CN109289526A - A kind of rotary low temperature hydrogen isotope separation system and separation method - Google Patents
A kind of rotary low temperature hydrogen isotope separation system and separation method Download PDFInfo
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- CN109289526A CN109289526A CN201811098571.8A CN201811098571A CN109289526A CN 109289526 A CN109289526 A CN 109289526A CN 201811098571 A CN201811098571 A CN 201811098571A CN 109289526 A CN109289526 A CN 109289526A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/22—Separation by extracting
- B01D59/26—Separation by extracting by sorption, i.e. absorption, adsorption, persorption
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Abstract
The present invention discloses a kind of rotary low temperature hydrogen isotope separation system and separation method, it solves to build complicated, state modulator complexity, operating cost height in the prior art, or it needs complicated helium supply, the separation of hydrogen helium and splitter regeneration treatment or palladium displcement chromatography filler valuableness and is easy to the problems such as failing.Separation system includes cryostat, reversing frame, splitter, feed hydrogen storage tank, light isotope storage tank, heavy isotope storage tank, vacuum pump and tail gas storage tank.Separation method is that the splitter for being adsorbed with feed hydrogen is detached from liquid nitrogen liquid level one by one to desorb hydrogen isotope to complete the rearrangement of hydrogen isotope in remaining splitter；Finally from circuit, light, heavy isotope is collected in remote, proximal end respectively.The present invention creatively utilizes simulated moving bed technology principle, hydrogen isotope can continuously circulate in closed loop separating circuit, the proximal end that heavy isotope concentration is desorbed from separating circuit is to distally gradually decreasing, and the concentration gradient of heavy isotope increases with adsorption/desorption number and constantly increases.
Description
Technical field
The present invention relates to Application of Nuclear Technology fields, and in particular to a kind of rotary low temperature hydrogen isotope separation system and separation
Method.
Background technique
Hydrogen isotope separation is one of the core technology of fusion reactor deuterium triton fuel recycle, by isotopic separation,
A large amount of unburned deuterium tritium gas in reactor operation can not only re-used, can also be achieved to fusion reaction stack operation
Effective control of the Environment release amount of tritium in the process.To meet the following fusion reaction stack operation to extensive hydrogen isotope separation need
It asks, a series of hydrogen isotope separation technology, including cryogenic rectification (LHD), low temperature chromatography (GC) and palladium has been developed at present
Displcement chromatography etc..
Cryogenic rectification method is separated using the boiling point difference of different Hydrogen isotopic molecules.Six kinds of molecules of hydrogen isotope
(H2、HD、D2, DT, HT and T2) in 20K-25K temperature range, their boiling point is there are minute differences, wherein H2Highest, T2Most
It is low.Using liquid helium as refrigeration source, run cryogenic rectification column to realize isotopic separation under liquid hydrogen temperature.Cryogenic rectification method exists
Separation system structure and complex operation and energy consumption are high, the separation system tritium amount of storing is big, system Construction and operating cost are high
The disadvantages of.
Subambient chromatography is separated using the chromatography effect of cryogenic absorption material.When helium by under liquid nitrogen temperature (-
196 DEG C), in advance when being adsorbed with the 5A molecular sieve splitter of hydrogen isotope mixed gas, due under low temperature molecular sieve to hydrogen isotope
The adsorption capacity of different component in mixed gas is different, when splitter long enough, will successively occur H in eluting gas2、
HD、HT、D2, DT and T2The peak of distinct six kinds of Hydrogen isotopic molecules, splitter is longer, and the spacing between peak is bigger.Not
It is collected respectively in peak position with the period, then available six kinds different hydrogen isotope gas.The shortcomings that this separation method is to divide
From must carry out under liquid nitrogen temperature, refrigerated separation column must consume a large amount of liquid nitrogen, and energy consumption is higher, and the product air lift of single separation
Take ratio lower.
Palladium displacement chromatography carries out isotopic separation using isotope effect of the palladium when forming hydride.Metal Palladium has very
Strong hydrogen isotope separation effect, compared with heavy isotope component deuterium (D) and tritium (T), light isotope composition protium (H) is easier
It is reacted with Metal Palladium and generates more stable solid-state palladium hydride, when equilibrium is reached, the partial pressure of heavy isotope component in gas phase
It is relatively high, and temperature is lower, separation effect is bigger.Divided method has palladium Hot swapping chromatography and thermal cycle absorption etc. at present.It should
The shortcomings that method is will be using expensive palladium as separating column packing, and separation process suction hydrogen repeatedly, hydrogen release can make
Disadvantageous changes occur for the hydrogen absorption characteristic of separation material palladium, such as separation material dusting, palladium and the interaction of palladium carrier material cause
Hydrogen absorption characteristic change etc., the useful life of splitter is short.
