CN105233691B - A kind of hydrogen isotope high efficiente callback device and recovery method cascaded based on catalytic reaction and UF membrane - Google Patents
A kind of hydrogen isotope high efficiente callback device and recovery method cascaded based on catalytic reaction and UF membrane Download PDFInfo
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- CN105233691B CN105233691B CN201510579340.9A CN201510579340A CN105233691B CN 105233691 B CN105233691 B CN 105233691B CN 201510579340 A CN201510579340 A CN 201510579340A CN 105233691 B CN105233691 B CN 105233691B
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Abstract
The invention discloses a kind of hydrogen isotope high efficiente callback device and recovery method cascaded based on catalytic reaction and UF membrane, when purpose is that solving existing membrane reactor carries out hydrogen isotope recovery, the problem of more foreign gas can cause palladium base film to ooze hydrogen rate reduction in raw material, and its optimal use temperature is difficult to take into account with rate of catalysis reaction.The device includes unstripped gas, fixed bed reactors, palladium membrane hydrogen separation device, air accumulator, booster pump etc..The pattern that the present invention is integrated using catalytic reaction with UF membrane ex situ, the utilization rate of palladium film can be effectively improved, reduce poisoning effect of the foreign gas to palladium film, extend the service life of palladium film, while the rate of recovery of hydrogen isotope can be effectively improved.In addition, the present invention can also form closed cycle, higher hydrogen isotope organic efficiency can be obtained.Reasonable in design, strong adaptability of the invention, disclosure satisfy that the recovery demand of hydrogen isotope, has the higher rate of recovery, for the economy and security realized the circulation of fusion reactor deuterium tritium fuel, improve reactor, have great importance.
Description
Technical field
The present invention relates to fusion reactor field, especially deuterium tritium fusion fuel cycle art, is specially that one kind is based on urging
Change the hydrogen isotope high efficiente callback device and recovery method of reaction and UF membrane cascade.
Background technology
Currently, as the shortage of fossil fuel and the getting worse of environmental pollution, fusion energy resource gradually cause people's
Pay attention to.In the evolution of fusion energy resource, deuterium tritium fuel circulation is the engineering technology problem that must be solved, and it realizes business
The basis of industry application.Because the reactivity of deuterium tritium in fusion facility is very low, a large amount of unreacted deuterium tritiums are caused to be present in ash discharge gas
In, from safe and environment-friendly and economic angle, it is necessary to ash discharge gas is handled, reclaims deuterium tritium fuel therein, improves deuterium tritium
The utilization rate of fuel, avoid its pollution to environment.
Deuterium tritium in fusion reactor ash discharge gas is mainly with Q2（Elemental）, hydrocarbon and water（Compound state）Form
In the presence of.Wherein, Q2Refer to by the simple substance of three kinds of isotopics of protium, i.e. H2、HD、HT、D2、DT、T2.Elemental deuterium tritium
Recovery it is relatively easy, it can be separated using palladium base film；And the recovery of compound state deuterium tritium is then complex, it is necessary to first
Elemental Q is translated into by catalytic reaction2, then by palladium base film Selective Separation.Because tritium has radioactivity and expensive,
Therefore, in the separation process, require very high for the rate of recovery of hydrogen isotope（More than 99.9999%）, using common approach
It is difficult to realize.
If catalytic reaction and UF membrane are integrated, reaction can be made to break through the limitation of equilibrium conversion, greatly improved
The conversion ratio of reaction and the rate of recovery of hydrogen isotope.At present, catalytic reaction and the integrated of UF membrane mainly use what original position integrated
Mode, i.e., using membrane reactor.
In industrial hydrogen production field（Such as methane, methanol decomposition hydrogen manufacturing, Water gas shift/WGS hydrogen manufacturing field）, membrane reactor obtained
Obtained application.In the deuterium tritium fuel circulatory system, German Tritium Laboratory of Karlsruhe（TLK）Research
Personnel use third unit of the membrane reactor as fusion reactor plasma ash discharge gas processing system（Referred to as " PERMCAT " is single
Member）, it, which can be reacted a small amount of compound state deuterium tritium by hydrogen isotopic exchange, replaces and separates, and improves the recovery to deuterium tritium
Rate and decontamination factor.PERMCAT general principle is as shown in Figure 1.The process that the unit carries out hydrogen isotopic exchange reaction is as follows：
H2Molecule penetrates into outside, under catalyst action, its CQ with adverse current on the inside of membrane tube4、Q2O etc. occurs isotope and exchanged instead
Should, the Q of generation2Pd films are passed through again, are separated and are reclaimed in per-meate side.
