning deuterium tritium plasma and release huge energy.
Fuel of the tritium as fusion energy can be by fusion reaction although it there's almost no in nature
Son and lithium reaction, to realize the production of tritium.However, extraction and recycling how simple, that safely realize tritium, then be that fusion energy can
Sustainable development needs issues that need special attention.
When the metal of neutron and lithium, alloy or compound react, after generating tritium, tritium is easy in the form of lithium tritide
In the presence of, and how to extract and recycle tritium from lithium tritide then becomes particularly important.
If at least needing to be heated to 700 DEG C or more, tritium could be significantly from tritium using the method for directly heating decomposition
Change and is released in lithium.If the thermal decomposition for carrying out lithium tritide in lithium-aluminium alloy mentions tritium, temperature need to generally be controlled 530
DEG C ~ 630 DEG C between.And when carrying out the tritium in electrolytic recovery lithium tritide in halide lithium salts, it is also desirable to by temperature control molten
500 DEG C of salt temperature.At the same time, for having completed to mention the tritiated waste of tritium, it usually needs pass through depth detritiation, just can be carried out
The processing of latter step.Currently, common hydrogen isotope gas-solid exchange process detritiation at least needs to complete at 580 DEG C or more.Phase
It is as follows to close bibliography：Jiang Guoqiang, Luo Deli, landblink reach, engineering technology [M] first edition of Sun Ling rosy clouds tritium and tritium, Beijing：
National Defense Industry Press, 2007；Li Guanxing, Wusheng nuclear fuel [M] first edition, Beijing：Chemical Industry Press, 2007.
Since at 450 DEG C or more, scattering and permeating of the tritium in the materials such as stainless steel is very serious, therefore, excessively high
Temperature will increase the seepage loss of tritium, and be unfavorable for the security protection and environmental protection of tritium.If the recycling of tritium in lithium tritide mentions
It takes, remove and can operate at low temperature, safety coefficient can not only be improved, reduce the osmosis pollution of tritium, moreover it is possible to extend and place production tritium target
The service life of part crucible.For this purpose, the present invention provides a kind of method for recycling hydrogen isotope from hydrogen isotope lithiumation object.
Summary of the invention
Goal of the invention of the invention is：For tritium is extracted and recycled from lithium tritide, the temperature of heat resolve need to be 700
DEG C or more, and in lithium-aluminium alloy carry out lithium tritide thermal decomposition mention tritium then need by temperature control 530 DEG C ~ 630 DEG C it
Between, and the problem at 580 DEG C or more is then needed using gas-solid exchange process detritiation, one kind is provided and is recycled from hydrogen isotope lithiumation object
The method of hydrogen isotope.The present invention can effectively solve the excessively high problem of existing method operation temperature, and it is easy to operate, effect is bright
Aobvious, low operation temperature, time are short, for reducing hydrogen isotope durings the recycling of hydrogen isotope, extraction, removing etc.
Seepage loss improves safety coefficient, and the protection for environment, promotes the development and application of hydrogen isotope fuel technology, has
Important realistic meaning and progress meaning.
To achieve the goals above, the present invention adopts the following technical scheme that：
A method of it recycling hydrogen isotope from hydrogen isotope lithiumation object, includes the following steps：
（1）Under protective atmosphere, hydrogen isotope lithiumation object, magnesium diboride are mixed, the first mixture is obtained；
（2）First mixture is subjected to hydrogen abstraction reaction, obtains inhaling hydrogen product；
（3）The resulting suction hydrogen product of step 2 is subjected to hydrogen release processing, and hydrogen isotope is realized back by hydrogen discharge reaction
It receives；
（4）Step 2,3 are repeated, the hydrogen isotope in the atmosphere discharged when hydrogen release processing no longer containing recycling in need is
Only.
In the hydrogen isotope lithiumation object, hydrogen isotope is protium（H）, deuterium（D）, tritium（T）It is one or more.