Summary of the invention
The technical problem to be solved by the present invention is providing a kind of rotary low temperature hydrogen isotope separation system and separation side
Method solves cryogenic rectification method system building complexity, state modulator complexity operating cost height, subambient chromatography in the prior art and needs
Helium supply, the separation of hydrogen helium and splitter regeneration treatment are complicated, and palladium displcement chromatography filler is expensive and is easy to the problems such as failing.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of rotary low temperature hydrogen isotope separation system is installed on the cryostat, including the interior cryostat, for storing liquid nitrogen
It is interior and can equidistantly be horizontally installed to the circumference of reversing frame outer ring relative to the circular ring shape reversing frame that the cryostat, rotates freely
Above and can be with n splitter of the reversing frame synchronous rotary, the n splitters are on the reversing frame by side clockwise
Form closed circuit to pipeline head and the tail connection is passed sequentially through, the n splitters successively from 1#, 2#, 3# ... (n-1) #, n# into
Row number.Separation system further includes the feed hydrogen for being stored with feed hydrogen and being connect respectively with 1#~(n-2) # splitter by pipeline
Storage tank, the light isotope storage tank for storing light isotope and being connect by pipeline with (n-1) # splitter are same for storing weight
Heavy isotope storage tank position element and connect by pipeline with 1# splitter, is connect with all splitters respectively by pipeline
Vacuum pump, and the tail gas storage tank being connect with the vacuum-pump line；The n splitters are on the reversing frame by clockwise
Direction passes sequentially through pipeline head and the tail connection and forms closed circuit, one and only one splitter is located at low in the n splitters
In warm slot more than the liquid level of liquid nitrogen, the remaining n-1 splitters are entirely located in the liquid level of liquid nitrogen in cryostat, hereinafter, the tail
Gas storage tank is connect with the feed hydrogen storage-tank pipeline.
Further, the reversing frame includes being horizontally installed in the cryostat, and can be relative to the cryostat, freedom
The rotary shaft of rotation, and be installed in the rotary shaft in the cryostat, and along longitudinal direction and can be in company with the rotary shaft
The circular ring shape aluminium chassis of synchronous rotary, it is upper on the excircle of the aluminium chassis longitudinal equidistantly to offer n and separated respectively with described
The round clamping hole that column matches, and the n splitters are respectively arranged in the n circles and clamp in hole.
Further, the both ends of the rotary shaft are extended to respectively outside the corresponding two sidewalls of the cryostat, the rotation
One end of axis is connected with the frequency control motor for being used to drive the rotary shaft rotation outside the cryostat, by shaft coupling,
The other end of the rotary shaft is connected with the Multi-path rotary connector that gas piping connection is used for outside the cryostat, described
Rotary shaft is hollow aluminum pipe, is connected to the pipeline of the n splitters by the inner cavity of the rotary shaft and the multi-path
Rotary joint cabling.
Further, the both ends of the rotary shaft are respectively installed with a cryogenic bearing, two cryogenic bearing difference
In the corresponding two sidewalls of the cryostat,.
Further, the splitter is that both ends are welded using flat seal and both ends of the surface are connected not by cutting ferrule respectively
Become rusty corrugated steel pipe, and the splitter pressure resistance reaches 1MPa.
Further, it is filled with the inorganic filler with low temperature hydrogen isotope effect in the splitter, it is described inorganic to fill out
Material is any one in molecular sieve, aluminum oxide or silica gel, and the inorganic filler is being filled into the splitter
Water process is removed by 300 DEG C or more of high-temperature activation before.
Further, tank connected feed hydrogen pipeline is stored up with the feed hydrogen be equipped with first flowmeter, and it is described light same
Position element stores up tank connected light isotope pipeline and is equipped with third flowmeter, stores up tank connected heavy isotope pipe with the heavy isotope
Road is equipped with second flowmeter.
Further, one is respectively provided on the pipeline that the feed hydrogen pipeline is connect with 1#~(n-2) # splitter respectively to open
Valve is closed, the pipeline that the light isotope pipeline is connect with (n-1) # splitter is equipped with a switch valve, the heavy isotope pipe
The pipeline that road is connect with 1# splitter respectively is equipped with a switch valve, and the vacuum pump is connect with the n splitters respectively
Pipeline on be respectively provided with a switch valve, be equipped with a starting differential pressure on the pipelines between the adjacent splitter of all connections
For the adjustable check valve of 0.1MPa~0.5MPa.
Further, the aluminium chassis is made of 1515 aluminum profiles.
