CN109289526B - Rotary low-temperature hydrogen isotope separation system and separation method - Google Patents
Rotary low-temperature hydrogen isotope separation system and separation method Download PDFInfo
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- CN109289526B CN109289526B CN201811098571.8A CN201811098571A CN109289526B CN 109289526 B CN109289526 B CN 109289526B CN 201811098571 A CN201811098571 A CN 201811098571A CN 109289526 B CN109289526 B CN 109289526B
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Abstract
The invention discloses a rotary low-temperature hydrogen isotope separation system and a rotary low-temperature hydrogen isotope separation method, which solve the problems that in the prior art, the construction is complicated, the parameter control is complicated, the operation cost is high, or the helium gas supply, the hydrogen-helium separation and the regeneration treatment of a separation column are required to be complicated, or a palladium replacement chromatographic filler is expensive and is easy to lose efficacy. The separation system comprises a low-temperature tank, a rotary frame, a separation column, a raw material hydrogen storage tank, a light isotope storage tank, a heavy isotope storage tank, a vacuum pump and a tail gas storage tank. The separation method comprises the steps of separating the separation columns adsorbing the raw material hydrogen from the liquid level of liquid nitrogen one by one to desorb hydrogen isotopes so as to complete rearrangement of the hydrogen isotopes in the other separation columns; finally, light and heavy isotopes are collected from the far end and the near end of the loop respectively. The invention creatively utilizes the technical principle of the simulated moving bed, the hydrogen isotope can continuously and circularly flow in the closed loop separation circuit, the concentration of the heavy isotope is gradually reduced from the near end to the far end of the separation circuit where desorption occurs, and the concentration gradient of the heavy isotope is continuously increased along with the increase of the times of adsorption/desorption.
Description
Technical Field
The invention relates to the field of nuclear technology application, in particular to a rotary type low-temperature hydrogen isotope separation system and a separation method.
Background
The separation of hydrogen isotopes is one of core technologies of the fusion reactor deuterium-tritium nuclear fuel circulation, and by isotope separation, a large amount of uncombusted deuterium-tritium gas in the operation of a reactor can be reused, and the effective control of the environmental release amount of tritium in the operation process of the fusion reactor can be realized. In order to meet the requirement of the future fusion reactor operation on large-scale hydrogen isotope separation, a series of hydrogen isotope separation technologies including low-temperature distillation (LHD), low-temperature chromatography (GC), palladium replacement chromatography and the like have been developed.
The cryogenic rectification method utilizes the difference of boiling points of different hydrogen isotope molecules for separation. Six molecules of hydrogen isotopes (H)2、HD、D2DT, HT and T2) In the temperature range of 20K to 25K, there is a slight difference in their boiling points, where H2Maximum, T2And the lowest. The low-temperature rectifying column is operated at the liquid hydrogen temperature to realize isotope separation by taking liquid helium as a refrigeration source. The low-temperature rectification method has the defects of complex structure and process operation of a separation system, high energy consumption, large tritium storage capacity of the separation system, high system construction and operation cost and the like.
Low temperature chromatography uses the chromatographic effect of cryoadsorptive materials for separation. When helium passes through a 5A molecular sieve separation column pre-adsorbed with hydrogen isotope mixed gas at the liquid nitrogen temperature of (-196 ℃), H will appear in the effluent gas in sequence when the separation column is long enough due to different adsorption capacities of the molecular sieve to different components in the hydrogen isotope mixed gas at low temperature2、HD、HT、D2DT and T2Peaks of completely separated six hydrogen isotope molecules, the longer the separation column, the larger the interval between peaks. Collecting at peak position in different time periods, six different hydrogen isotope gases can be obtained. The disadvantages of this separation method are that the separation must be carried out at liquid nitrogen temperature, the cooling of the separation column consumes a large amount of liquid nitrogen, the energy consumption is high and the extraction ratio of the product gas from a single separation is low.
Palladium displacement chromatography utilizes the isotope effect of palladium in forming a hydride for isotope separation. The metallic palladium has a strong hydrogen isotope separation effect, the light isotope component protium (H) reacts with the metallic palladium more easily to generate a more stable solid palladium hydride than the heavy isotope components deuterium (D) and tritium (T), and when equilibrium is reached, the partial pressure of the heavy isotope component in the gas phase is relatively high and the separation effect is greater the lower the temperature. The current subdivision methods comprise palladium heat replacement chromatography, heat cycle adsorption and the like. The method has the disadvantages that expensive palladium is used as a separating column filler, and the repeated hydrogen absorption and hydrogen desorption in the separation process can cause the hydrogen absorption characteristics of the separating material palladium to be changed undesirably, such as pulverization of the separating material, change of the hydrogen absorption characteristics caused by interaction of the palladium and a palladium carrier material, and the like, so that the effective life of the separating column is short.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the rotary low-temperature hydrogen isotope separation system and the separation method solve the problems that a low-temperature rectification method system in the prior art is complex in construction, complex in parameter control and high in operation cost, a low-temperature chromatography method needs helium gas supply, hydrogen-helium separation and separation column regeneration treatment are complex, a palladium replacement chromatographic packing is expensive and prone to failure, and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a rotary low-temperature hydrogen isotope separation system comprises a low-temperature tank internally storing liquid nitrogen, a circular ring-shaped rotary frame which is arranged in the low-temperature tank and can freely rotate relative to the low-temperature tank, and n separation columns which are horizontally arranged on the circumference of the outer ring of the rotary frame at equal intervals and can synchronously rotate along with the rotary frame, wherein the n separation columns are sequentially connected end to end through pipelines on the rotary frame in a clockwise direction to form a closed loop, and the n separation columns are sequentially numbered from No. 1, No. 2, No. 3# … … (n-1), and No. n. The separation system also comprises a raw material hydrogen storage tank which stores raw material hydrogen and is respectively connected with the 1# - (n-2) # separation columns through pipelines, a light isotope storage tank which is used for storing light isotopes and is connected with the (n-1) # separation columns through pipelines, a heavy isotope storage tank which is used for storing heavy isotopes and is connected with the 1# separation columns through pipelines, a vacuum pump which is respectively connected with all the separation columns through pipelines, and a tail gas storage tank which is connected with the vacuum pump through pipelines; the n separation columns are sequentially connected end to end through pipelines in a clockwise direction on the rotary frame to form a closed loop, only one separation column in the n separation columns is located above the liquid level of liquid nitrogen in the low-temperature tank, the rest n-1 separation columns are all located below the liquid level of the liquid nitrogen in the low-temperature tank, and the tail gas storage tank is connected with the raw material hydrogen storage tank through a pipeline.
