The specific embodiment
Design of the present utility model is as follows:
The technical solution adopted in the utility model is: utilize stable isotope crystal cut in process, the separated simultaneously and hydrogen isotope of hydrogen isotope in the water and oxygen isotope is than the segregative characteristic of oxygen isotope, by changing the operating condition of heavy oxygen water separation device, change the emission at first order rectifying column top in the aquatic product process of heavy oxygen into depleted water, output depleted water intermittently when continuously producing heavy oxygen water.Heavy oxygen water separation device 1 of the present utility model is generally by multistage (T
1~T
n, be generally 3~10 grades) and cascade rectifying column composition, the specific operation condition of employing heavy oxygen water separation device first order tower can the Batch Process D abundance be the depleted water of 0.2ppm~125ppm, the heavy oxygen of extraction simultaneously water.In this production process, the oxygen isotope in the water is constantly separated in cascade unit, and hydrogen isotope is also simultaneously separated, can obtain to be shelled light the water of heavy hydrogen at the top of first order tower, the bottom of afterbody tower has then the obtained enrichment water of heavy oxygen.Change heavy oxygen water separation device operating condition, can be when producing heavy oxygen water continuously, Batch Process depleted water product.
Below various piece of the present utility model is described in detail:
Cascade rectification device
Cascade rectification device of the present utility model is by multistage rectification tower (T
1)~(T
n) be formed by connecting, and n is the integer between 3~10.The series connection of rectifying column inter-stage, each grade rectifying column can be a tower, also can be composed in parallel by a plurality of towers, rectifying progression can be more than 10 grades.
Reflux operation
Described natural water raw material (S
0) in above-mentioned cascade rectification device (1), carry out following steps respectively:
(i) at multistage rectification tower (T
1)~(T
n) in carry out cascade rectifying, at described first order rectifying column (T
1) in carry out, partial reflux or zero reflux operation, thus at final stage rectifying column (T
n) the bottom obtain heavy oxygen aquatic products (S
4);
(ii) in described first order rectifying column (T1), carry out total reflux operation, thereby at first order rectifying column (T
1) the top obtain the depleted water (S of D abundance between 0.2ppm~125ppm
1), at final stage rectifying column (T
n) the bottom obtain heavy oxygen aquatic products (S
4).
Wherein, step (i) is the partial reflux step, and step (ii) is the infinite reflux step.
The tower pressure of described step (i), temperature, cascade flow, add heat, condensation number is not specifically limited, only otherwise goal of the invention of the present utility model is produced restriction to get final product.Its scope of selecting for use can be selected according to workshop manual or manufacturer's standard.
(ii) tower pressure, temperature, cascade flow of described step, add heat, condensation number is not specifically limited, only otherwise goal of the invention of the present utility model is produced restriction to get final product.Its scope of selecting for use can be selected according to workshop manual or manufacturer's standard.
Step (i) can be identical with step technological parameter (ii), also can be different.
The utility model has utilized the characteristic of cascade erratic process, obtains the required heavy oxygen water and the depleted water of specific concentrations by partial reflux step and the infinite reflux step that hockets.Particularly, be to derive by extensive experimental with to material balance and mass transport process, set up the related of heavy oxygen water cascade unit production operation parameter and depleted water product D abundance, and according to this association and according to required product adjusting technological parameter.Described related empirical equation is as follows:
In the formula:
X: the abundance of deuterium in the depleted water product, ppm;
X
0: raw material (S
0) in the abundance of deuterium, ppm;
H: output is the liquid measure in the phegma storage tank (2), kg;
H
0: the liquid holdup in the cascade unit, kg;
A: coefficient, relevant with the cascade unit separating power, when the theoretical cam curve of cascade unit reaches 2500~4000, A=180;
α: separation;
L: capacity of returns, kg/hr;
T: the time of Batch Process (being the total reflux operation time), hr.