A kind of separation method of rotary low temperature hydrogen isotope separation system, comprising the following steps:
1) n splitter is numbered sequence first, and number is respectively 1#, 2#, 3# ... (n-1) #, n#, then will
Each splitter is connected to vacuum pump, is opened vacuum pump and is extracted remaining gas in each splitter, backward cryostat, in injection liquid
Nitrogen is immersed in 1#~(n-1) # in liquid nitrogen, and the n# splitter for being located at turn around frame top is higher than liquid nitrogen liquid level；
2) valve that 1# splitter is connected to feed hydrogen storage tank is opened, feed hydrogen is injected into system, makes 1#~(n-1) #
Splitter reaches saturated extent of adsorption；
3) frequency control motor is opened, rotates reversing frame counterclockwise, 1# splitter is moved up and is detached from liquid nitrogen liquid level,
N# splitter, which moves down, simultaneously immerses in liquid nitrogen；1# splitter absorbs atmospheric heat, and hydrogen isotope desorption makes 1#~(n-1) #
Hydrogen isotope in splitter successively moves backward, and finally completes to reset for the first time in 2#~n# splitter；When 1# splitter
When hydrogen isotope release is completed, remaining hydrogen isotope in vacuum line abstraction 1# splitter is opened；
4) rotation reversing frame counterclockwise again, moves up 2# splitter and is detached from liquid nitrogen liquid level, 1# splitter is to moving down
It is dynamic to immerse in liquid nitrogen；2# splitter absorb atmospheric heat desorb hydrogen isotope gas, in each splitter hydrogen isotope successively to
After move, finally complete second in 3#~n# and 1# splitter and reset；When 2# splitter, which desorbs, to be completed, connection 2# is opened
Hydrogen isotope is remained in the vacuum line abstraction 2# splitter of splitter；
5) step 4 is repeated, the lock out operation of 3#~n-1# splitter is carried out respectively, makes hydrogen isotope in 1#~n# splitter
Sequence is mobile in the loop checking installation of composition, and the separation of hydrogen isotope is constantly promoted to reset；After the completion of the desorption of the n-th # splitter, hydrogen
Isotope has carried out n-th rearrangement, and hydrogen isotope is distributed in 1#~(n-1) # splitter again, and expression system, which completes, once to be followed
Ring separation；Hydrogen isotope forms significant hydrogen isotope concentration gradient, and the 1# splitter top heavy isotope of circuit proximal end is (such as
Deuterium, tritium) concentration highest, and the heavy isotope concentration of (n-1) # of circuit distal end separation column bottom is minimum；
6) pipeline that light isotope storage tank is connect with (n-1) # splitter is opened, while opening frequency control motor to make to turn round
Frame rotates clockwise, and (n-1) # splitter is made to climb away liquid nitrogen liquid level, and light same position is discharged from the bottom of (n-1) # splitter
Element simultaneously collects the pipeline for having collected that closing light isotope storage tank is connect with (n-1) # splitter afterwards into light isotope storage tank；Later
The pipeline that heavy isotope storage tank is connect with 1# splitter is opened, while opening frequency control motor makes reversing frame by rotation counterclockwise
Turn, 1# splitter is made to climb away liquid level, heavy isotope is discharged from the top of 1# splitter and collects into heavy isotope storage tank；
7) to the isotope abundance sampling analysis in 2#~n-2# splitter, abundance and the close separation of feed hydrogen are chosen
Column injects feed hydrogen from its top, and the light isotope and heavy isotope collected in feed hydrogen injection rate and light isotope storage tank store up
The total collection for the heavy isotope collected in tank is equal；Then the lock out operation of next circulation is carried out；If one cycle separates
Light same position and heavy isotope abundance and extracted amount be not up to desired value, can by increase splitter quantity or cycle-index come
Bigger hydrogen isotope concentration gradient is obtained, to reach expected separating effect.
Compared with prior art, the invention has the following advantages:
The present invention creatively utilizes simulated moving bed technology principle, and hydrogen isotope can connect in closed loop splitter circuit
Continuous to circulate, the proximal end that heavy isotope (deuterium, tritium) concentration is desorbed from separating circuit is to distally gradually decreasing, and again
The concentration gradient of isotope increases with adsorption/desorption number and constantly increases, and this method flexible operation can easily pass through work
Skill control obtains the heavy isotope and light isotope of different abundance.
The present invention is used for hydrogen isotope separation, using accumulation loop lock out operation, relative to cryogenic rectification method, system bulk
Be substantially reduced, state modulator it is simple, the hydrogen isotope hold-up in system is low, and operation energy consumption can be greatly reduced.
The present invention is used for hydrogen isotope separation, opposite palladium displacement chromatography, and packing material is cheap molecular sieve etc.
Inorganic filler does not need to use expensive palladium as filler, and it is physical process, material that hydrogen release is inhaled in separation process
Matter is stablized, and can be used for a long time, thus system cost is greatly lowered.
The present invention is used for hydrogen isotope separation, opposite Conventional cryogenic chromatography, does not need helium as carrier gas, therefore system knot
Structure is simpler, and subsequent hydrogen/helium separating technology link is not present, therefore operates easier.In addition, at separation system main body
In hydrogen adsorption saturation state, therefore the effective rate of utilization of splitter is higher, and system scale can be smaller, and construction can be significantly reduced
Cost.
The present invention relative to cryogenic rectification, Conventional cryogenic chromatography and palladium displcement chromatography, system structure is simple, filler is cheap,
Easy to control, equipment scale is smaller, and construction cost is lower, and hydrogen isotope separation operation can be carried out using semi-continuous mode and is made
Obtain heavy isotope and light isotope.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of separation system of the present invention.
Fig. 2 is splitter arrangement view on reversing frame in invention separation system.
Fig. 3 is that the process layout of separation system of the present invention schemes.
Wherein, the corresponding title of appended drawing reference are as follows:
1- cryostat, 2- reversing frame, 3- splitter, 4- feed hydrogen storage tank, 5- light isotope storage tank, the storage of 6- heavy isotope
Tank, 7- vacuum pump, 8- tail gas storage tank, 9- first flowmeter, 10- second flowmeter, 11- third flowmeter, 21- rotary shaft, 22-
Aluminium chassis, 23- frequency control motor, 24- Multi-path rotary connector, 25- cryogenic bearing.
Specific embodiment
The invention will be further described with embodiment for explanation with reference to the accompanying drawing, and mode of the invention includes but not only limits
In following embodiment.