Membrane reactor intergration model can be by product Q2Reaction system is isolated in original position, its can not only make chemical balance to
The direction for generating product hydrogen is carried out, and and can extends the time that reactant contacts with catalyst, favorably by way of reducing flow velocity
In the further generation of reaction, it is thus possible to obtain very high transformation efficiency.
However, there is also following shortcoming for membrane reactor：（1）More foreign gas can contact with Pd films in raw material, reduce
It oozes hydrogen speed, or even causes Pd poisoning；（2）Q near reactor inlet2Concentration is relatively low, and osmotic driving force is smaller, causes
The efficiency of palladium base UF membrane hydrogen reduces；（3）Because the reactions such as methane cracking, steam reforming are typically higher than palladium base film optimal use
Under temperature conditionss, higher reaction rate is just had, causes both rate of catalysis reaction and temperature in use of palladium base film to be difficult to
U.S.A takes into account.
Therefore, there is an urgent need to a kind of new device to solve the above problems.
The content of the invention
The goal of the invention of the present invention is：It is more in raw material when carrying out hydrogen isotope recovery for existing membrane reactor
Foreign gas palladium base film can be made to ooze hydrogen speed and separative efficiency reduce, its optimal use temperature is difficult to simultaneous with rate of catalysis reaction
A kind of the problem of Gu, there is provided hydrogen isotope high efficiente callback device and recovery method cascaded based on catalytic reaction and UF membrane.This
The pattern that invention is integrated using catalytic reaction with UF membrane ex situ, the utilization rate of palladium film can be effectively improved, reduce impurity gas
Body extends the service life of palladium film, while can effectively improve the rate of recovery of hydrogen isotope to the poisoning effect of palladium film.In addition,
The present invention can also form closed cycle, can obtain higher hydrogen isotope organic efficiency.Reasonable in design, strong adaptability of the invention,
The recovery demand of hydrogen isotope is disclosure satisfy that, there is the higher rate of recovery, for realizing the circulation of fusion reactor deuterium tritium fuel, carrying
The economy and security of high reactor, have great importance.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of hydrogen isotope high efficiente callback device cascaded based on catalytic reaction and UF membrane, including unstripped gas, for urging
Change fixed bed reactors, palladium membrane hydrogen separation device, the first air accumulator, the second air accumulator, the first booster of reaction, the original
Material gas is connected by pipeline with fixed bed reactors, the fixed bed reactors, the first air accumulator, the first booster, the second storage
Gas tank, palladium membrane hydrogen separation device are sequentially connected by pipeline, what second air accumulator was connected with palladium membrane hydrogen separation device
Flow control valve is provided with pipeline.
The reaction product of the fixed bed reactors can be entered in the first air accumulator by pipeline, in first air accumulator
Reaction product can after the first charger boost enter the second air accumulator in, the reaction product in second air accumulator can be entered
Enter in palladium membrane hydrogen separation device and separated.
Also include the hydrogen gas leakage warning device for monitoring hydrogen content.
Also include pressure gauge, the pressure gauge is connected with the first air accumulator, the second air accumulator respectively, and the pressure gauge can divide
The first air accumulator, the pressure in the second air accumulator are not shown.
Also include pressure warning unit, the pressure warning unit is connected with the first air accumulator, the second air accumulator respectively.
The control system for also include pressure discharge device, being connected with pressure discharge device, the pressure discharge device are separately positioned on the first storage
On gas tank, the second air accumulator, the pressure discharge device can be arranged when the pressure of the first air accumulator, the second air accumulator exceedes setting value
Gas.
Pressure-reducing valve, stop valve are respectively arranged with the pipeline that the unstripped gas is connected with fixed bed reactors.