By correlation (1) as can be known, the variation of D abundance is relevant with liquid holdup, theoretical cam curve, production operation industrial and mineral, output (being the liquid measure in the phegma storage tank), the production time (being infinite reflux running time) of cascade separator.Change the operating condition of heavy oxygen water separation device, first order rectifying column with the heavy oxygen water separation device, change total reflux operation into by original partial reflux, this moment, system did not have charging, cat head not to have emission, reflux stream is returned in the tower through the phegma storage tank, and in tower, hydrogen isotope in the water and oxygen isotope are simultaneously separated, the top area of first order tower obtain stripping light the depleted water of deuterium, the bottom section of afterbody tower obtains the heavy oxygen water of enriched in oxygen-18.For existing heavy oxygen water separation device, after the production operation industrial and mineral is determined,, can obtain the depleted water product of the different D abundances of 0.2ppm~125ppm scope by changing Batch Process time and output.
Light component (protium in the hydrogen isotope and the oxygen in the oxygen isotope-16) is constantly toward the cat head enrichment, heavy component (deuterium in the hydrogen isotope and the oxygen in the oxygen isotope-18) is constantly toward the enrichment of tower still, the water of can obtain enrichment at the top of first order rectifying column protium and oxygen-16 (
1H
2 16O), the water of the bottom of afterbody tower heavy hydrogen that then obtained enrichment and heavy oxygen (
2H
2 18O).Material in the phegma storage tank, increase along with the infinite reflux time, the abundance of deuterium constantly reduces, the speed that D abundance descends and the separative efficiency of separator, the production operation industrial and mineral, the time of staying of phegma in storage tank is relevant, for existing heavy oxygen water separation device, after the production operation industrial and mineral is determined, the time of staying of phegma in storage tank short more (being that liquid holdup is few more in the phegma storage tank), D abundance descends fast more in the phegma, by changing the infinite reflux running time and the time of staying of phegma in storage tank, can in the phegma storage tank, obtain the depleted water of the different D abundances of 0.2ppm~125ppm scope, according to the depleted water in demand extraction at the intermittence phegma storage tank of different D abundances.
The utility model adopts total reflux operation to prepare depleted water, irrelevant with the feed entrance point of heavy oxygen water separation device, and the theoretical cam curve that preparation heavy oxygen water needs is more than depleted water, and therefore every employing crystal heats up in a steamer the various separators that legal system is equipped with heavy oxygen water and all can adopt the utility model technology intermission to prepare depleted water.
Below in conjunction with specific embodiment, further illustrate the utility model.Should be understood that these embodiment only to be used to the utility model is described and be not used in the restriction scope of the present utility model.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Ratio and percentage are based on weight, unless stated otherwise.
Unless otherwise defined or explanation, the meaning that all specialties used herein are familiar with scientific words and those skilled in the art is identical.Any in addition method similar or impartial to described content and material all can be applicable in the utility model method.
Embodiment 1
As shown in Figure 1, a kind of isotopic separation device of Batch Process depleted water, this device is formed by connecting (n is the integer between the 3-10) by n level rectifying column, wherein, first order rectifying column T
1Cat head by condenser E
1Connect backflow fluid reservoir 2, this backflow fluid reservoir 2 connects first order rectifying column T by liquid delivery pump 3
1, second level rectifying column T
2Cat head by condenser E
3Connect first order rectifying column T
1The bottom, first order rectifying column T
1The tower still is provided with reboiler E
2, first order rectifying column T
1The tower still connects second level rectifying column T
2Cat head, the rectifying column T of subordinate
nCat head by condenser E
2n-1Connect higher level's rectifying column T
N-1The bottom, higher level's rectifying column T
N-1The tower still connect the rectifying column T of subordinate
nCat head, the tower still of rectifying columns at different levels is equipped with reboiler, as second level rectifying column T
2The tower still be provided with reboiler E
4, n-1 level rectifying column T
N-1The tower still be provided with reboiler E
2n-2, n level rectifying column T
nThe tower still be provided with reboiler E
2nFirst order rectifying column T
1Connection natural water storage tank, natural water S
0Input first order rectifying column T from the natural water storage tank
1, backflow fluid reservoir 2 connects depleted water gatherer, depleted water S
3From 2 outputs of backflow fluid reservoir, afterbody rectifying Tata still connects heavy oxygen aquatic products S
4Gatherer.