In the step 1, the molar ratio of hydrogen isotope lithiumation object and magnesium diboride is 2：1~10.
In the step 1, hybrid mode is grinding or ball milling.
In the step 1, protective atmosphere is inert gas or hydrogen.
The inert gas is helium or argon gas.
In the step 2, the temperature of hydrogen abstraction reaction is 200 ~ 450 DEG C, and the Hydrogen Vapor Pressure of hydrogen abstraction reaction is 1 ~ 10 MPa.
In the step 3, the temperature of hydrogen discharge reaction is 250 ~ 500 DEG C, and the Hydrogen Vapor Pressure of hydrogen discharge reaction is 0 ~ 0.4 MPa.
For foregoing problems, the present invention provides a kind of method that hydrogen isotope is recycled from hydrogen isotope lithiumation object.This hair
It is bright to can effectively solve operation temperature higher problem when recycling, extract from hydrogen isotope lithiumation object, removing hydrogen isotope, tool
There is the advantages of simple method, significant effect, low operation temperature.Using the present invention, be conducive to the recycling in hydrogen isotope, extraction,
During removing etc., the seepage loss of hydrogen isotope is reduced, improves safety coefficient and the protection to environment, for promoting hydrogen same
The development and application of the plain fuel technology in position, have great importance.
This method comprises the following steps.
（1）Prepare the first mixture
Firstly, hydrogen isotope lithiumation object, magnesium diboride are mixed according to the ratio, obtain the first mixture in protective atmosphere.
Wherein, hydrogen isotope includes protium（H）, deuterium（D）, tritium（T）It is one or more, can using grinding or ball milling by the way of be mixed
It closes, protective gas used by protective atmosphere is inert gas or hydrogen.Preferably, hydrogen isotope lithiumation object and magnesium diboride
Molar ratio be 2：1~10.
（2）Hydrogen abstraction reaction
The first obtained mixture is subjected to hydrogen abstraction reaction, obtains inhaling hydrogen product.
（3）Hydrogen release processing
Obtained suction hydrogen product is subjected to hydrogen discharge reaction, hydrogen isotope can be realized by hydrogen discharge reaction and be recycled.
Repeat step（2）, step（3）, until the hydrogen in the atmosphere discharged when hydrogen release processing no longer containing recycling in need is same
Position element.In the application, the temperature of hydrogen abstraction reaction is 200-450 DEG C, and the Hydrogen Vapor Pressure of hydrogen abstraction reaction is 1-10 MPa；Hydrogen discharge reaction
Temperature be 250-500 DEG C, the Hydrogen Vapor Pressure of hydrogen discharge reaction is 0-0.4 MPa.
It can effectively be recycled from hydrogen isotope lithiumation object using the present invention by actual verification, extract, go dehydrogenation same
Position element, and effectively solve the problems, such as that existing method operation temperature is high.Compared with prior art, the present invention has simple process, effect
The feature that fruit is obvious, low operation temperature, time are short, is conducive to reduce hydrogen during recycling, extraction, removing of hydrogen isotope etc.
The seepage loss of isotope improves safety coefficient and environmental protection, for promoting the development and application of hydrogen isotope fuel technology,
With important progress meaning.
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is the XRD spectrum distinguished upon mixing, after hydrogen release, after hydrogen release, after hydrogen release in embodiment 1,1,2,4；
Hydrogen-sucking amount time history plot when Fig. 2 is hydrogen abstraction reaction in embodiment 1；
Hydrogen-sucking amount time history plot when Fig. 3 is hydrogen abstraction reaction in embodiment 2；
Fig. 4 is the XRD spectrum of reaction product in embodiment 2 after hydrogen abstraction reaction；
Hydrogen desorption capacity time history plot when Fig. 5 is hydrogen discharge reaction in embodiment 2；
The curve graph that hydrogen desorption capacity varies with temperature when Fig. 6 is hydrogen discharge reaction in embodiment 3.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.