Furthermore, the revolving frame comprises a rotating shaft which is horizontally arranged in the low-temperature tank and can freely rotate relative to the low-temperature tank, and a circular aluminum frame which is positioned in the low-temperature tank, is longitudinally arranged on the rotating shaft and can synchronously rotate along with the rotating shaft, n circular clamping holes which are respectively matched with the separating columns are longitudinally arranged on the outer circumference of the aluminum frame at equal intervals, and the n separating columns are respectively arranged in the n circular clamping holes.
Further, the both ends of rotation axis extend respectively outside the corresponding both sides wall of low temperature groove, the one end of rotation axis has through the coupling joint to be located the low temperature groove is used for the drive outward the rotatory variable frequency speed regulating motor of rotation axis, the other end of rotation axis is connected with and is located the outer multichannel rotary joint that is used for gas piping connection of low temperature groove, the rotation axis is hollow aluminum pipe, connects in n the pipeline of knockout column all passes through the inner chamber of rotation axis reaches the multichannel rotary joint is walked the line.
Furthermore, two ends of the rotating shaft are respectively sleeved with a low-temperature bearing, and the two low-temperature bearings are respectively embedded in two corresponding side walls of the low-temperature groove.
Furthermore, the two ends of the separation column are welded in a plane sealing mode, the two end faces of the separation column are respectively connected with the stainless steel corrugated pipe through the clamping sleeves, and the pressure resistance of the separation column reaches 1 MPa.
Further, the separation column is filled with an inorganic filler with a low-temperature hydrogen isotope effect, the inorganic filler is any one of a molecular sieve, aluminum oxide or silica gel, and the inorganic filler is subjected to high-temperature activation dehydration treatment at 300 ℃ or above before being filled into the separation column.
Furthermore, a first flowmeter is arranged on a raw material hydrogen pipeline connected with the raw material hydrogen storage tank, a third flowmeter is arranged on a light isotope pipeline connected with the light isotope storage tank, and a second flowmeter is arranged on a heavy isotope pipeline connected with the heavy isotope storage tank.
Furthermore, the pipelines of the raw material hydrogen pipeline respectively connected with the 1# - (n-2) # separation columns are respectively provided with a switch valve, the pipelines of the light isotope pipeline connected with the (n-1) # separation columns are respectively provided with a switch valve, the pipelines of the heavy isotope pipeline respectively connected with the 1# separation columns are respectively provided with a switch valve, the pipelines of the vacuum pump respectively connected with the n separation columns are respectively provided with a switch valve, and all the pipelines connected between the adjacent separation columns are respectively provided with a one-way valve with adjustable opening pressure difference of 0.1 MPa-0.5 MPa.
Further, the aluminum frame is made of 1515 aluminum profiles.
A separation method of a rotary low-temperature hydrogen isotope separation system comprises the following steps:
1) firstly, sequentially numbering n separation columns, wherein the numbering is 1#, 2#, 3# … … (n-1) #andn #, then communicating each separation column with a vacuum pump, starting the vacuum pump to pump out residual gas in each separation column, and then injecting liquid nitrogen into a low-temperature tank to ensure that 1# - (n-1) # is immersed in the liquid nitrogen, and the n # separation column positioned at the top end of a rotary frame is higher than the liquid level of the liquid nitrogen;
2) starting a valve for communicating the 1# separation column with the raw material hydrogen storage tank, and injecting the raw material hydrogen into the system to ensure that the 1# to (n-1) # separation columns reach the saturated adsorption capacity;
3) starting a variable-frequency speed regulating motor to enable the rotary frame to rotate anticlockwise, so that the 1# separation column moves upwards to be separated from the liquid level of liquid nitrogen, and the n # separation column moves downwards to be immersed in the liquid nitrogen; the 1# separation column absorbs air heat, hydrogen isotopes in the 1# to (n-1) # separation columns are sequentially moved backwards through hydrogen isotope desorption, and finally first rearrangement is completed in the 2# to n # separation columns; when the release of the hydrogen isotopes in the 1# separation column is finished, starting a vacuum pipeline to pump out the residual hydrogen isotopes in the 1# separation column;
4) rotating the revolving frame anticlockwise again to enable the 2# separation column to move upwards to be separated from the liquid level of the liquid nitrogen, and enable the 1# separation column to move downwards to be immersed in the liquid nitrogen; the 2# separation column absorbs the heat of the air to desorb hydrogen isotope gas, the hydrogen isotopes in each separation column move backwards in sequence, and finally secondary rearrangement is completed in the 3# to n # and 1# separation columns; when the desorption of the 2# separation column is finished, starting a vacuum pipeline connected with the 2# separation column to pump out residual hydrogen isotopes in the 2# separation column;