As shown in Figure 1-3, a kind of rotary low temperature hydrogen isotope separation system provided by the invention, relative to low temperature essence
It evaporates, Conventional cryogenic chromatography and palladium displcement chromatography, system structure is simple, filler is cheap, easy to control, and equipment scale is smaller, builds
Cost is lower, hydrogen isotope separation operation can be carried out using semi-continuous mode, acquisition heavy isotope and light isotope is made.This
Inventing rotary low temperature hydrogen isotope separation system includes the interior cryostat, 1 for storing liquid nitrogen, is installed in the cryostat, 1 and can phase
For the circular ring shape reversing frame 2 that the cryostat, 1 rotates freely, on the circumferentially equidistant circumference for being horizontally installed to 2 outer ring of reversing frame
And can with the n splitter 3 of 2 synchronous rotary of reversing frame, be stored with feed hydrogen and by feed hydrogen pipeline respectively with 1#
The feed hydrogen storage tank 4 that~(n-2) # splitter 3 connects, for storing light isotope and being connect by pipeline with (n-1) splitter 3
Light isotope storage tank 5, the heavy isotope storage tank 6 for storing heavy isotope and being connect with 1# splitter 3 by pipeline passes through
The vacuum pump 7 that pipeline is connect with all splitters 3 respectively, and the tail gas storage tank 8 being connect with 7 pipeline of vacuum pump；n
A splitter 3 passes sequentially through pipeline head and the tail connection in the direction of the clock on the reversing frame 2 and forms closed circuit, and n is a
One and only one splitter 3 is located in cryostat, 1 more than the liquid level of liquid nitrogen in the splitter 3, the remaining n-1 separation
Column 3 is entirely located in the liquid level of liquid nitrogen in cryostat, 1 hereinafter, the tail gas storage tank 8 is connect with 4 pipeline of feed hydrogen storage tank, and n is a
The splitter is successively numbered from 1#, 2#, 3# ... (n-1) #, n#.
Reversing frame 2 described in the rotary low temperature hydrogen isotope separation system of the present invention includes being horizontally installed to the cryostat, 1
Rotary shaft 21 that is interior and being rotated freely relative to the cryostat, 1, and be installed in the cryostat, 1 and along longitudinal direction
And it can be in company with the circular ring shape aluminium chassis 22 of 21 synchronous rotary of rotary shaft, the outer circle of the aluminium chassis 22 in the rotary shaft 21
It is longitudinal on week equidistantly to offer the n round clamping holes to match respectively with the splitter 3, and the n splitters 3 divide
It is not installed in the n round clamping holes.The both ends of the rotary shaft 21 extend to the corresponding two sides of the cryostat, 1 respectively
Outside wall, one end of the rotary shaft 21 is connected with outside the cryostat, 1 by shaft coupling for driving the rotary shaft 21
The frequency control motor 23 of rotation, the other end of the rotary shaft 21 are connected with outside the cryostat, 1 for gas piping
The Multi-path rotary connector 24 of connection, the rotary shaft 21 are hollow aluminum pipe, and the pipeline for being connected to the n splitters 3 is logical
Cross the rotary shaft 21 inner cavity and 24 cabling of Multi-path rotary connector.The both ends of the rotary shaft 21 are respectively installed with one
A cryogenic bearing 25, two cryogenic bearings 25 are flush-mounted in the corresponding two sidewalls of the cryostat, 1 respectively, the aluminium frame
Frame 22 is made of 1515 aluminum profiles.
Splitter 3 described in the rotary low temperature hydrogen isotope separation system of the present invention be both ends welded using flat seal and
Both ends of the surface connect corrugated stainless steel tubing by cutting ferrule respectively, and 3 pressure resistance of splitter reaches 1MPa.It is filled in the splitter 3
Inorganic filler with low temperature hydrogen isotope effect, the inorganic filler are any in molecular sieve, aluminum oxide or silica gel
One kind, and high-temperature activation of the inorganic filler before being filled into the splitter 3 by 300 DEG C or more removes water
Processing.The feed hydrogen pipeline connecting with the feed hydrogen storage tank 4 is equipped with first flowmeter 9, connects with the light isotope storage tank 5
The light isotope pipeline connect is equipped with third flowmeter 11, sets on the heavy isotope pipeline connecting with the heavy isotope storage tank 6
There is second flowmeter 10.One is respectively provided on the pipeline that the feed hydrogen pipeline is connect with 1#~(n-2) # splitter 3 respectively to open
Valve is closed, the pipeline that the light isotope gas pipeline is connect with (n-1) # splitter 3 is equipped with a switch valve, the heavy same position
The pipeline that plain gas pipeline is connect with 1# splitter 3 is equipped with a switch valve, the vacuum pump 7 respectively with n is described separates
The pipeline that column 3 connects is equipped with a switch valve, is equipped with one on all pipelines connected between the adjacent splitter 3 and opens
Opening pressure difference is the adjustable check valve of 0.1MPa~0.5MPa, when pressure is more than that setting value can be to back segment point in previous splitter
From column one-way flow.
