CN106474924A - A kind of enrichment method of trace tritium - Google Patents
A kind of enrichment method of trace tritium Download PDFInfo
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- CN106474924A CN106474924A CN201610980213.4A CN201610980213A CN106474924A CN 106474924 A CN106474924 A CN 106474924A CN 201610980213 A CN201610980213 A CN 201610980213A CN 106474924 A CN106474924 A CN 106474924A
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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
Abstract
The invention provides a kind of enrichment method of trace tritium.The present invention adopts the united mode of operation of twin columns, can expand separating power while reducing pressure drop, and the separating power of single detached dowel can be overcome to be unable to, because of pressure drop, the defect that is extended.Working temperature constant of the present invention, can overcome the shortcomings of the high energy consumption that other alternating temperature separation methods lead to.The method that the present invention provides is semicontinuous separation, the semicontinuous extraction of the semicontinuous charging of achievable raw material and product, tail gas.Semicontinuous separating experiment result shows, after the protium hydrogen tritide isotope mixed gas for 100ppm for the tritium abundance are enriched with through the enrichment method that the present invention provides, total extraction ratio of product and tail gas is 10%, and the tritium abundance of product gas is about 1000ppm, and the tritium level in tail gas is about 1～2ppm.
Description
Technical field
The present invention relates to technical field of isotope separation, particularly to a kind of enrichment method of trace tritium in hydrogen isotope.
Background technology
ITER construction, Chinese fusion engineering experiment heap construction, the inland construction of nuclear power station and relate to tritium
Elimination of nuclear facilities etc. all proposes demand to the concentration and separation of trace tritium in extensive hydrogen isotope.
For the hydrogen isotope separation technology of current international mature, cryogenic rectification method complex process, disposable input
Larger, construction cost and operating cost are high；Thermal diffusion method separation hydrogen isotope needs high thermograde, separates column radius not
Can expand leads to separating power limited；Separation material in the chromatographic column of palladium displacement chromatography is often to carry palladium or palladium-based materials,
For extensive separation because cost is too high and inapplicable, and it is based on molecular sieve, Woelm Alumina, activated carbon, carbon-based molecular sieve etc.
The chromatographic isolation technique of low-cost sorbent is expected to be used for the separation of low tritium abundance hydrogen isotope on a large scale.
In terms of low tritium abundance chromatographic isolation hydrogen isotope on a large scale, pressure-variable adsorption can be divided into separate and to separate with temp.-changing adsorption
Two ways.Temp.-changing adsorption separate need repeatedly to heat with liquid nitrogen cooling lead to operating cost higher, and pressure-variable adsorption mode because
The separation of hydrogen isotope is realized in the change of dependence pressure, and temperature keeps constant, therefore can significantly reduce operating cost.Base of the present invention
In characterization of adsorption on molecular screen material for the hydrogen isotope it is proposed that the method for twin columns Vacuum Pressure Swing Adsorption.
Content of the invention
It is an object of the invention to provide a kind of efficiently, trace tritium method in energy-conservation, extensive enrichment hydrogen isotope, tritium is rich
After spending the enrichment method enrichment that protium hydrogen tritide isotope mixed gas for 100ppm provide through the present invention, the tritium abundance of product gas
It is about 1000ppm, the tritium level in tail gas is about 1～2ppm.
In order to realize foregoing invention purpose, the present invention provides technical scheme below：
The present invention comprises the steps：
(1) the first detached dowel and the second detached dowel are activated；
(2) the first detached dowel after described activation and the second detached dowel are carried out pre-cooling；
(3) unstripped gas to be separated the first detached dowel after described pre-cooling, is once enriched with tritium gas；
The tail gas of (4) first detached dowels separates column outlet by described first and flows out；
(5) tritium gas being once enriched with described first detached dowel is passed through the second detached dowel, secondary enrichment tritium gas, tail gas by
Described second separates column outlet flows out；
(6) during described secondary enrichment tritium gas, be passed through described second detached dowel also includes raw material to be separated
Gas；
(7), after described secondary enrichment tritium gas, collect the gas in described first detached dowel；
(8) tritium gas of secondary enrichment in described second detached dowel is passed through the first detached dowel, three enrichment tritium gas；
(9) during described three times enrichment tritium gas, be passed through described first detached dowel also includes raw material to be separated
Gas；
(10), after described three enrichment tritium gas, collect the gas in described second detached dowel；
Gas in second detached dowel of the gas in the first detached dowel of described collection and collection is what enrichment obtained
Tritium gas.