5) repeating the step 4, and respectively carrying out separation operations of the 3# to n-1# separation columns to enable the hydrogen isotopes to sequentially move in the annular loop formed by the 1# to n # separation columns, so as to continuously promote the separation and rearrangement of the hydrogen isotopes; after the n # separation column finishes desorption, the hydrogen isotopes are rearranged for the n number, and are distributed in the 1# - (n-1) # separation columns again, which indicates that the system finishes one-time circular separation; the hydrogen isotopes form a significant hydrogen isotope concentration gradient, the concentration of heavy isotopes (such as deuterium and tritium) at the top of the 1# separation column at the near end of the loop is the highest, and the concentration of heavy isotopes at the bottom of the (n-1) # separation column at the far end of the loop is the lowest;
6) opening a pipeline connecting the light isotope storage tank and the (n-1) # separation column, simultaneously starting a variable-frequency speed regulating motor to enable the rotary frame to rotate clockwise, enabling the (n-1) # separation column to rise and separate from the liquid nitrogen liquid level, discharging the light isotope from the bottom of the (n-1) # separation column and collecting the light isotope into the light isotope storage tank, and closing the pipeline connecting the light isotope storage tank and the (n-1) # separation column after the light isotope storage tank is collected; then, a pipeline connecting the heavy isotope storage tank and the 1# separation column is opened, and simultaneously, a variable-frequency speed regulating motor is started to enable the rotary frame to rotate anticlockwise, so that the 1# separation column rises to be separated from the liquid level, and the heavy isotopes are discharged from the top of the 1# separation column and collected into the heavy isotope storage tank;
7) sampling and analyzing the isotope abundance in the 2# to n-2# separation column, selecting the separation column with the abundance close to that of the raw material hydrogen, and injecting the raw material hydrogen from the top of the separation column, wherein the injection amount of the raw material hydrogen is equal to the total collection amount of the light isotopes collected in the light isotope storage tank and the heavy isotopes collected in the heavy isotope storage tank; then carrying out the next cycle of separation operation; if the abundance and extraction amount of the light isotope and the heavy isotope in one circulation separation do not reach the expected values, a larger hydrogen isotope concentration gradient can be obtained by increasing the number of the separation columns or the circulation times, so as to achieve the expected separation effect.
Compared with the prior art, the invention has the following beneficial effects:
the invention creatively utilizes the technical principle of a simulated moving bed, hydrogen isotopes can continuously and circularly flow in a closed-loop separation column loop, the concentration of heavy isotopes (deuterium and tritium) is gradually reduced from a near end to a far end of the separation loop, and the concentration gradient of the heavy isotopes is continuously increased along with the increase of the times of adsorption/desorption.
The invention is used for separating hydrogen isotopes, adopts the accumulative cycle separation operation, and has the advantages of obviously reduced system volume, simple parameter control, low hydrogen isotope retention in the system and greatly reduced operation energy consumption compared with a low-temperature rectification method.
The invention is used for hydrogen isotope separation, compared with the palladium replacement chromatography, the filling material is inorganic filling materials such as molecular sieve with low price, the palladium with high price is not needed to be used as the filling material, and the hydrogen absorption and desorption in the separation process is a physical process, the material property is stable, and the material can be used for a long time, thereby greatly reducing the system cost.
Compared with the traditional low-temperature chromatography, the method is used for separating the hydrogen isotopes, and does not need helium as carrier gas, so that the system structure is simpler, and the subsequent hydrogen/helium separation process link does not exist, so that the operation is simpler and more convenient. In addition, the separation system main body is in a hydrogen adsorption saturation state, so that the effective utilization rate of the separation column is higher, the system scale can be smaller, and the construction cost can be obviously reduced.
Compared with low-temperature rectification, conventional low-temperature chromatography and palladium replacement chromatography, the invention has the advantages of simple system structure, low-cost filler, convenient control, smaller equipment scale and lower construction cost, and can adopt a semi-continuous mode to carry out hydrogen isotope separation operation to obtain heavy isotopes and light isotopes.
Drawings
FIG. 1 is a schematic diagram of the separation system of the present invention.
FIG. 2 is a view showing the distribution of the separation columns on the turret in the separation system of the present invention.
FIG. 3 is a process layout of the separation system of the present invention.
Wherein, the names corresponding to the reference numbers are:
the device comprises a 1-low-temperature tank, a 2-revolving frame, a 3-separation column, a 4-raw material hydrogen storage tank, a 5-light isotope storage tank, a 6-heavy isotope storage tank, a 7-vacuum pump, an 8-tail gas storage tank, a 9-first flowmeter, a 10-second flowmeter, an 11-third flowmeter, a 21-rotating shaft, a 22-aluminum frame, a 23-variable-frequency speed-regulating motor, a 24-multi-channel rotating joint and a 25-low-temperature bearing.
Detailed Description
The present invention will be further described with reference to the following description and examples, which include but are not limited to the following examples.