The mode of production of heavy oxygen water is with natural water S
0Be raw material, enter heavy oxygen water separation device 1 first order rectifying column T
1, at first order rectifying column T
1The surplus liquid depleted water of top discharge heavy oxygen water S
3, at final stage rectifying column T
nThe bottom obtain heavy oxygen aquatic products S
4, producing in the process of heavy oxygen water first order rectifying column T continuously
1Finite reflux operation is (for S
0From the production technology that cat head enters first order rectifying column, first order rectifying column T
1Can not reflux), change first order rectifying column T
1Operating condition, keep the operating parameter (tower pressure, temperature, cascade flow, add heat, condensation number etc.) of rectifying columns at different levels constant, at first in phegma storage tank 2, add the natural water of certain design flow, stop first order rectifying column T then simultaneously
1Charging (S
0=0) and cat head extraction (S
3=0), with first order rectifying column T
1Change total reflux operation into by partial reflux, first order rectifying column T
1The condensate liquid S of cat head
1The phegma storage tank 2 of flowing through, with liquid delivery pump 3 with phegma S
2In the input tower, phegma S
2Flow and condensate liquid S
1Flow equate (S
1=S
2), in tower, hydrogen isotope in the water and oxygen isotope are simultaneously separated, light component (protium in the hydrogen isotope and the oxygen in the oxygen isotope-16) is constantly toward the cat head enrichment, heavy component (deuterium in the hydrogen isotope and the oxygen in the oxygen isotope-18) is constantly toward the enrichment of tower still, the water vapour of can obtain enrichment at the top of first order rectifying column protium and oxygen-16 is through condenser E
1Flow into phegma storage tank 2 (being depleted water) after the condensation, the water (being heavy oxygen water) of the bottom of afterbody tower has then obtained enrichment heavy hydrogen and heavy oxygen, material in the phegma storage tank 2, increase along with the infinite reflux time, the abundance of deuterium constantly reduces, the speed that D abundance descends is relevant with separative efficiency, production operation industrial and mineral, the time of staying of phegma in storage tank 2 of separator, regulates the abundance of deuterium according to following formula (1):
In the formula:
X: the abundance of deuterium in the depleted water product, ppm;
X
0: natural water raw material (S
0) in the abundance of deuterium, ppm;
H: output is the liquid measure in the phegma storage tank (2), kg;
H
0: the liquid holdup in the cascade rectification device, kg;
A: cascade rectification device separating power coefficient;
α: separation;
L: capacity of returns, kg/hr;
T: infinite reflux time, hr.
In another specific embodiment, above-mentioned change first order rectifying column (T
1) the operating condition process in, also can not be used in the phegma storage tank 2 and to inject a certain amount of natural water, but at first stop T
1Cat head extraction (the S of tower
3=0), the material in this moment phegma storage tank 2 constantly increases, and when reaching certain design flow, stops T again
1Charging (the S of tower
0=0), with T
1Tower changes total reflux operation into by partial reflux.
In another specific embodiment, heavy oxygen water separation device for prior art is transformed, after the production operation operating mode is determined, the time of staying of phegma in storage tank 2 is short more, D abundance descends fast more in the phegma, by changing infinite reflux running time (the infinite reflux time is preferred: 4 hours~400 hours) and the time of staying (time of staying preferred 0.5 hour~10 hour) of phegma in storage tank 2, can in phegma storage tank 2, obtain the depleted water of the different D abundances of 0.2ppm~125ppm scope, according to the depleted water in demand extraction at the intermittence phegma storage tank 2 of different D abundances.Repeat above-mentioned natural water S
0The operating process that charging is later, constantly Batch Process depleted water.