Preferably, after described step (10) is terminated, using the product gas collected as unstripped gas, according to described step (4)
～step (10) is a circulation, proceeds multiple circulation collection.
Preferably, be filled with molecular sieve in described first detached dowel, molecular sieve for 70～85g/mm3；
Be filled with molecular sieve in described second detached dowel, molecular sieve for 70～85g/mm3；
The particle diameter of described molecular sieve is 1～2mm；The porosity of described molecular sieve is -0.45～0.55.
Preferably, in separation process the temperature of the first detached dowel and the second detached dowel constant all the time for -190～-200 DEG C.
Preferably, the temperature of described activation is 280～320 DEG C；
The vacuum pressure of described activation is less than or equal to 10Pa；
The time of described activation is more than 20 hours.
Preferably, the temperature constant of described pre-cooling is -200～-190 DEG C.
Preferably, during described once enrichment tritium gas, the flow of unstripped gas is 0.5～2.5L/min.
Preferably, the flow of the tritium gas being once enriched with during described secondary enrichment tritium gas is 0.5～2.5L/min；
During described secondary enrichment tritium gas, the flow of unstripped gas is 0.5～1.5L/min.
Preferably, during described three enrichment tritium gas, the flow of the tritium gas of secondary enrichment is 0.5～2.5L/min；
During described three enrichment tritium gas, the flow of unstripped gas is 0.5～1.5L/min.
Preferably, described collect the first detached dowel in gas when, the pressure in the first detached dowel be 90～110Pa；
Described collect the second detached dowel in gas when, the pressure in the second detached dowel be 90～110Pa.
The present invention adopts the united mode of operation of twin columns, can expand separating power while reducing pressure drop, can
The separating power of single detached dowel is overcome to be extended because of the method that the problem of pressure drop is unable to simply by increasing column length
Defect.The present invention, by the way of constant temperature transformation, can overcome the shortcomings of the high energy consumption leading to because of intermittent warming.Experimental result
Show, after the protium hydrogen tritide isotope mixed gas for 100ppm for the tritium abundance are enriched with through the enrichment method that the present invention provides, product
Total extraction ratio with tail gas is 10%, and the tritium abundance of product gas is about 1000ppm, and the tritium level in tail gas is about 1～2ppm.
Brief description
The process chart of the enrichment method of the trace tritium that Fig. 1 provides for the embodiment of the present invention 1；
In figure：1- first detached dowel, 2- second detached dowel, 3- head tank, 4- products pot, 5- tail gas tank, 6- circulating pump.
Specific embodiment
The invention provides a kind of enrichment method of trace tritium, comprise the steps：
(1) the first detached dowel and the second detached dowel are activated；
(2) the first detached dowel after described activation and the second detached dowel are carried out pre-cooling；
(3) unstripped gas to be separated the first detached dowel after described pre-cooling, is once enriched with tritium gas；
The tail gas of (4) first detached dowels separates column outlet by described first and flows out；
(5) tritium gas being once enriched with described first detached dowel is passed through the second detached dowel, secondary enrichment tritium gas, tail gas by
Described second separates column outlet flows out；
(6) during described secondary enrichment tritium gas, be passed through described second detached dowel also includes raw material to be separated
Gas；
(7), after described secondary enrichment tritium gas, collect the gas in described first detached dowel；
(8) tritium gas of secondary enrichment in described second detached dowel is passed through the first detached dowel, three enrichment tritium gas；
(9) during described three times enrichment tritium gas, be passed through described first detached dowel also includes raw material to be separated
Gas；
(10), after described three enrichment tritium gas, collect the gas in described second detached dowel；
Gas in second detached dowel of the gas in the first detached dowel of described collection and collection is what enrichment obtained
Tritium gas.