As shown in fig. 1-3, the rotary low-temperature hydrogen isotope separation system provided by the invention has the advantages of simple system structure, low-cost filler, convenient control, smaller equipment scale and lower construction cost compared with low-temperature rectification, conventional low-temperature chromatography and palladium replacement chromatography, and can adopt a semi-continuous mode to perform hydrogen isotope separation operation to obtain heavy isotopes and light isotopes. The rotary low-temperature hydrogen isotope separation system comprises a low-temperature groove 1 for storing liquid nitrogen, a circular ring-shaped revolving frame 2 which is arranged in the low-temperature groove 1 and can freely rotate relative to the low-temperature groove 1, n separation columns 3 which are circumferentially and equidistantly horizontally arranged on the circumference of the outer ring of the revolving frame 2 and can synchronously rotate along with the revolving frame 2, a raw material hydrogen storage tank 4 which stores raw material hydrogen and is respectively connected with the 1# - (n-2) # separation columns 3 through a raw material hydrogen pipeline, a light isotope storage tank 5 for storing light isotopes and connected with the (n-1) separation column 3 through a pipeline, a heavy isotope storage tank 6 used for storing heavy isotopes and connected with the No. 1 separation column 3 through a pipeline, the vacuum pump 7 is respectively connected with all the separation columns 3 through pipelines, and the tail gas storage tank 8 is connected with the vacuum pump 7 through pipelines; the n separation columns 3 are sequentially connected end to end through pipelines in a clockwise direction on the rotary frame 2 to form a closed loop, only one separation column 3 in the n separation columns 3 is located above the liquid level of liquid nitrogen in the low-temperature tank 1, the rest n-1 separation columns 3 are all located below the liquid level of the liquid nitrogen in the low-temperature tank 1, the tail gas storage tank 8 is connected with the raw material hydrogen storage tank 4 through a pipeline, and the n separation columns are sequentially numbered from 1#, 2#, 3# … … (n-1) #andn #.
The rotary frame 2 of the rotary low-temperature hydrogen isotope separation system comprises a rotating shaft 21 which is horizontally arranged in the low-temperature tank 1 and can freely rotate relative to the low-temperature tank 1, and a circular aluminum frame 22 which is positioned in the low-temperature tank 1, is longitudinally arranged on the rotating shaft 21 and can synchronously rotate along with the rotating shaft 21, n circular clamping holes which are respectively matched with the separation columns 3 are longitudinally arranged on the outer circumference of the aluminum frame 22 at equal intervals, and the n separation columns 3 are respectively arranged in the n circular clamping holes. The both ends of rotation axis 21 extend respectively outside the corresponding both sides wall of low-temperature groove 1, the one end of rotation axis 21 is located through the coupling joint have low-temperature groove 1 is used for the drive outward the rotatory variable frequency speed motor 23 of rotation axis 21, the other end of rotation axis 21 is connected with and is located low-temperature groove 1 is used for the multichannel rotary joint 24 that the gas piping connects outward, rotation axis 21 is hollow aluminum pipe, connects in n the pipeline of separation post 3 all passes through the inner chamber of rotation axis 21 reaches multichannel rotary joint 24 walks the line. Two ends of the rotating shaft 21 are respectively sleeved with a low-temperature bearing 25, the two low-temperature bearings 25 are respectively embedded in two corresponding side walls of the low-temperature tank 1, and the aluminum frame 22 is made of 1515 aluminum profiles.
The two ends of the separation column 3 of the rotary low-temperature hydrogen isotope separation system are welded in a plane sealing mode, the two end faces of the separation column are respectively connected with a stainless steel corrugated pipe through a clamping sleeve, and the pressure resistance of the separation column 3 reaches 1 MPa. The separation column 3 is filled with an inorganic filler with a low-temperature hydrogen isotope effect, the inorganic filler is any one of a molecular sieve, aluminum oxide or silica gel, and the inorganic filler is subjected to high-temperature activation dehydration treatment at 300 ℃ or above before being filled into the separation column 3. A first flow meter 9 is arranged on a raw material hydrogen pipeline connected with the raw material hydrogen storage tank 4, a third flow meter 11 is arranged on a light isotope pipeline connected with the light isotope storage tank 5, and a second flow meter 10 is arranged on a heavy isotope pipeline connected with the heavy isotope storage tank 6. The raw material hydrogen pipeline is respectively provided with a switch valve on the pipeline connected with the 1# - (n-2) # separation column 3, the pipeline connected with the light isotope gas pipeline and the (n-1) # separation column 3 is provided with a switch valve, the pipeline connected with the heavy isotope gas pipeline and the 1# separation column 3 is provided with a switch valve, the pipeline connected with the n separation columns 3 by the vacuum pump 7 is provided with a switch valve, all the pipelines connected between the adjacent separation columns 3 are provided with a one-way valve with adjustable opening pressure difference of 0.1 MPa-0.5 MPa, and the pressure in the current one separation column exceeds a set value and can flow to the back section separation column in a one-way manner.