Embodiment 1
In the glove box filled with argon gas, by 1:1 molar ratio weighs two kinds of raw material powders of lithium deuteride and magnesium diboride,
In the ball grinder for entering the stainless steel material that volume is 100 ml, and under an argon, with 2 h of planetary ball mill ball milling, carry out
Mechanical mixture processing, obtains the first mixture, XRD spectrum such as Fig. 1（a）It is shown.
After the first mixture that ball milling is obtained is packed into reaction kettle, it is vacuumized, then reaction kettle is placed in heating furnace,
And reaction kettle is heated to 400 DEG C；Then, it is quickly filled with the hydrogen that purity is 99.99% into reaction kettle to 6 MPa, carries out suction hydrogen
15 min are reacted, hydrogen abstraction reaction curve is as shown in Figure 2.It can be seen in fig. 2 that carrying out 10 min or so in reaction, hydrogen is inhaled with regard to base
This completion.Later, the temperature of reaction kettle being maintained at 400 DEG C, hydrogen pressure drop makes to inhale hydrogen product generation hydrogen discharge reaction as low as 3 bar,
Deuterium can release during hydrogen discharge reaction.After hydrogen release 30min, reaction kettle is taken out from heating furnace, is cooled to
Room temperature；Again in the glove box filled with argon gas, the reaction product after hydrogen release is taken out from reaction kettle, the reaction product after hydrogen release
XRD spectrum such as Fig. 1（b）It is shown.
Embodiment 2
In the glove box filled with argon gas, by 2:1 molar ratio weighs two kinds of raw material powders of lithium deuteride and magnesium diboride,
In the ball grinder for entering the stainless steel material that volume is 100 ml, and under an argon, with 1 h of planetary ball mill ball milling, carry out
Mechanical mixture processing, obtains the first mixture.
After the first mixture after ball milling is packed into reaction kettle, it is vacuumized, then reaction kettle is placed in heating furnace, and
Reaction kettle is heated to 350 DEG C；Then, it is 99.99% hydrogen to 5MPa that purity is quickly filled with into reaction kettle, and it is anti-to carry out suction hydrogen
120 min are answered, hydrogen abstraction reaction curve is as shown in Figure 3.As can be seen from Fig. 3,90 min or so are carried out in reaction, inhales hydrogen with regard to basic
It completes.Inhale hydrogen after XRD as shown in figure 4, it can be found that, inhale hydrogen after be converted to LiBQ4And MgQ2.Later, by the temperature of reaction kettle
Degree is maintained at 400 DEG C, and hydrogen pressure drop makes to inhale hydrogen product generation hydrogen discharge reaction, deuterium can be released during hydrogen discharge reaction as low as 4 bar
It releases, Hydrogen desorption isotherms are as shown in Figure 5.After hydrogen release 40min, reaction kettle is taken out from heating furnace, is cooled to room temperature,
And in the glove box filled with argon gas, the reaction product after hydrogen release is taken out from reaction kettle, the XRD spectrum of reaction product is as schemed
1（c）It is shown.
Embodiment 3
In the glove box filled with argon gas, by 2:1 molar ratio weighs two kinds of raw material powders of lithium deuteride and magnesium diboride, and
Under an argon, with mortar grinder 10min, mixed processing is carried out, the first mixture is obtained.
After the first mixture after ball milling is packed into reaction kettle, it is vacuumized, then reaction kettle is placed in heating furnace, is added
Thermal response kettle is to 250 DEG C；Then, it is 99.99% hydrogen to 7 MPa that purity is quickly filled with into reaction kettle, and it is anti-to carry out suction hydrogen
It answers.After inhaling hydrogen completion, the temperature of reaction kettle is cooled to room temperature, hydrogen pressure drop is as low as 0 bar, then with the heating of 5 DEG C/min
Rate heats reaction kettle, makes to inhale hydrogen product generation hydrogen discharge reaction, deuterium can release during hydrogen discharge reaction, and hydrogen release is bent
Line is as shown in fig. 6, it can be found that the major temperature section of hydrogen release is at 200-500 DEG C.By hydrogen release to after 500 DEG C, by reaction kettle
400 DEG C are cooled to, above-mentioned suction, hydrogen release process is repeated, can further release deuterium.
Embodiment 4
In the glove box filled with argon gas, by 2:1 molar ratio weighs two kinds of raw material powders of lithium deuteride and magnesium diboride, and
Under an argon, with mortar grinder 5min, mixed processing is carried out, the first mixture is obtained.