First detached dowel and the second detached dowel are activated by the present invention.The present invention is to described first detached dowel and second point
Structure from post does not have particular/special requirement, using detached dowel well-known to those skilled in the art.In the present invention, described
The structure of one detached dowel and the second detached dowel is identical.In a specific embodiment of the present invention, described first detached dowel
Length is preferably 1m, and the internal diameter of described first detached dowel is preferably 16mm；The length of described second detached dowel is preferably 1m, described
The internal diameter of the second detached dowel is preferably 16mm.
In the present invention, preferably load molecular sieve in described first detached dowel and the second detached dowel.In the present invention, described
The specifically commercially available product type of molecular sieve can be 5A and 13X.The present invention selects the molecular sieve structure using stable, the irradiation of resistance to tritium,
Regenerating easily after adsorbing contaminant, the materials'use life-span significantly extends.In the present invention, the particle diameter of described molecular sieve be preferably 1～
2mm, more preferably 1.2～1.8mm, most preferably 1.4～1.6mm；The porosity of described molecular screen material be preferably -0.45～
0.55, more preferably -0.25～0.35, most preferably -0.15～0.15.
In the present invention, the loading density of the molecular sieve in described first detached dowel is preferably 70～85g/mm3, more preferably
For 78～83g/mm3, most preferably 80g/mm3.In the present invention, the loading density of the molecular sieve in described second detached dowel is excellent
Elect 70～85g/mm as3, more preferably 78～83g/mm3, most preferably 80g/mm3.In a specific embodiment of the present invention
In, in described first detached dowel and the second detached dowel, the loading density of molecular sieve is 78.5g/mm3.
The present invention does not have particular/special requirement to the specific embodiment of described activation, using well-known to those skilled in the art
Activation method carries out activating, and is specifically as follows heating, vacuum activation.In the present invention, the temperature of described activation is preferably
280～320 DEG C, more preferably 290～310 DEG C, most preferably 295～300 DEG C；The vacuum pressure of described activation is preferably smaller than etc.
In 10Pa, more preferably less than it is equal to 9Pa, be most preferably less than equal to 8Pa；The preferably greater than 20 hours time of described activation,
It is more preferably greater than 25 hours and is less than 50 hours, be most preferably more than 30 hours and be less than 40 hours.
The first detached dowel after described activation and the second detached dowel are carried out pre-cooling by the present invention.In the present invention, described pre-
Cold temperature is preferably -200～-190 DEG C, more preferably -198～-194 DEG C, most preferably -196 DEG C.In the present invention one
In specific embodiment, the present invention preferably carries out pre-cooling by being placed in described first detached dowel and the second detached dowel in liquid nitrogen,
More preferably whole process carries out the enrichment of described trace tritium under liquid nitrogen temperature.
After described pre-cooling, the present invention first detached dowel after described pre-cooling by unstripped gas to be separated, once it is enriched with
Tritium gas, tail gas separates column outlet by described first and flows out.In the present invention, described unstripped gas is the protium tritium of 100ppm for tritium abundance
Hydrogen isotope mixed gas.In the present invention, described once enrichment tritium gas during unstripped gas flow be preferably 0.5～
2.5L/min, more preferably 0.8～2.3L/min, most preferably 2L/min；Unstripped gas during described once enrichment tritium gas
Feed time preferably 5～20 minutes, more preferably 8～15 minutes, most preferably 10～12 minutes.Present invention preferably uses it is former
Batch can, head tank is connected with the arrival end of the first detached dowel, is once enriched with tritium gas.In the present invention, described once rich
After collection tritium gas, the pressure in the first detached dowel is preferably 90～110kPa, more preferably 95～105kPa, most preferably
100kPa.