The invention provides a separation method of a rotary low-temperature hydrogen isotope separation system, which creatively utilizes the technical principle of a simulated moving bed, hydrogen isotopes can continuously and circularly flow in a closed loop separation column loop, the concentration of heavy isotopes (deuterium and tritium) is gradually reduced from a near end to a far end where desorption occurs in the separation loop, and the concentration gradient of the heavy isotopes is continuously increased along with the increase of the times of adsorption/desorption, the method has flexible operation, and the heavy isotopes and the light isotopes with different abundances can be conveniently obtained through process control, and the separation method comprises the following steps:
1) firstly, sequentially numbering n separation columns, wherein the numbering is 1#, 2#, 3# … … (n-1) #andn #, then communicating each separation column with a vacuum pump, starting the vacuum pump to pump out residual gas in each separation column, and then injecting liquid nitrogen into a low-temperature tank to ensure that 1# - (n-1) # is immersed in the liquid nitrogen, and the n # separation column positioned at the top end of a rotary frame is higher than the liquid level of the liquid nitrogen;
2) starting a valve for communicating the 1# separation column with the raw material hydrogen storage tank, and injecting the raw material hydrogen into the system to ensure that the 1# to (n-1) # separation columns reach the saturated adsorption capacity;
3) starting a variable-frequency speed regulating motor to enable the rotary frame to rotate anticlockwise, so that the 1# separation column moves upwards to be separated from the liquid level of liquid nitrogen, and the n # separation column moves downwards to be immersed in the liquid nitrogen; the 1# separation column absorbs air heat, hydrogen isotopes in the 1# to (n-1) # separation columns are sequentially moved backwards through hydrogen isotope desorption, and finally first rearrangement is completed in the 2# to n # separation columns; when the release of the hydrogen isotopes in the 1# separation column is finished, starting a vacuum pipeline to pump out the residual hydrogen isotopes in the 1# separation column, and pumping the residual hydrogen isotopes through a vacuum pump to enter a tail gas storage tank;
4) rotating the revolving frame anticlockwise again to enable the 2# separation column to move upwards to be separated from the liquid level of the liquid nitrogen, and enable the 1# separation column to move downwards to be immersed in the liquid nitrogen; the 2# separation column absorbs the heat of the air to desorb hydrogen isotope gas, the hydrogen isotopes in each separation column move backwards in sequence, and finally secondary rearrangement is completed in the 3# to n # and 1# separation columns; when the desorption of the 2# separation column is finished, starting a vacuum pipeline connected with the 2# separation column to pump out residual hydrogen isotopes in the 2# separation column;
5) repeating the step 4, and respectively carrying out separation operations of the 3# to n-1# separation columns to enable the hydrogen isotopes to sequentially move in the annular loop formed by the 1# to n # separation columns, so as to continuously promote the separation and rearrangement of the hydrogen isotopes; after the n # separation column finishes desorption, the hydrogen isotopes are rearranged for the n number, and are distributed in the 1# - (n-1) # separation columns again, which indicates that the system finishes one-time circular separation; the hydrogen isotopes form a significant hydrogen isotope concentration gradient, the heavy isotope concentration at the top of the 1# separation column at the proximal end of the loop is the highest, and the heavy isotope concentration at the bottom of the (n-1) # separation column at the distal end of the loop is the lowest;
6) opening a pipeline connecting the light isotope storage tank and the (n-1) # separation column, simultaneously starting a variable-frequency speed regulating motor to enable the rotary frame to rotate clockwise, enabling the (n-1) # separation column to rise and separate from the liquid nitrogen liquid level, discharging the light isotope from the bottom of the (n-1) # separation column and collecting the light isotope into the light isotope storage tank, and closing the pipeline connecting the light isotope storage tank and the (n-1) # separation column after the light isotope storage tank is collected; then, a pipeline connecting the heavy isotope storage tank and the 1# separation column is opened, and simultaneously, a variable-frequency speed regulating motor is started to enable the rotary frame to rotate anticlockwise, so that the 1# separation column rises to be separated from the liquid level, and the heavy isotopes are discharged from the top of the 1# separation column and collected into the heavy isotope storage tank;
7) sampling and analyzing the isotope abundance in the 2# to n-2# separation column, selecting the separation column with the abundance close to that of the raw material hydrogen, and injecting the raw material hydrogen from the top of the separation column, wherein the injection amount of the raw material hydrogen is equal to the total collection amount of the light isotopes collected in the light isotope storage tank and the heavy isotopes collected in the heavy isotope storage tank; then carrying out the next cycle of separation operation; if the abundance and extraction amount of the light isotope and the heavy isotope in one circulation separation do not reach the expected values, a larger hydrogen isotope concentration gradient can be obtained by increasing the number of the separation columns or the circulation times, so as to achieve the expected separation effect.
In order to make those skilled in the art better understand the technical solution of the present invention, the following examples are provided to further illustrate the technical solution of the present invention.
Example 1: single cycle mode hydrogen isotope separation
In the embodiment, 8 separating columns are selected, namely 1#, 2#, 3#, 4#, 5#, 6#, 7# and 8# separating columns, and the separating columns are sequentially connected end to end in the clockwise direction according to the number (1# → 2# → … → 8# → 1#) to form a closed loop; the rotary frame for placing the separation columns is placed in a low-temperature tank, the low-temperature tank is cooled by liquid nitrogen, the separation columns on the top of the rotary frame are positioned above the liquid level, and the rest separation columns are immersed below the liquid level. The system also comprises a raw material hydrogen storage tank, a light isotope storage tank, a heavy isotope storage tank, a tail gas storage tank, a flowmeter, a vacuum pump, and pipelines and valves for connecting the devices.
The separation column is a stainless steel corrugated pipe with the outer diameter of DN50, the wall thickness of 0.2mm and the length of 1000, the pressure resistance can reach 1MPa, two ends of the corrugated pipe are plane welding sealing structures, and the end surfaces are connected with a 1/4-inch stainless steel pipe through clamping sleeves. The packing of the separation column is a 5A molecular sieve with phi 1-phi 2, and the single column packing amount is 1.3 kg; the filler is heated to 350 ℃ before filling, the temperature is kept for more than 4h, and high-temperature activation dehydration treatment is carried out. One-way valves (numbered from V1 to V8) are arranged between the separation columns, the opening differential pressure of the one-way valves is adjustable between 0.1MPa and 0.5MPa, and when the pressure in the separation columns exceeds a set value, the one-way valves can flow to the rear separation columns in a one-way mode.