Also include the 3rd air accumulator, the 4th air accumulator, the second booster, the palladium membrane hydrogen separation device, the 3rd gas storage
Tank, the second booster, the 4th air accumulator, fixed bed reactors are sequentially connected by pipeline.
Pressure gauge, pressure discharge device are respectively provided with 3rd air accumulator and the 4th air accumulator.
Pressure-reducing valve, stop valve are respectively arranged with the pipeline that 4th air accumulator is connected with fixed bed reactors.
A kind of recovery method of the hydrogen isotope high efficiente callback device cascaded based on catalytic reaction and UF membrane, including it is as follows
Step：Raw material in unstripped gas obtains reaction product after pipeline enters fixed bed reactors reaction, and reaction product enters first
In air accumulator, then the reaction product of the first air accumulator is pressurized by the first booster, the reaction product after supercharging enters
In second air accumulator, finally enter palladium membrane hydrogen separation device and separated, reclaim elemental hydrogen isotope therein.
For foregoing problems, the present invention provides a kind of hydrogen isotope high efficiente callback cascaded based on catalytic reaction and UF membrane
Device and recovery method.The device include unstripped gas, the fixed bed reactors for catalytic reaction, palladium membrane hydrogen separation device,
First air accumulator, the second air accumulator, the first booster, unstripped gas are connected by pipeline with fixed bed reactors, so that fixed
The reaction product of bed reactor can be entered in the first air accumulator by pipeline；Fixed bed reactors, the first air accumulator, the first supercharging
Device, the second air accumulator, palladium membrane hydrogen separation device are sequentially connected by pipeline, enable the reaction product in the first air accumulator through
Enter after one charger boost in the second air accumulator, the reaction product in the second air accumulator can enter in palladium membrane hydrogen separation device
Separated；Flow control valve is provided with the pipeline that second air accumulator is connected with palladium membrane hydrogen separation device, is adjusted by flow
The gas flow that section valve can be adjusted into palladium membrane hydrogen separation device is adjusted.
In the present invention, fixed bed reactors are the place of catalytic reaction, can be methane cracking, steam reforming, the same position of hydrogen
The reactions such as element exchange provide the conditions such as suitable temperature, pressure, catalyst, so as to which compound state hydrogen isotope is converted into simple substance
State.Palladium membrane hydrogen separation device then can separate elemental hydrogen isotope with other foreign gases, obtain the same position of high-purity hydrogen
Plain simple substance（Permeate gas）.
Further, in addition to hydrogen gas leakage warning device, by the device can be around real-time monitoring system hydrogen contain
Amount, it is ensured that the security of system.Also include pressure warning unit, pressure warning unit respectively with the first air accumulator, the second gas storage
Tank is connected, and the gas pressure in air accumulator can be monitored by pressure warning unit.Also include pressure discharge device, with pressure discharge device phase
Control system even, when pressure is higher than 0.7MPa, sound and light alarm, and gas in drain tank in time are sent, avoids superpressure situation
Generation.
Further, in addition to the 3rd air accumulator, the 4th air accumulator, the second booster, palladium membrane hydrogen separation device, the 3rd store up
Gas tank, the second booster, the 4th air accumulator, fixed bed reactors are sequentially connected by pipeline.
Using the recovery method of aforementioned means, comprise the following steps：Raw material in unstripped gas is anti-into fixed bed through pipeline
After answering device to react, reaction product is obtained, reaction product enters in the first air accumulator, then the reaction product of the first air accumulator is passed through
First booster is pressurized, and the reaction product after supercharging enters in the second air accumulator, finally enters palladium membrane hydrogen separation device
Separated, reclaim elemental hydrogen isotope therein.
In order to while high efficiente callback hydrogen isotope, improve the utilization rate of palladium film, poison of the foreign gas to palladium film is reduced
Change acts on, and the present invention uses and integrates the ex situ of fixed bed reactors and palladium membrane hydrogen separation device, i.e. catalytic reaction and film
Separation cascade, first introduces Pd/Ag membrane separators by the reaction product of the catalytic reactions such as methane cracking, steam reforming（That is palladium film hydrogen
Air separation）, elemental hydrogen isotope therein is separated and recovered, to promote the progress of positive reaction, improves the same position of compound state hydrogen
The conversion ratio of element.Meanwhile if still there is the hydrogen isotope of high level in the tail gas of palladium membrane hydrogen separation device, can also be through the 3rd storage
Gas tank, the 4th air accumulator, the recovery system of the second booster composition, secondary response again is returned in fixed bed reactors by tail gas,
Closed cycle is thusly-formed, higher hydrogen isotope organic efficiency can be obtained.