In the present invention, after described once enrichment tritium gas, tail gas is flowed out by the outlet of the first detached dowel, described tail gas stream
The flow going out is preferably 0.5～1.5L/min, more preferably 0.8～1.3L/min, most preferably 1L/min.In the present invention,
Described tail gas preferably flows in tail gas reception system, the outlet phase of the entrance of described tail gas reception system and described first detached dowel
Connection；After described once enrichment tritium gas, during, flow out tail gas and stop preferably when tail gas tritium abundance reaches 1～2ppm, more
It is preferably 1.2～1.8ppm, most preferably 1.5ppm.In the present invention, described tail gas reception system is preferably tail gas tank.
After described once enrichment, the tritium gas being once enriched with described first detached dowel is passed through the second detached dowel by the present invention,
Secondary enrichment tritium gas, tail gas separates column outlet by described second and flows out；During described secondary enrichment tritium gas, it is passed through described
Second detached dowel also include unstripped gas to be separated.In the present invention, during described secondary enrichment tritium gas, described first point
The tritium gas being once enriched with post flows into the entrance of the second detached dowel by the outlet of the first detached dowel；The described tritium gas being once enriched with
Flow be preferably 0.5～2.5L/min, more preferably 0.8～2.3L/min, most preferably 2L/min.In the present invention, institute
State secondary enrichment tritium gas during unstripped gas by head tank flow into the second detached dowel entrance；The flow of described unstripped gas is preferably
0.5～1.5L/min, more preferably 0.8～1.3L/min, most preferably 1L/min；The inlet amount of described unstripped gas is preferably 3
～5L, can be specifically 3L, 4L or 5L.
In the middle of secondary enrichment process of the present invention, described tail gas is flowed out by the outlet of the second detached dowel；Described tail gas
The flow flowing out is preferably 0.5～1.5L/min, more preferably 0.8～1.3L/min, most preferably 1L/min；Described tail gas stream
Go out and preferably stop when the tritium abundance flowing out tail gas reaches 1～2ppm, more preferably 1.2～1.8ppm, most preferably 1.5ppm.
During secondary enrichment tritium gas of the present invention, described unstripped gas is preferably flowing into described the by the first detached dowel
Tritium abundance in the gas of two detached dowels reaches and starts during 90～110ppm to feed, more preferably 95～105ppm, most preferably
100ppm.In the present invention, described secondary enrichment tritium gas preferably stops when the pressure of the first detached dowel is 90～110Pa, more
It is preferably 95～105Pa, most preferably 100Pa.
During described secondary enrichment tritium gas, pressure reduction between the first detached dowel and the second detached dowel can be from being just changed into
Negative.When pressure reduction between the first detached dowel and the second detached dowel is zero, the present invention preferably connects first respectively by circulating pump
The outlet of detached dowel and the entrance of the second detached dowel, continue to make the first detached dowel feed to the second detached dowel.
The present invention, after described secondary enrichment tritium gas, collects the gas in described first detached dowel.In the present invention, receive
The flow collecting the gas in described first detached dowel is preferably 0.5～2.5L/min, more preferably 0.8～2.3L/min, optimum
Elect 2L/min as；The gas collected in described first detached dowel preferably stops when the pressure of the first detached dowel is 15～25Pa,
More preferably 18～23Pa, most preferably 20Pa.The present invention preferably passes through circulating pump by the entrance of the first detached dowel and products pot
Connect, collect the gas in described first detached dowel.
The tritium gas of secondary enrichment in described second detached dowel is passed through the first detached dowel, three enrichment tritium gas by the present invention；?
During described three enrichment tritium gas, be passed through described first detached dowel also includes unstripped gas to be separated.In the present invention,
The flow preferably 0.5～2.5L/min of the tritium gas of secondary enrichment during described three enrichment tritium gas, more preferably 0.8～
2.3L/min, most preferably 2L/min.In the present invention, during described three enrichment tritium gas, the flow of unstripped gas is preferably
0.5～1.5L/min, more preferably 0.8～1.3L/min, most preferably 1L/min；The inlet amount of described unstripped gas is preferably 3
～5L, can be specifically 3L, 4L or 5L.