The revolving frame is a cylindrical aluminum frame consisting of a central rotating shaft and 1515 aluminum profiles which are arranged along the radial direction and the circumferential direction, the diameter of the circumference is 800, holes with the diameter of phi 8 are drilled on the aluminum profile spokes along the circumference at an angle of 45 degrees, 1/4-inch steel pipes welded on two end surfaces of the separation column penetrate through the holes, and the separation column can be fixed on the revolving frame. The external connection of the revolving frame is shown in figure 1, a rotating shaft in the center of the revolving frame is an aluminum pipe with the outer diameter phi of 40 and the wall thickness of 2mm, two ends of the rotating shaft extend out of the low-temperature tank, the left end of the rotating shaft is connected with a variable-frequency speed-regulating motor through a coupler and used for driving the revolving frame to rotate, and the rotating speed of the motor is 0.1-10 r/min. The right end of the rotating shaft is connected with the multi-channel rotating joint, the inlet and outlet pipelines of the separation column are all connected with the rotor end of the multi-channel rotating joint through the inner hole of the rotating shaft, and the fixed end of the rotating joint is connected with the matched valve control assembly through a pipeline. The two ends of the rotating shaft are sleeved with low-temperature bearings, and the low-temperature bearings are fixed on the inner wall of the low-temperature groove. The position of the rotating shaft penetrating through the side wall of the low-temperature groove is sealed by low-temperature glue so as to prevent liquid nitrogen from flowing out.
According to the system composition, the separation method of the rotary low-temperature hydrogen isotope separation system utilizes the principle of a simulated moving bed, and the specific realization method is as follows:
(1) connecting each separation column with a vacuum pump, pumping out residual gas in each column, and then injecting liquid nitrogen into the low-temperature tank to ensure that the 1# to 7# separation columns are all immersed in the liquid nitrogen, and the 8# separation column at the topmost end is higher than the liquid level.
(2) Opening an inlet valve of the 1# separation column, injecting natural hydrogen (with deuterium content of about 150ppm) into the system, and allowing the natural hydrogen to enter the 1# to 7# separation column; when the pressure in the 7# column reached 0.02MPa (gauge pressure), it indicated that the raw material hydrogen adsorption was saturated, and the total amount of hydrogen adsorption was about 1000L.
(3) And rotating the rotating device anticlockwise to enable the 8# separation column to move downwards to be immersed into liquid nitrogen and the 1# separation column to move upwards to be separated from the liquid level. Desorbing hydrogen isotopes in the 1# column, increasing the pressure in the column, moving the hydrogen isotopes backwards to enter the 2# column when the pressure exceeds the opening pressure of the one-way valve by 0.1MPa, so that the hydrogen isotopes in the 2# column enter the 3# column through the one-way valve, performing a similar process on a subsequent separation column, and finally enabling all the hydrogen isotopes in the 1# to 7# separation column to enter the 2# to 8# separation column to complete the first rearrangement; the heavy isotope concentration gradually decreases along 2# → 8 #. When the pressure in the 1# separation column does not change significantly, the desorption is finished, and then the 1# column is vacuumized to remove residual hydrogen isotopes so as to regenerate the 1# column.
(4) Rotating the rotating device anticlockwise again to enable the 2# separation column to move upwards to be separated from the liquid level, and enabling the 1# separation column to move downwards to be immersed into liquid nitrogen; the 2# column absorbs the heat of the air to release hydrogen isotopes, and the hydrogen isotopes in each column move backwards in sequence, and finally the second rearrangement is completed in the 3# to 8# and 1# columns. And when the 2# column finishes desorption, opening a vacuum pipeline connected with the 2# column to pump out residual hydrogen isotopes.
(5) According to the same mode, the subsequent separation operations of the columns are carried out, so that the hydrogen isotopes move in the annular loop formed by the 1# to 8# separation columns in sequence, and the separation effect of the hydrogen isotopes is improved continuously.
(6) After the 8# separation column is desorbed, the hydrogen isotopes are rearranged for the 8 th time, and are distributed on the 1# to 7# separation columns again, which shows that the system completes one cycle separation; the hydrogen isotopes form a significant hydrogen isotope concentration gradient, with deuterium at the top of the 1# column at the proximal end of the loop) being the highest concentration and deuterium at the bottom of the 7# column at the distal end being the lowest concentration.
(7) Extracting products and filling raw materials according to basic experimental data and a material conservation principle: connecting a light isotope storage tank pipeline, moving the rotating frame clockwise to enable the 7# separation column to rise to be separated from the liquid level, desorbing the isotope in the column, and discharging the light isotope from the bottom of the column, wherein the deuterium-depleted hydrogen collection amount is about 110L, and the deuterium concentration is about 10 ppm; connecting a heavy isotope storage tank pipeline, moving the rotating frame anticlockwise to enable the 1# separation column to rise to be separated from the liquid level, and discharging heavy isotopes from the top of the column, wherein the deuterium-enriched hydrogen collection amount is about 30L, and the deuterium concentration is about 650 ppm; the isotope abundance in the 2# to 6# separation column is sampled and analyzed to show that the 3# separation column is close to the abundance of the raw material gas, the raw material hydrogen is injected from the top of the 3# separation column, and the injection amount is 140L; the deuterium concentration gradient of the hydrogen isotope distribution zone is not obviously influenced based on the mode.
(8) Repeating steps (1) - (7) allows separation of natural hydrogen in a semi-continuous mode to obtain deuterium depleted hydrogen with deuterium concentration of about 10ppm and deuterium enriched hydrogen with deuterium concentration of 650 ppm.