Described heavy oxygen water and depleted water are such outputs simultaneously:
Because heavy oxygen moisture is big from difficulty, the separator that the water rectification method prepares heavy oxygen water need reach 2500~4000 blocks of theoretical trays, usually form by 3~10 grades of rectifying column cascades (series connection or series/parallel), from being dosed into the time of producing the general needs of product is 5~10 months, therefore the aquatic product of heavy oxygen is continuous production, and the water rectification method prepares depleted water, than heavy oxygen moisture from easily, its separator generally needs 30~300 blocks of theoretical trays, utilize the crystal to heat up in a steamer the stalling characteristic of hydrogen isotope and oxygen isotope in the process, change the operating condition of heavy oxygen water separation device, first order rectifying column with the heavy oxygen water separation device, change total reflux operation into by original partial reflux, this moment, system did not have charging, cat head does not have emission, reflux stream is returned in the tower through the phegma storage tank, in tower, hydrogen isotope in the water and oxygen isotope are simultaneously separated, light component (protium in the hydrogen isotope and the oxygen in the oxygen isotope-16) is constantly toward the cat head enrichment, heavy component (deuterium in the hydrogen isotope and the oxygen in the oxygen isotope-18) is constantly toward the enrichment of tower still, the water of can obtain enrichment at the top of first order rectifying column protium and oxygen-16 (
1H
2 16O), the water of the bottom of afterbody tower heavy hydrogen that then obtained enrichment and heavy oxygen (
2H
2 18O).Material in the phegma storage tank, increase along with the infinite reflux time, the abundance of deuterium constantly reduces, the speed that D abundance descends and the separative efficiency of separator, the production operation industrial and mineral, the time of staying of phegma in storage tank is relevant, for existing heavy oxygen water separation device, after the production operation industrial and mineral is determined, the time of staying of phegma in storage tank short more (being that liquid holdup is few more in the phegma storage tank), D abundance descends fast more in the phegma, by changing the infinite reflux running time and the time of staying of phegma in storage tank, can in the phegma storage tank, obtain the depleted water of the different D abundances of 0.2ppm~125ppm scope, according to the depleted water in demand extraction at the intermittence phegma storage tank of different D abundances.
Embodiment 2
A kind of isotopic separation device of Batch Process depleted water, this device is formed by connecting by 3 grades of rectifying columns, wherein, the cat head of first order rectifying column connects the backflow fluid reservoir by condenser, this backflow fluid reservoir connects first order rectifying column by liquid delivery pump, the cat head of second level rectifying column connects the bottom of first order rectifying column by condenser, the tower still of first order rectifying column connects second level rectifying column cat head, the cat head of third level rectifying column is by the bottom of condenser connection second level rectifying column, and the tower still of second level rectifying column connects third level rectifying column cat head.
With natural water is raw material, D abundance 150ppm, flow with 250kg/hr enters first order rectifying column, the operating reflux ratio of first order rectifying column is 1,2500 of the theoretical cam curves of heavy oxygen water separation device, the operating pressure of rectifying columns at different levels is 120mmHg (absolute pressure), 50 ℃~52 ℃ of tower top temperatures, final stage rectifier bottoms heavy oxygen aquatic products produced quantity is 5g/hr, the natural water that in the phegma storage tank, adds, make the material total amount in the storage tank reach 1000kg, stop the charging and the cat head extraction of first order rectifying column then simultaneously, change first order rectifying column into total reflux operation by partial reflux, the condensate stream at first order rectifying column top is imported phegma in the tower with liquid delivery pump through the phegma storage tank, the flow of phegma equates with the flow of overhead condensation liquid, the time of staying of material is 2hr in this moment phegma storage tank, and control infinite reflux running time is 200hr, and the D abundance of depleted water is 2ppm in the phegma storage tank.
The quantum of output 5 gram/hr of heavy oxygen water, oxygen-18 abundance is greater than 95%.