In the present invention, described unstripped gas preferably start when the tritium abundance of the first detached dowel reaches 90～110ppm into
Material, more preferably 95～105ppm, most preferably 100ppm；Being enriched with tritium gas described three times in the pressure of the second detached dowel is preferably
Stop during 90～110Pa, more preferably 95～105Pa, most preferably 100Pa.
After described three enrichment tritium gas, the present invention collects the gas in described second detached dowel.In the present invention, collect
The flow of the gas in described second detached dowel is preferably 0.5～2.5L/min, more preferably 0.8～2.3L/min, most preferably
For 2L/min；The gas collected in described second detached dowel preferably stops when the pressure of the second detached dowel is 15～25Pa, more
It is preferably 18～23Pa, most preferably 20Pa.The present invention preferably passes through circulating pump and separates column inlet and products pot connection by second,
Collect the gas in described second detached dowel.
The present invention, after described step (10) terminates, is a circulation according to described step (4)～step (10), continues
It is circulated enrichment.The present invention does not have particular/special requirement to the cycle-index of described circulation collection, can be wanted according to actual technology
Ask and set.
In the enrichment process of trace tritium of the present invention, described tritium abundance is preferably detected by ionization chamber；Described pressure reduction
Preferably detected by pressure transducer；Described flow is preferably detected by effusion meter.
After the enrichment process of described trace tritium terminates, the present invention is preferably by the entrance of the first detached dowel and the second detached dowel
End is connected with head tank；After described connection, the first detached dowel and the second detached dowel are preferably departed from liquid nitrogen by the present invention simultaneously, put
Under room temperature environment.Under described room temperature environment, the gas in the first detached dowel and the second detached dowel can be spontaneous to head tank
Middle inflow.When the first detached dowel and the second detached dowel are equal with the pressure of head tank, present invention preferably employs circulating pump makes
Gas in one detached dowel and the second detached dowel is transferred to head tank, until the air pressure in detached dowel is less than 10Pa.
The invention provides a kind of enrichment method of trace tritium.The present invention adopts the united mode of operation of twin columns, is reducing
Separating power can be expanded, the separating power that can overcome single detached dowel can not because of the problem of pressure drop while pressure drop
Enough defects being extended simply by the method increasing column length.The method that the present invention provides, separates column temperature in separation process
In constant all the time can overcome the shortcomings of, at -190～-200 degrees Celsius, the high energy consumption that intermittent warming technique leads to, and separate imitate
Rate significantly improves.The clastotype of the method that the present invention provides is semicontinuous separation, the semicontinuous charging of achievable raw material and product
Product, the semicontinuous extraction of tail gas.Test result indicate that, tritium abundance is the protium hydrogen tritide isotope mixed gas of 100ppm through the present invention
After the enrichment method enrichment providing, total extraction ratio of product and tail gas is 10%, and the tritium abundance of product gas is about 1000ppm,
Tritium level in tail gas is about 1～2ppm.
The enrichment method of the trace tritium present invention being provided with reference to embodiment is described in detail, but can not be
They are interpreted as limiting the scope of the present invention.
Embodiment 1
Unstripped gas in this enforcement is the protium hydrogen tritide isotope mixed gas of 100ppm for tritium abundance.In this example, first
The column length of detached dowel and the second detached dowel is 1m, separates column internal diameter and is 16mm, charge is 157g, and bed voidage is equal
For 0.48.This example adopts spherical 5A molecular sieve, and particle size is 1～2mm, and porosity is 0.51.
1. detached dowel activation：The first detached dowel and the second detached dowel that have loaded 5A molecular sieve are heated to 300 DEG C and protect
Temperature.Meanwhile, evacuation process is carried out using vacuum pump, treat that the reduced pressure in the first detached dowel and the second detached dowel to 10Pa and adds
The hot time be 20 little constantly stop heating and evacuate, close detached dowel terminal valve and be simultaneously air cooled to room temperature.