In the present invention, the impurity such as hydrocarbon, water in raw material is most of to be converted into Q after catalytic reaction2, obtain
To reaction product, reaction product enters in the first air accumulator, then the reaction product of the first air accumulator is entered by the first booster
Row supercharging, the reaction product after supercharging are passed through palladium membrane hydrogen separation device and separated.Catalytic reaction is being realized using the present invention
While cascade with UF membrane, palladium membrane hydrogen separation device can be touched to the initial concentration rise of hydrogen simple substance in unstripped gas,
Increase the driving force of hydrogen simple substance infiltration, greatly improve per membrane area oozes hydrogen efficiency and the utilization rate of film.Also, the present invention's
Fixed bed reactors can be fully reacted unstripped gas, so as to which the foreign gas content adversely affected to palladium base film properties be dropped
It is low, weaken the poisoning effect to palladium base film, effectively extend the service life of palladium base film in palladium membrane hydrogen separation device.In addition, adopt
With the mode of the present invention, when designing catalytic reaction, influence of the reaction temperature to palladium base membrane stability and service life can not be considered,
The design difficulty of reduction system, improve the adaptability of device.
To sum up, compared with membrane reactor intergration model, the present invention can reduce the design difficulty of device, have stronger reality
With property, and the hydrogen efficiency of oozing of per membrane area can be increased, improve the utilization rate of palladium film, extend its service life.
Brief description of the drawings
Fig. 1 is existing PERMCAT（Catalytic film reactor）Basic principle schematic.
Fig. 2 is the structural representation of the present invention.
Marked in figure：1 is unstripped gas, and 2 be fixed bed reactors, and 3 be palladium membrane hydrogen separation device, and 4 be the first air accumulator,
5 be the second air accumulator, and 6 be the first booster, and 7 be pressure gauge, and 8 be the 3rd air accumulator, and 9 be the 4th air accumulator, and 10 be the second increasing
Depressor.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent by other or with similar purpose
Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics
.
Embodiment 1
As illustrated, the device includes unstripped gas, the fixed bed reactors for catalytic reaction, palladium-membrane hydrogen separation dress
Put, the first air accumulator, the second air accumulator, the first booster, the 3rd air accumulator, the 4th air accumulator, the second booster, unstripped gas leads to
Piping is connected with fixed bed reactors, fixed bed reactors, the first air accumulator, the first booster, the second air accumulator, palladium film hydrogen
Air separation is sequentially connected by pipeline, palladium membrane hydrogen separation device, the 3rd air accumulator, the second booster, the 4th air accumulator,
Fixed bed reactors are sequentially connected by pipeline, and stream is provided with the pipeline that the second air accumulator is connected with palladium membrane hydrogen separation device
Adjustable valve.On the pipeline that unstripped gas is connected with fixed bed reactors, the pipeline that the 4th air accumulator is connected with fixed bed reactors
On be respectively arranged with pressure-reducing valve, stop valve.The reaction product of fixed bed reactors can be entered in the first air accumulator by pipeline, the
Reaction product in one air accumulator can enter in the second air accumulator after the first charger boost, the reaction production in the second air accumulator
Thing, which can enter in palladium membrane hydrogen separation device, to be separated.The tail gas of palladium membrane hydrogen separation device separation can be through successively through the 3rd storage
Gas tank, the second booster, the 4th air accumulator are back in fixed bed reactors by pipeline.
Further, the device also includes the hydrogen gas leakage warning device, pressure warning unit, pressure for monitoring hydrogen content
Power meter, pressure discharge device, the control system being connected with pressure discharge device, pressure warning unit respectively with the first air accumulator, the second gas storage
Tank, the 3rd air accumulator, the 4th air accumulator are connected.Pressure gauge, pressure discharge device are respectively several, and pressure gauge, pressure discharge device are distinguished
Be arranged on the first air accumulator, the second air accumulator, the 3rd air accumulator, on the 4th air accumulator.