A kind of separation method of rotary low temperature hydrogen isotope separation system provided by the invention creatively utilizes simulation
Moving bed technique principle, hydrogen isotope can continuously circulate in closed loop splitter circuit, heavy isotope (deuterium, tritium) concentration
The proximal end desorbed from separating circuit is to distally gradually decreasing, and the concentration gradient of heavy isotope is with adsorption/desorption
Number, which increases, constantly to be increased, and this method flexible operation can easily obtain the heavy isotope of different abundance by technology controlling and process
And light isotope, separation method of the present invention the following steps are included:
1) n splitter is numbered sequence first, and number is respectively 1#, 2#, 3# ... (n-1) #, n#, then will
Each splitter is connected to vacuum pump, is opened vacuum pump and is extracted remaining gas in each splitter, backward cryostat, in injection liquid
Nitrogen is immersed in 1#~(n-1) # in liquid nitrogen, and the n# splitter for being located at turn around frame top is higher than liquid nitrogen liquid level；
2) valve that 1# splitter is connected to feed hydrogen storage tank is opened, feed hydrogen is injected into system, makes 1#~(n-1) #
Splitter reaches saturated extent of adsorption；
3) frequency control motor is opened, rotates reversing frame counterclockwise, 1# splitter is moved up and is detached from liquid nitrogen liquid level,
N# splitter, which moves down, simultaneously immerses in liquid nitrogen；1# splitter absorbs atmospheric heat, and hydrogen isotope desorption makes 1#~(n-1) #
Hydrogen isotope in splitter successively moves backward, and finally completes to reset for the first time in 2#~n# splitter；When 1# splitter
When hydrogen isotope release is completed, remaining hydrogen isotope in vacuum line abstraction 1# splitter, remaining hydrogen isotope warp are opened
It crosses after vacuum pump extracts and enters tail gas storage tank；
4) rotation reversing frame counterclockwise again, moves up 2# splitter and is detached from liquid nitrogen liquid level, 1# splitter is to moving down
It is dynamic to immerse in liquid nitrogen；2# splitter absorb atmospheric heat desorb hydrogen isotope gas, in each splitter hydrogen isotope successively to
After move, finally complete second in 3#~n# and 1# splitter and reset；When 2# splitter, which desorbs, to be completed, connection 2# is opened
Hydrogen isotope is remained in the vacuum line abstraction 2# splitter of splitter；
5) step 4 is repeated, the lock out operation of 3#~n-1# splitter is carried out respectively, makes hydrogen isotope in 1#~n# splitter
Sequence is mobile in the loop checking installation of composition, and the separation of hydrogen isotope is constantly promoted to reset；After the completion of the desorption of the n-th # splitter, hydrogen
Isotope has carried out n-th rearrangement, and hydrogen isotope is distributed in 1#~(n-1) # splitter again, and expression system, which completes, once to be followed
Ring separation；Hydrogen isotope forms significant hydrogen isotope concentration gradient, heavy isotope concentration at the top of the 1# splitter of circuit proximal end
Highest, and the heavy isotope concentration of (n-1) # of circuit distal end separation column bottom is minimum；
6) pipeline that light isotope storage tank is connect with (n-1) # splitter is opened, while opening frequency control motor to make to turn round
Frame rotates clockwise, and (n-1) # splitter is made to climb away liquid nitrogen liquid level, and light same position is discharged from the bottom of (n-1) # splitter
Element simultaneously collects the pipeline for having collected that closing light isotope storage tank is connect with (n-1) # splitter afterwards into light isotope storage tank；Later
The pipeline that heavy isotope storage tank is connect with 1# splitter is opened, while opening frequency control motor makes reversing frame by rotation counterclockwise
Turn, 1# splitter is made to climb away liquid level, heavy isotope is discharged from the top of 1# splitter and collects into heavy isotope storage tank；
7) to the isotope abundance sampling analysis in 2#~n-2# splitter, abundance and the close separation of feed hydrogen are chosen
Column injects feed hydrogen from its top, and the light isotope and heavy isotope collected in feed hydrogen injection rate and light isotope storage tank store up
The total collection for the heavy isotope collected in tank is equal；Then the lock out operation of next circulation is carried out；If one cycle separates
Light same position and heavy isotope abundance and extracted amount be not up to desired value, can by increase splitter quantity or cycle-index come
Bigger hydrogen isotope concentration gradient is obtained, to reach expected separating effect.
In order to make those skilled in the art of the present technique better understood when technical solution of the present invention, following instance is provided
Technical solution of the present invention is further elaborated.
Example 1: single cycle mode hydrogen isotope separation
This example selects 8 splitters, respectively 1#, 2#, 3#, 4#, 5#, 6#, 7# and 8# splitter, and each splitter is by volume
Number (1# → 2# →...→ 8# → 1#) is sequentially connected from head to tail to form closed circuit along clockwise direction；Place the reversing frame of splitter
It is placed in cryostat, cryostat, uses liquid nitrogen cooling, and the splitter at the top of reversing frame is located at liquid level or more, the submergence of remaining splitter
Below liquid level.This instance system further includes feed hydrogen storage tank, light isotope storage tank, heavy isotope storage tank, tail gas storage tank, flow
The pipeline and valve of meter, vacuum pump and the above-mentioned device of connection.
Splitter is the corrugated stainless steel tubing that outer diameter is DN50, wall thickness 0.2mm, length are 1000, the reachable 1MPa of pressure resistance,
Bellows both ends are plane-welding sealing structure, and end face connects 1/4 inch of stainless steel tube by cutting ferrule.Separating column packing is Φ 1
The 5A molecular sieve of~Φ 2, single-column loading amount are 1.3kg；Filler was heated to 350 DEG C before filling, kept the temperature 4h or more, carried out high temperature
Activation removes water process.Check valve (check valve number is V1~V8) is set between splitter, and check valve starting differential pressure is 0.1MPa
~0.5MPa is adjustable, when pressure can be to back segment splitter one-way flow more than setting value in splitter.