2. detached dowel pre-cooling：Will be good for activation and be cooled to the first detached dowel of room temperature and the second detached dowel is simultaneously immersed in liquid nitrogen
Interior, cool time is 30min, to ensure that material is fully achieved thermal balance.
3. feed：Head tank is connected with the arrival end of the first detached dowel, unstripped gas start under the control of effusion meter to
First detached dowel charging, flow-control is 2.0 liters per minute, and feed time is 10 minutes, and charging terminates gas phase in rear detached dowel
Pressure is 100kPa.
4. semicontinuous separation：
The process chart of the enrichment method of trace tritium that the present invention provides is as shown in figure 1, in figure：1- first detached dowel,
2- second detached dowel, 3- head tank, 4- products pot, 5- tail gas tank, 6- circulating pump.The enrichment being provided according to Fig. 1, the present invention
The technological process of method is specific as follows：
Connection first separates column outlet and tail gas tank, under pressure reduction and effusion meter control, gas in the first detached dowel by
First separates column outlet shifts into tail gas tank, and flow is 1.0 liters/min；Tritium abundance is monitored using ionization chamber, when tritium abundance is high
Stop first and separate the gas transfer to tail gas tank for the column outlet when 1.5ppm；
First separates column outlet is connected with the entrance of the second detached dowel, under pressure reduction and effusion meter control, the first detached dowel
Interior gas separates column outlet from first and shifts to the second detached dowel, and flow is 2.0 liters/min；Rich using ionization chamber monitoring tritium
Degree, when tritium abundance rises to 100ppm, the entrance of the second detached dowel is separated simultaneously column outlet and head tank connection with first,
Under pressure reduction and effusion meter control, the gas in the first detached dowel and head tank flows simultaneously into the second detached dowel, feed gas flow rates
It is controlled to 1.0 liters/min, inlet amount is controlled to 4.0 liters；After charging terminates, cut-off head tank separates between column inlet with second
Connection, the gas in the first detached dowel continues to shift to the second detached dowel；
After the pressure that the first separation column outlet and second separates column inlet is equal, using circulating pump by the first detached dowel
Gas continue into the second detached dowel transfer, until the reduced pressure in the first detached dowel is to 100Pa；
Pump entry is connected with the entrance of the first detached dowel, circulating-pump outlet is connected with products pot；Make in circulating pump
With under, the gas in the first detached dowel shifts into products pot, until the reduced pressure in the first detached dowel exit is to 20Pa；
The outlet of the second detached dowel is connected with tail gas tank, and under the control of pressure reduction and effusion meter, gas is by the second detached dowel
Outlet to tail gas tank shift, flow be 1.0 liters/min；Tritium abundance is monitored using ionization chamber, when tritium abundance is higher than 1.5ppm
Stop first and separate the gas transfer to tail gas tank for the column outlet；
Second separates column outlet is connected with the entrance of the first detached dowel, under pressure reduction and effusion meter control, the second detached dowel
Interior gas separates column outlet from second and shifts to the first detached dowel, not higher than 2.0 liters/min of flow；Using ionization chamber monitoring
Tritium abundance, when tritium abundance rises to 100ppm, the entrance of the first detached dowel is separated column outlet and head tank with second simultaneously
Connection, under pressure reduction and effusion meter control, the gas in the second detached dowel and head tank flows simultaneously into the first detached dowel, unstripped gas
Not higher than 1.0 liters/min of flow speed control, inlet amount is controlled to 4.0 liters；After charging terminates, cut-off head tank is entered with the first detached dowel
Connection between mouthful, the gas in the second detached dowel continues to shift to the first detached dowel；
After the pressure that the first separation column inlet and second separates column outlet is equal, using circulating pump by the second detached dowel
Gas continue to shift to the first detached dowel, until the reduced pressure in the second detached dowel is to 100Pa；
Pump entry is connected with the entrance of the second detached dowel, circulating-pump outlet is connected with products pot；Make in circulating pump
With under, gas in the second detached dowel shifts to products pot, until the reduced pressure of the second detached dowel porch is to 20Pa.