When the present invention starts, unstripped gas enters in fixed bed reactors through pipeline, and is reacted under catalyst action,
Reaction product enters in the first air accumulator through pipeline.Then, start the first booster, the reacting gas in the first air accumulator is sent
Enter in the second air accumulator, pressure gauge can show the first air accumulator, the pressure of the second air accumulator.It will be pressurizeed again in the second air accumulator
Reacting gas be sent into palladium membrane hydrogen separation device in, be connected by the second air accumulator with palladium membrane hydrogen separation device on pipeline
Flow control valve can adjusting gas flow, so as to control the speed of reaction.The infiltration isolated from palladium membrane hydrogen separation device
Gas（High-purity Q2）It is recovered, if Q contents are relatively low in tail gas, can directly discharges；If Q contents are higher, pass through recovery system
It is back in fixed bed reactors and is reacted again.I.e. tail gas enters in the 3rd air accumulator, and passes through the second charger boost
Afterwards, the pipeline being connected into the 4th air accumulator, the tail gas after the interior supercharging of the 4th air accumulator through it with fixed bed reactors, is back to
Fixed bed reactors carry out catalytic reaction again, to form closed cycle.
By taking methane cracking as an example.
Unstripped gas is CH4, NiCu/SiO is loaded in fixed bed reactors2Catalyst, reaction temperature is 800 DEG C, through a secondary fissure
Solution reaction, methane conversion is about 25%, obtains reaction product, CH in reaction product4And H2Content be respectively 60% and 40%（Body
Fraction）.Reaction product reaches membrane separator through the first air accumulator, the first booster, the second air accumulator successively（Operating temperature is
400℃）, the infiltration gas of UF membrane is the H that purity is higher than 99.9%2（Directly recycle）, then contain a large amount of unreacteds in tail gas
CH4With a small amount of H2, its content is respectively 95% and 5%（Volume fraction）.Tail gas is successively through the 3rd air accumulator, the second booster,
Four air accumulators enter fixed bed reactors secondary response again, CH in product4And H2Content be respectively 57.6% and 42.4%（Volume integral
Number）, then membrane separator is reached through the first air accumulator, the first booster, the second air accumulator successively, infiltration gas can be reclaimed directly
High-purity H2, contain unreacted CH in tail gas4With a small amount of H2, turn again to fixed bed reactors.After so circulating five times, CH4In
The conversion rate of recovery of protium is more than 90%.
The invention is not limited in foregoing embodiment.The present invention, which expands to, any in this manual to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (9)
1. a kind of hydrogen isotope efficient recycling method cascaded based on catalytic reaction and UF membrane, it is characterised in that including as follows
Step：Raw material in unstripped gas obtains reaction product after pipeline enters fixed bed reactors reaction, and reaction product enters first
In air accumulator, then the reaction product of the first air accumulator is pressurized by the first booster, the reaction product after supercharging enters
In second air accumulator, finally enter palladium membrane hydrogen separation device and separated, reclaim elemental hydrogen isotope therein；
The device that it is used is as follows：The device includes unstripped gas, the fixed bed reactors for catalytic reaction, palladium-membrane hydrogen separation
Device, the first air accumulator, the second air accumulator, the first booster, the unstripped gas are connected by pipeline with fixed bed reactors, institute
Fixed bed reactors, the first air accumulator, the first booster, the second air accumulator, palladium membrane hydrogen separation device are stated by pipeline successively
It is connected, flow control valve is provided with the pipeline that second air accumulator is connected with palladium membrane hydrogen separation device；
Wherein, fixed bed reactors integrate with palladium membrane hydrogen separation device ex situ.
2. the hydrogen isotope efficient recycling method cascaded according to claim 1 based on catalytic reaction and UF membrane, its feature
It is, in addition to the hydrogen gas leakage warning device for monitoring hydrogen content.