Reversing frame is by centre rotational axis and radially and the cylinder-shaped aluminium frame that constitutes of 1515 aluminum profiles of circumferencial direction arrangement
Frame, circle diameter 800 are circumferentially played the hole of diameter of phi 8, the welding of splitter both ends of the surface by 45° angle on aluminum profile spoke
1/4 inch of steel pipe be pierced by from the hole, splitter can be fixed on reversing frame.Reversing frame external connection is shown in Fig. 1, in reversing frame
The rotary shaft of the heart is the aluminum pipe of outer diameter Φ 40, wall thickness 2mm, and both ends extend to outside cryostat, and the left end of rotary shaft passes through shaft coupling
Frequency control motor is connected, for driving reversing frame to rotate, motor speed is 0.1~10 turn/min.The right end of rotary shaft connects
The inlet and outlet pipeline of Multi-path rotary connector, splitter all passes through the inner hole of rotary shaft and the rotor-end of Multi-path rotary connector
It is connected, the fixing end of rotary joint is connected by pipeline with matched valve control component.The both ends of rotary shaft are set with cryogenic bearing, low
Warm bearing is fixed on cryostat, inner wall.The position that rotary shaft passes through low temperature groove sidewall is sealed using low temperature glue, to prevent liquid
Nitrogen outflow.
It is formed according to above system, the separation method of rotary low temperature hydrogen isotope separation system utilizes Simulation moving bed
Principle, concrete methods of realizing are as follows:
(1) each splitter is connected into vacuum pump, extracts remaining gas in each column, liquid nitrogen is then injected into cryostat,
It is immersed in 1#~7# splitter in liquid nitrogen, the 8# splitter of top is higher than liquid level.
(2) 1# splitter inlet valve is opened, natural hydrogen (deuterium content about 150ppm) is injected into system, into 1#~7#
Splitter；When pressure reaches 0.02MPa (gauge pressure) in 7# column, feed hydrogen adsorption saturation is indicated, corresponding hydrogen absorption total amount is about
For 1000L.
(3) slewing equipment is rotated counterclockwise, 8# splitter is made to move down immersion liquid nitrogen, and 1# splitter moves up disengaging
Liquid level.Hydrogen isotope desorbs in 1# column, and pressure rises in column, when being more than unidirectional valve opening pressure 0.1MPa, hydrogen isotope
2# column is moved back into, and then the hydrogen isotope of 2# column is caused to enter 3# column by check valve, later separation column occurs similar
Process finally makes the hydrogen isotope in 1#~7# splitter fully enter 2#~8# splitter, completes to reset for the first time；The same position of weight
Plain concentration is gradually decreased along 2# → 8#.When in 1# splitter then pressure vacuumizes exclusion without significant changes expression desorption completion
1# column remnants hydrogen isotope makes its regeneration.
(4) it rotates slewing equipment counterclockwise again, so that 2# splitter is moved upwardly off liquid level, 1# splitter moves down
Immerse liquid nitrogen；2# column absorbs atmospheric heat and releases hydrogen isotope, and each column hydrogen isotope successively moves backward, finally in 3#~8# and
It completes to reset for second in 1# column.It is completed when 2# column desorbs, opens the vacuum line abstraction residual hydrogen isotope of connection 2# column.
(5) according to mode same as before, subsequent each post separation operation is carried out, makes hydrogen isotope in 1#~8# splitter group
At loop checking installation in sequentially move, be continuously improved hydrogen isotope separation effect.
(6) after the completion of the desorption of 8# splitter, hydrogen isotope has carried out the 8th rearrangement, and hydrogen isotope is distributed in again
1#~7# splitter, expression system complete one cycle separation；Hydrogen isotope forms significant hydrogen isotope concentration gradient, returns
The capital the 1# deuterium of road proximal end) concentration highest, the deuterium concentration at the 7# column bottom of distal end is minimum.
(7) weighing apparatus principle is kept with material according to infrastest data and carry out product extraction and raw material filling: connecting light isotope
Storage tank pipeline, moves swivel mount clockwise, and 7# splitter is made to climb away liquid level, and isotope desorbs in column, from column bottom
Light isotope is discharged, poor deuterium hydrogen collecting amount is about 110L, and deuterium concentration is about 10ppm；Heavy isotope storage tank pipeline is connected, counterclockwise
Mobile swivel mount, makes 1# splitter climb away liquid level, heavy isotope is discharged from column top, rich deuterium hydrogen collecting amount is about 30L, deuterium
Concentration is about 650ppm；3# splitter connects with unstripped gas abundance to be shown to the isotope abundance sampling analysis in 2#~6# splitter
Closely, feed hydrogen, injection rate 140L are injected at the top of 3#；The deuterium concentration gradient of band will not be distributed to hydrogen isotope based on which
Formation significantly affects.
(8) step (1)~(7) are repeated, separation can be carried out to natural hydrogen with semi-continuous mode and obtain deuterium concentration about 10ppm
Poor deuterium hydrogen and deuterium concentration be 650ppm rich deuterium hydrogen.