After the first mixture after ball milling is packed into reaction kettle, it is vacuumized, then reaction kettle is placed in heating furnace, is added
Thermal response kettle is to 400 DEG C；Then, it is 99.99% hydrogen to 6.5MPa that purity is quickly filled with into reaction kettle, and it is anti-to carry out suction hydrogen
It answers.After inhaling hydrogen completion, the temperature of reaction kettle is cooled to room temperature, hydrogen pressure drop is as low as 0 bar, then with the heating of 5 DEG C/min
Rate heats reaction kettle, makes to inhale hydrogen product generation hydrogen discharge reaction, deuterium can release during hydrogen discharge reaction.By hydrogen release
To after 600 DEG C, reaction kettle is taken out from heating furnace, is cooled to room temperature, in the glove box filled with argon gas, anti-after hydrogen release
Product is answered to take out from reaction kettle, XRD result such as Fig. 1 of product（d）.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (8)
1. a kind of method for recycling hydrogen isotope from hydrogen isotope lithiumation object, which is characterized in that include the following steps：
(1) under protective atmosphere, hydrogen isotope lithiumation object, magnesium diboride is mixed, the first mixture is obtained；
(2) the first mixture is subjected to hydrogen abstraction reaction, obtains inhaling hydrogen product；
(3) by step（ 2）Resulting suction hydrogen product carries out hydrogen release processing, and hydrogen isotope is realized back by hydrogen discharge reaction
It receives；
(4) step is repeated（ 2） ,（ 3）, the same position of hydrogen when hydrogen release processing in the atmosphere that discharges no longer containing recycling in need
Until element.
2. the method according to claim 1, wherein in the hydrogen isotope lithiumation object, hydrogen isotope be protium,
Deuterium, tritium it is one or more.
3. the method according to claim 1, wherein the step（ 1）In, hydrogen isotope lithiumation object and two boron
The molar ratio for changing magnesium is 2：1~10.
4. the method according to claim 1, wherein the step（ 1）In, hybrid mode is grinding or ball
Mill.
5. method according to claim 1-4, which is characterized in that the step（ 1）In, protective atmosphere is lazy
Property gas or hydrogen.
6. according to the method described in claim 5, it is characterized in that, the inert gas is helium or argon gas.
7. the method according to claim 1, wherein the step（ 2）In, the temperature of hydrogen abstraction reaction is 200
~450 DEG C, the Hydrogen Vapor Pressure of hydrogen abstraction reaction is 1~10MPa.
8. the method according to claim 1, wherein the step（ 3）In, the temperature of hydrogen discharge reaction is 250
~500 DEG C, the Hydrogen Vapor Pressure of hydrogen discharge reaction is 0~0.4MPa.
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| CN103831098A (en) * | 2014-03-04 | 2014-06-04 | 华东理工大学 | Catalyst for catalytic oxidation of gaseous hydrogen tritide, and preparation method and application of catalyst |
| CN103922285A (en) * | 2014-05-12 | 2014-07-16 | 四川材料与工艺研究所 | Method for synthesizing lithium borohydride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103831098A (en) * | 2014-03-04 | 2014-06-04 | 华东理工大学 | Catalyst for catalytic oxidation of gaseous hydrogen tritide, and preparation method and application of catalyst |
| CN103922285A (en) * | 2014-05-12 | 2014-07-16 | 四川材料与工艺研究所 | Method for synthesizing lithium borohydride |
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