3. the hydrogen isotope efficient recycling method cascaded according to claim 1 based on catalytic reaction and UF membrane, its feature
It is, in addition to pressure gauge, the pressure gauge are connected with the first air accumulator, the second air accumulator respectively, the pressure gauge can be distinguished
Show the first air accumulator, the pressure in the second air accumulator.
4. the hydrogen isotope efficient recycling method cascaded according to claim 1 based on catalytic reaction and UF membrane, its feature
It is, in addition to pressure warning unit, the pressure warning unit are connected with the first air accumulator, the second air accumulator respectively.
5. the hydrogen isotope efficient recycling method cascaded according to claim 1 based on catalytic reaction and UF membrane, its feature
It is, in addition to pressure discharge device, the control system that is connected with pressure discharge device, the pressure discharge device are separately positioned on the first gas storage
On tank, the second air accumulator, the pressure discharge device can be vented when the pressure of the first air accumulator, the second air accumulator exceedes setting value.
6. the hydrogen isotope efficient recycling method cascaded according to claim 1 based on catalytic reaction and UF membrane, its feature
It is, pressure-reducing valve, stop valve is respectively arranged with the pipeline that the unstripped gas is connected with fixed bed reactors.
7. the hydrogen isotope high efficiente callback side cascaded according to claim any one of 1-6 based on catalytic reaction and UF membrane
Method, it is characterised in that also including the 3rd air accumulator, the 4th air accumulator, the second booster, the palladium membrane hydrogen separation device,
Three air accumulators, the second booster, the 4th air accumulator, fixed bed reactors are sequentially connected by pipeline.
8. the hydrogen isotope efficient recycling method cascaded according to claim 7 based on catalytic reaction and UF membrane, its feature
It is, pressure gauge, pressure discharge device is respectively provided with the 3rd air accumulator, the 4th air accumulator.
9. the hydrogen isotope efficient recycling method cascaded according to claim 7 based on catalytic reaction and UF membrane, its feature
It is, pressure-reducing valve, stop valve is respectively arranged with the pipeline that the 4th air accumulator is connected with fixed bed reactors.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105923604B (en) * | 2016-04-20 | 2018-03-30 | 中国工程物理研究院核物理与化学研究所 | Deuterium tritium Rapid recovery device and method in a kind of fusion reactor ash discharge gas |
| CN105903349B (en) * | 2016-06-07 | 2017-06-27 | 中国工程物理研究院核物理与化学研究所 | A kind of large area palladium film device for hydrogen isotope separation |
| CN107051205B (en) * | 2017-02-15 | 2019-02-12 | 中国工程物理研究院材料研究所 | A kind of low temperature palladium displacement separation method |
| CN107879312B (en) * | 2017-12-07 | 2021-04-06 | 中国工程物理研究院核物理与化学研究所 | Corrugated membrane reactor device for hydrogen isotope exchange |
| CN112037958B (en) * | 2020-09-09 | 2022-09-23 | 中国工程物理研究院核物理与化学研究所 | High-concentration tritium water treatment device |
| CN115138186A (en) * | 2022-06-29 | 2022-10-04 | 中国石油大学(华东) | Hydrogen separation device with spiral structure membrane module |
| CN115285940A (en) * | 2022-08-23 | 2022-11-04 | 中国原子能科学研究院 | Method and system for recovering hydrogen isotopes in process waste gas |
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| CN1097398A (en) * | 1993-07-13 | 1995-01-18 | 中国科学院山西煤炭化学研究所 | The method and apparatus of preparing nitrogen atmosphere by barrier separation for metallic heat treatment |
| CN1320555A (en) * | 2000-04-26 | 2001-11-07 | 中国科学院大连化学物理研究所 | Process for preparing hydrogen by reaction of mixture of methane, ethane, propane and butane gases with CO2 and oxygen |
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| CN1097398A (en) * | 1993-07-13 | 1995-01-18 | 中国科学院山西煤炭化学研究所 | The method and apparatus of preparing nitrogen atmosphere by barrier separation for metallic heat treatment |
| CN1320555A (en) * | 2000-04-26 | 2001-11-07 | 中国科学院大连化学物理研究所 | Process for preparing hydrogen by reaction of mixture of methane, ethane, propane and butane gases with CO2 and oxygen |
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