Example 2: dual cycle mode natural hydrogen separation
Example 2 the rotary cryogenic hydrogen isotope separation system used was the same as in example 1, and the specific separation method was as follows:
i, carrying out the operations of the steps (1) to (6) in the example 1 to complete one-time circulation separation;
II, repeating the operations of the steps (1) to (6) in the example 1 to complete the second circulation separation;
III, connecting a pipeline of a light isotope storage tank, moving the rotating frame clockwise to enable the 7# separation column to rise to be separated from the liquid level, desorbing the isotope in the column, and discharging the light isotope from the bottom of the column, wherein the deuterium-depleted hydrogen collection amount is about 125L, and the deuterium concentration is about 1 ppm; connecting a heavy isotope storage tank pipeline, moving the rotating frame anticlockwise to enable the 1# separation column to rise to be separated from the liquid level, and discharging heavy isotopes from the top of the column, wherein the deuterium-enriched hydrogen collection amount is about 15L, and the deuterium concentration is about 1400 ppm; the isotopic abundance in the 2# to 6# separation columns is sampled and analyzed, the 2# separation column is close to the abundance of the raw material gas, the raw material hydrogen is injected from the top of the 2# separation column, and the injection amount is 140L.
IV, repeating the steps I-III, and separating the natural hydrogen in a semi-continuous mode to obtain deuterium-depleted hydrogen with deuterium concentration of about 1ppm and deuterium-enriched hydrogen with deuterium concentration of 1400 ppm.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (10)
1. A rotary low-temperature hydrogen isotope separation system is characterized by comprising a low-temperature tank (1) for internally storing liquid nitrogen, a circular ring-shaped rotary frame (2) which is arranged in the low-temperature tank (1) and rotates along the radial direction of the low-temperature tank (1), n separation columns (3) which are horizontally arranged on the circumference of the outer ring of the rotary frame (2) at equal intervals and can synchronously rotate along with the rotary frame (2), a raw material hydrogen storage tank (4) which stores raw material hydrogen and is respectively connected with the 1# - (n-2) # separation columns (3) through pipelines, a light isotope storage tank (5) which is used for storing light isotopes and is connected with the (n-1) # separation columns (3) through pipelines, a heavy isotope storage tank (6) which is used for storing heavy isotopes and is connected with the 1# separation columns (3) through pipelines, and a vacuum pump (7) which is respectively connected with all the separation columns (3) through pipelines, and a tail gas storage tank (8) connected with the vacuum pump (7) through a pipeline; the device comprises n separation columns (3), wherein the separation columns (3) are connected end to end through pipelines in sequence in the clockwise direction on a rotary frame (2) to form a closed loop, only one separation column (3) in the n separation columns (3) is located above the liquid level of liquid nitrogen in a low-temperature tank (1), the rest n-1 separation columns (3) are all located below the liquid level of the liquid nitrogen in the low-temperature tank (1), a tail gas storage tank (8) is connected with a raw material hydrogen storage tank (4) through pipelines, and the n separation columns are sequentially numbered from 1#, 2#, 3# … … (n-1) #andn #.
2. The rotary cryogenic hydrogen isotope separation system of claim 1, wherein the rotary frame (2) comprises a rotary shaft (21) horizontally installed in the cryogenic tank (1) and freely rotating relative to the cryogenic tank (1), and a circular aluminum frame (22) located in the cryogenic tank (1) and longitudinally installed on the rotary shaft (21) and synchronously rotating with the rotary shaft (21), wherein n circular clamping holes respectively matched with the separation columns (3) are longitudinally and equidistantly formed in the circumference of the aluminum frame (22), and the n separation columns (3) are respectively installed in the n circular clamping holes.
3. The rotary type cryogenic hydrogen isotope separation system of claim 2, wherein two ends of the rotating shaft (21) extend to two corresponding side walls of the cryogenic tank (1) respectively, one end of the rotating shaft (21) is connected with a variable frequency speed regulation motor (23) which is located outside the cryogenic tank (1) and used for driving the rotating shaft (21) to rotate through a coupling, the other end of the rotating shaft (21) is connected with a multichannel rotary joint (24) which is located outside the cryogenic tank (1) and used for connecting a gas pipeline, the rotating shaft (21) is a hollow aluminum pipe, and pipelines connected to the n separation columns (3) are all wired through an inner cavity of the rotating shaft (21) and the multichannel rotary joint (24).
4. The rotary cryogenic hydrogen isotope separation system according to claim 3, wherein two ends of the rotating shaft (21) are respectively sleeved with a cryogenic bearing (25), and the two cryogenic bearings (25) are respectively embedded in two corresponding side walls of the cryogenic tank (1).
5. The rotary type cryogenic hydrogen isotope separation system according to claim 4, wherein the two ends of the separation column (3) are welded in a plane sealing manner, the two end surfaces of the separation column are respectively connected with a stainless steel corrugated pipe through a clamping sleeve, and the pressure resistance of the separation column (3) is up to 1 MPa.
6. The rotary type cryogenic hydrogen isotope separation system according to claim 5, wherein the separation column (3) is filled with an inorganic filler having a cryogenic hydrogen isotope effect, the inorganic filler is any one of a molecular sieve, alumina or silica gel, and the inorganic filler is subjected to a high temperature activation water removal treatment at 300 ℃ or above before being filled into the separation column (3).
7. The rotary type cryogenic hydrogen isotope separation system according to claim 6, wherein a first flowmeter (9) is arranged on a raw material hydrogen pipeline connected with the raw material hydrogen storage tank (4), a third flowmeter (11) is arranged on a light isotope gas pipeline connected with the light isotope storage tank (5), and a second flowmeter (10) is arranged on a heavy isotope gas pipeline connected with the heavy isotope storage tank (6).