Example 2: the natural hydrogen separation of Two-way Cycle mode
Rotary low temperature hydrogen isotope separation system selected by example 2 is identical as example 1, and specific separation method is as follows:
I, step (1)~(6) operation in example 1 is carried out, one cycle separation is completed；
II, step (1)~(6) operation in example 1 is repeated, second of multi-cycle separation is completed；
III, light isotope storage tank pipeline is connected, moves swivel mount clockwise, 7# splitter is made to climb away liquid level, in column
Isotope desorbs, and light isotope is discharged from column bottom, poor deuterium hydrogen collecting amount is about 125L, and deuterium concentration is about 1ppm；It connects
Heavy isotope storage tank pipeline, moves swivel mount counterclockwise, and 1# splitter is made to climb away liquid level, from the column top same position of discharge weight
Element, rich deuterium hydrogen collecting amount are about 15L, and deuterium concentration is about 1400ppm；To the isotope abundance sampling analysis in 2#~6# splitter
Show that 2# splitter and unstripped gas abundance are close, injects feed hydrogen, injection rate 140L from the top 2#.
IV, step I~III is repeated, separation can be carried out to natural hydrogen with semi-continuous mode and obtain the poor of deuterium concentration about 1ppm
The rich deuterium hydrogen that deuterium hydrogen and deuterium concentration are 1400ppm.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention
It encloses, as long as that in body design thought of the invention and mentally makes has no the change of essential meaning or polishing, is solved
The technical issues of it is still consistent with the present invention, should all be included within protection scope of the present invention.
Claims (10)
1. a kind of rotary low temperature hydrogen isotope separation system, which is characterized in that including the interior cryostat, (1) for storing liquid nitrogen, installation
And it can be equidistant horizontal relative to the circular ring shape reversing frame (2) that the cryostat, (1) rotates freely in the cryostat, (1)
It is installed on the circumference of reversing frame (2) outer ring and can be stored with the n splitter (3) of the reversing frame (2) synchronous rotary
Feed hydrogen and the feed hydrogen storage tank (4) being connect respectively with 1#~(n-2) # splitter (3) by pipeline, for storing light isotope
And the light isotope storage tank (5) connect with (n-1) # splitter (3) by pipeline, for store heavy isotope and pass through pipeline and
The heavy isotope storage tank (6) of 1# splitter (3) connection, the vacuum pump being connect respectively with all splitters (3) by pipeline
(7), the tail gas storage tank (8) and with the vacuum pump (7) pipeline connecting；The n splitters (3) are in the reversing frame (2)
On pass sequentially through pipeline head and the tail connection in the direction of the clock and form closed circuit, one and only one in the n splitters (3)
Splitter (3) is located in cryostat, (1) more than the liquid level of liquid nitrogen, and the remaining n-1 splitters (3) are entirely located in cryostat,
(1) liquid level of liquid nitrogen is hereinafter, the tail gas storage tank (8) is connect with feed hydrogen storage tank (4) pipeline in, the n splitters
Successively it is numbered from 1#, 2#, 3# ... (n-1) #, n#.
2. a kind of rotary low temperature hydrogen isotope separation system according to claim 1, which is characterized in that the reversing frame
(2) include be horizontally installed in the cryostat, (1) and can relative to the rotary shaft (21) that the cryostat, (1) rotates freely,
And be located at the cryostat, (1) in and be installed on the rotary shaft (21) along longitudinal direction and can in company with the rotary shaft (21) together
The circular ring shape aluminium chassis (22) for walking rotation, on the circumference of the aluminium chassis (22) it is longitudinal equidistantly offer n respectively with described point
From the round clamping hole that column (3) matches, and the n splitters (3) are respectively arranged in the n circles and clamp in hole.
3. a kind of rotary low temperature hydrogen isotope separation system according to claim 2, which is characterized in that the rotary shaft
(21) both ends are extended to respectively outside the corresponding two sidewalls of the cryostat, (1), and one end of the rotary shaft (21) passes through shaft coupling
Device is connected with positioned at the cryostat, (1) outside for driving the frequency control motor (23) of the rotary shaft (21) rotation, described
The other end of rotary shaft (21) is connected with the Multi-path rotary connector connected outside for gas piping positioned at the cryostat, (1)
(24), the rotary shaft (21) is hollow aluminum pipe, is connected to the pipeline of the n splitters (3) by the rotary shaft
(21) inner cavity and the Multi-path rotary connector (24) cabling.
4. a kind of rotary low temperature hydrogen isotope separation system according to claim 3, which is characterized in that the rotary shaft
(21) both ends are respectively installed with a cryogenic bearing (25), and two cryogenic bearings (25) are flush-mounted in the cryostat, respectively
(1) in corresponding two sidewalls.
5. a kind of rotary low temperature hydrogen isotope separation system according to claim 4, which is characterized in that the splitter
(3) it is welded for both ends using flat seal and both ends of the surface connects corrugated stainless steel tubing, the splitter (3) by cutting ferrule respectively
Pressure resistance reaches 1MPa.
6. a kind of rotary low temperature hydrogen isotope separation system according to claim 5, which is characterized in that the splitter
(3) inorganic filler with low temperature hydrogen isotope effect is filled in, the inorganic filler is molecular sieve, aluminum oxide or silicon
Any one in glue, and the inorganic filler before being filled into the splitter (3) by 300 DEG C or more high
Temperature activation removes water process.