Repeat above-mentioned semicontinuous separating step, until having processed the unstripped gas of a batch.
5. separate and terminate
At the end of separating, the arrival end of two detached dowels is connected with raw material gas tank；Subsequently two detached dowels are departed from liquid
Nitrogen as in normal temperature environment；Gas in molecular sieve is spontaneous to be desorbed and flows in head tank；When the pressure in detached dowel no longer
During change, using circulating pump, the gas in detached dowel is continued to be transferred to head tank, until the pressure in detached dowel is less than 10Pa；
Finally close the valve of head tank.
It is computed understanding, total extraction ratio of product and tail gas is 10%, and the tritium abundance of product gas is about 1000ppm, tail gas
In tritium level be about 1～2ppm.
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of enrichment method of trace tritium, comprises the steps：
(1) the first detached dowel and the second detached dowel are activated；
(2) the first detached dowel after described activation and the second detached dowel are carried out pre-cooling；
(3) unstripped gas to be separated the first detached dowel after described pre-cooling, is once enriched with tritium gas；
The tail gas of (4) first detached dowels separates column outlet by described first and flows out；
(5) tritium gas being once enriched with described first detached dowel is passed through the second detached dowel, secondary enrichment tritium gas, tail gas is by described
Second separates column outlet flows out；
(6) during described secondary enrichment tritium gas, be passed through described second detached dowel also includes unstripped gas to be separated；
(7), after described secondary enrichment tritium gas, collect the gas in described first detached dowel；
(8) tritium gas of secondary enrichment in described second detached dowel is passed through the first detached dowel, three enrichment tritium gas；
(9) during described three times enrichment tritium gas, be passed through described first detached dowel also includes unstripped gas to be separated；
(10), after described three enrichment tritium gas, collect the gas in described second detached dowel；
Gas in second detached dowel of the gas in the first detached dowel of described collection and collection is as enriched with the tritium gas obtaining.
2. the enrichment method of trace tritium according to claim 1, will it is characterised in that after described step (10) terminates
Described step (4)～step (10), as a circulation step, proceeds circulation collection.
3. the enrichment method of trace tritium according to claim 1 is it is characterised in that be filled with described first detached dowel point
Son sieve, molecular sieve for 70～85g/mm3；
Be filled with molecular sieve in described second detached dowel, molecular sieve for 70～85g/mm3；
The particle diameter of described molecular sieve is 1～2mm；The porosity of described molecular sieve is -0.45～0.55.
4. the enrichment method of trace tritium according to claim 1 is it is characterised in that the first detached dowel and in separation process
The temperature of two detached dowels constant all the time for -190～-200 DEG C.
5. the enrichment method of trace tritium according to claim 1 is it is characterised in that the temperature of described activation is 280～320
℃；
The vacuum pressure of described activation is less than or equal to 10Pa；
The time of described activation is more than 20 hours.
6. the enrichment method of trace tritium according to claim 1 is it is characterised in that the temperature constant of described pre-cooling is -200
～-190 DEG C.
7. trace tritium according to claim 1 enrichment method it is characterised in that described once enrichment tritium gas process in former
The flow of material gas is 0.5～2.5L/min.
8. trace tritium according to claim 1 enrichment method it is characterised in that described secondary enrichment tritium gas during one
The flow of the tritium gas of secondary enrichment is 0.5～2.5L/min；
During described secondary enrichment tritium gas, the flow of unstripped gas is 0.5～1.5L/min.
9. the enrichment method of trace tritium according to claim 1 is it is characterised in that described three times are enriched with two during tritium gas
The flow of the tritium gas of secondary enrichment is 0.5～2.5L/min；
During described three enrichment tritium gas, the flow of unstripped gas is 0.5～1.5L/min.
10. the enrichment method of trace tritium according to claim 1 is it is characterised in that in described collection first detached dowel
During gas, the pressure in the first detached dowel is 90～110Pa；
Described collect the second detached dowel in gas when, the pressure in the second detached dowel be 90～110Pa.
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