8. The rotary low-temperature hydrogen isotope separation system of claim 7, wherein the pipelines of the raw material hydrogen pipeline respectively connected with the 1# - (n-2) # separation columns (3) are respectively provided with a switch valve, the pipeline of the light isotope gas pipeline connected with the (n-1) # separation column (3) is provided with a switch valve, the pipeline of the heavy isotope gas pipeline connected with the 1# separation column (3) is provided with a switch valve, the pipelines of the vacuum pump (7) respectively connected with the n separation columns (3) are respectively provided with a switch valve, and all the pipelines connected between the adjacent separation columns (3) are respectively provided with a one-way valve with adjustable opening pressure difference of 0.1 MPa-0.5 MPa.
9. Rotary cryogenic hydrogen isotope separation system according to claim 8, characterized in that the aluminium frame (22) is made of 1515 aluminium profiles.
10. A separation method of a rotary low-temperature hydrogen isotope separation system is characterized by comprising the following steps:
1) firstly, sequentially numbering n separation columns, wherein the numbering is 1#, 2#, 3# … … (n-1) #andn #, then communicating each separation column with a vacuum pump, starting the vacuum pump to pump out residual gas in each separation column, and then injecting liquid nitrogen into a low-temperature tank to ensure that 1# - (n-1) # is immersed in the liquid nitrogen, and the n # separation column positioned at the top end of a rotary frame is higher than the liquid level of the liquid nitrogen;
2) starting a valve for communicating the 1# separation column with the raw material hydrogen storage tank, and injecting the raw material hydrogen into the system to ensure that the 1# to (n-1) # separation columns reach the saturated adsorption capacity;
3) starting a variable-frequency speed regulating motor to enable the rotary frame to rotate anticlockwise, so that the 1# separation column moves upwards to be separated from the liquid level of liquid nitrogen, and the n # separation column moves downwards to be immersed in the liquid nitrogen; the 1# separation column absorbs air heat, hydrogen isotopes in the 1# to (n-1) # separation columns are sequentially moved backwards through hydrogen isotope desorption, and finally first rearrangement is completed in the 2# to n # separation columns; when the release of the hydrogen isotopes in the 1# separation column is finished, starting a vacuum pipeline to pump out the residual hydrogen isotopes in the 1# separation column;
4) rotating the revolving frame anticlockwise again to enable the 2# separation column to move upwards to be separated from the liquid level of the liquid nitrogen, and enable the 1# separation column to move downwards to be immersed in the liquid nitrogen; the 2# separation column absorbs the heat of the air to desorb hydrogen isotope gas, the hydrogen isotopes in each separation column move backwards in sequence, and finally secondary rearrangement is completed in the 3# to n # and 1# separation columns; when the desorption of the 2# separation column is finished, starting a vacuum pipeline connected with the 2# separation column to pump out residual hydrogen isotopes in the 2# separation column;
5) repeating the step 4, and respectively carrying out separation operations of the 3# - (n-1) # separation columns to enable the hydrogen isotopes to sequentially move in the annular loop formed by the 1# -n # separation columns, thereby continuously promoting the separation and rearrangement of the hydrogen isotopes; after the n # separation column finishes desorption, the hydrogen isotopes are rearranged for the n number, and are distributed in the 1# - (n-1) # separation columns again, which indicates that the system finishes one-time circular separation; the hydrogen isotopes form a significant hydrogen isotope concentration gradient, the heavy isotope concentration at the top of the 1# separation column at the proximal end of the loop is the highest, and the heavy isotope concentration at the bottom of the (n-1) # separation column at the distal end of the loop is the lowest;
6) opening a pipeline connecting the light isotope storage tank and the (n-1) # separation column, simultaneously starting a variable-frequency speed regulating motor to enable the rotary frame to rotate clockwise, enabling the (n-1) # separation column to rise and separate from the liquid nitrogen liquid level, discharging the light isotope from the bottom of the (n-1) # separation column and collecting the light isotope into the light isotope storage tank, and closing the pipeline connecting the light isotope storage tank and the (n-1) # separation column after the light isotope storage tank is collected; then, a pipeline connecting the heavy isotope storage tank and the 1# separation column is opened, and simultaneously, a variable-frequency speed regulating motor is started to enable the rotary frame to rotate anticlockwise, so that the 1# separation column rises to be separated from the liquid level, and the heavy isotopes are discharged from the top of the 1# separation column and collected into the heavy isotope storage tank;
7) sampling and analyzing the isotope abundance in the No. 2 to (n-2) # separation column, selecting the separation column with the abundance approximate to that of the raw material hydrogen, and injecting the raw material hydrogen from the top of the separation column, wherein the injection amount of the raw material hydrogen is equal to the total collection amount of the light isotopes collected in the light isotope storage tank and the heavy isotopes collected in the heavy isotope storage tank; then carrying out the next cycle of separation operation; if the abundance and extraction quantity of the light isotope and the heavy isotope of one-time circulation separation do not reach the expected value, a larger hydrogen isotope concentration gradient is obtained by increasing the number of the separation columns or the circulation times, so as to achieve the expected separation effect.
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| CN114768531B (en) * | 2022-05-31 | 2023-04-07 | 中国工程物理研究院材料研究所 | Hydrogen isotope water separation system and method |
| GB2610262B (en) * | 2022-06-14 | 2023-12-27 | Atomic Energy Authority Uk | Improvements in and relating to isotope separation in a fusion power system |
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