7. a kind of rotary low temperature hydrogen isotope separation system according to claim 6, which is characterized in that with the raw material
The feed hydrogen pipeline of hydrogen storage tank (4) connection is equipped with first flowmeter (9), and what is connect with the light isotope storage tank (5) is light same
The plain gas pipeline in position is equipped with third flowmeter (11), the heavy isotope gas pipeline connecting with the heavy isotope storage tank (6)
It is equipped with second flowmeter (10).
8. a kind of rotary low temperature hydrogen isotope separation system according to claim 7, which is characterized in that the feed hydrogen
A switch valve, the light isotope flue are respectively provided on the pipeline that pipeline is connect with 1#~(n-2) # splitter (3) respectively
The pipeline that road is connect with (n-1) # splitter (3) is equipped with a switch valve, the heavy isotope gas pipeline and 1# splitter
(3) on the pipeline that the pipeline connected is connect with the n splitters (3) respectively equipped with a switch valve, the vacuum pump (7)
It is respectively provided with a switch valve, being equipped with a starting differential pressure on all pipelines connected between the adjacent splitter (3) is
The adjustable check valve of 0.1MPa~0.5MPa.
9. a kind of rotary low temperature hydrogen isotope separation system according to claim 8, which is characterized in that the aluminium chassis
(22) it is made of 1515 aluminum profiles.
10. a kind of separation method of rotary low temperature hydrogen isotope separation system, which comprises the following steps:
1) n splitter is numbered sequence first, and number is respectively 1#, 2#, 3# ... (n-1) #, n#, then by each point
Be connected to from column with vacuum pump, open vacuum pump and extract remaining gas in each splitter, backward cryostat, in injection liquid nitrogen, make
1#~(n-1) # is immersed in liquid nitrogen, and the n# splitter for being located at turn around frame top is higher than liquid nitrogen liquid level；
2) valve that 1# splitter is connected to feed hydrogen storage tank is opened, feed hydrogen is injected into system, makes 1#~(n-1) # separation
Column reaches saturated extent of adsorption；
3) frequency control motor is opened, rotates reversing frame counterclockwise, 1# splitter is moved up and is detached from liquid nitrogen liquid level, simultaneously
N# splitter, which moves down, to be immersed in liquid nitrogen；1# splitter absorbs atmospheric heat, and hydrogen isotope desorption makes 1#~(n-1) # separation
Hydrogen isotope in column successively moves backward, and finally completes to reset for the first time in 2#~n# splitter；When 1# splitter hydrogen is same
When position element release is completed, remaining hydrogen isotope in vacuum line abstraction 1# splitter is opened；
4) it rotates reversing frame counterclockwise again, moves up 2# splitter and be detached from liquid nitrogen liquid level, 1# splitter moves down leaching
Enter in liquid nitrogen；2# splitter absorbs atmospheric heat and desorbs hydrogen isotope gas, and hydrogen isotope successively moves back in each splitter
It is dynamic, second is finally completed in 3#~n# and 1# splitter resets；When 2# splitter, which desorbs, to be completed, connection 2# separation is opened
Hydrogen isotope is remained in the vacuum line abstraction 2# splitter of column；
5) step 4 is repeated, carries out the lock out operation of 3#~n-1# splitter respectively, forms hydrogen isotope in 1#~n# splitter
Loop checking installation in sequence it is mobile, constantly promote the separation of hydrogen isotope to reset；After the completion of the desorption of the n-th # splitter, the same position of hydrogen
Element has carried out n-th rearrangement, and hydrogen isotope is distributed in 1#~(n-1) # splitter again, and expression system completes one cycle point
From；Hydrogen isotope forms significant hydrogen isotope concentration gradient, heavy isotope concentration highest at the top of the 1# splitter of circuit proximal end,
And the heavy isotope concentration of (n-1) the # separation column bottom of circuit distal end is minimum；
6) open the pipeline that light isotope storage tank is connect with (n-1) # splitter, at the same open frequency control motor make reversing frame by
It rotates clockwise, (n-1) # splitter is made to climb away liquid nitrogen liquid level, simultaneously from the bottom of (n-1) # splitter discharge light isotope
It collects and closes the pipeline that light isotope storage tank is connect with (n-1) # splitter after having collected into light isotope storage tank；It is open-minded later
The pipeline that heavy isotope storage tank is connect with 1# splitter, while opening frequency control motor makes reversing frame by rotation counterclockwise, makes
1# splitter climbs away liquid level, and heavy isotope is discharged from the top of 1# splitter and collects into heavy isotope storage tank；
7) to the isotope abundance sampling analysis in 2#~n-2# splitter, abundance and the close splitter of feed hydrogen are chosen, from
Feed hydrogen is injected at its top, is received in the light isotope and heavy isotope storage tank collected in feed hydrogen injection rate and light isotope storage tank
The total collection of the heavy isotope of collection is equal；Then the lock out operation of next circulation is carried out；If one cycle separation is light same
Position and heavy isotope abundance and extracted amount are not up to desired value, can be obtained more by increasing splitter quantity or cycle-index
Big hydrogen isotope concentration gradient, to reach expected separating effect.
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