Embodiment 3
A kind of isotopic separation device of Batch Process depleted water, this device is formed by connecting by 10 grades of rectifying columns, wherein, the cat head of first order rectifying column connects the backflow fluid reservoir by condenser, this backflow fluid reservoir connects first order rectifying column by liquid delivery pump, the cat head of subordinate's rectifying column is by the bottom of condenser connection higher level rectifying column, and the tower still of higher level's rectifying column connects subordinate's rectifying column cat head.
With natural water is raw material, D abundance 150ppm, flow with 250kg/hr enters first order rectifying column from cat head, 2500 of the theoretical cam curves of heavy oxygen water separation device, the operating pressure of rectifying columns at different levels is 70mmHg (absolute pressure), 40 ℃~42 ℃ of tower top temperatures, final stage rectifier bottoms heavy oxygen aquatic products produced quantity is 2.8g/hr, in the phegma storage tank, add natural water, make the inventory in the storage tank reach 500kg, stop the charging and the cat head extraction of first order rectifying column then simultaneously, change first order rectifying column into total reflux operation, the condensate stream at first order rectifying column top is through the phegma storage tank, with liquid delivery pump phegma is imported in the tower, the flow of phegma equates that with the flow of overhead condensation liquid the time of staying of material is 2hr in the phegma storage tank at this moment, control infinite reflux running time is 400hr, and the D abundance of depleted water is 0.2ppm in the phegma storage tank.
The quantum of output 2.2 gram/hr of heavy oxygen water, oxygen-18 abundance is greater than 95%.
Embodiment 4
A kind of isotopic separation device of Batch Process depleted water, this device is formed by connecting by 5 grades of rectifying columns, wherein, the cat head of first order rectifying column connects the backflow fluid reservoir by condenser, this backflow fluid reservoir connects first order rectifying column by liquid delivery pump, the cat head of subordinate's rectifying column is by the bottom of condenser connection higher level rectifying column, and the tower still of higher level's rectifying column connects subordinate's rectifying column cat head.
With natural water is raw material, D abundance 150ppm, flow with 500kg/hr enters first order rectifying column from cat head, 4000 of the theoretical cam curves of heavy oxygen water separation device, the operating pressure of rectifying columns at different levels is 120mmHg (absolute pressure), 50 ℃~52 ℃ of tower top temperatures, final stage rectifier bottoms heavy oxygen aquatic products produced quantity is 7.2g/hr, in the phegma storage tank, add natural water, make the inventory in the storage tank reach 500kg, stop the charging and the cat head extraction of first order rectifying column then simultaneously, change first order rectifying column into total reflux operation, the condensate stream at first order rectifying column top is through the phegma storage tank, with liquid delivery pump phegma is imported in the tower, the flow of phegma equates that with the flow of overhead condensation liquid the time of staying of material is 1hr in the phegma storage tank at this moment, control infinite reflux running time is 24hr, and the D abundance of depleted water is 50ppm in the phegma storage tank.
The quantum of output 4.8 gram/hr of heavy oxygen water, oxygen-18 abundance is greater than 98%.
Embodiment 5
With natural water is raw material, D abundance 150ppm, flow with 100kg/hr enters first order rectifying column, the operating reflux ratio of first order rectifying column is 4,4000 of the theoretical cam curves of heavy oxygen water separation device, the operating pressure of rectifying columns at different levels is 100mmHg (absolute pressure), 46 ℃~48 ℃ of tower top temperatures, final stage rectifier bottoms heavy oxygen aquatic products produced quantity is 6g/hr, the natural water that in the phegma storage tank, adds, make the material total amount in the storage tank reach 4000kg, stop the charging and the cat head extraction of first order rectifying column then simultaneously, change first order rectifying column into total reflux operation by partial reflux, the condensate stream at first order rectifying column top is imported phegma in the tower with liquid delivery pump through the phegma storage tank, the flow of phegma equates with the flow of overhead condensation liquid, the time of staying of material is 8hr in this moment phegma storage tank, and control infinite reflux running time is 100hr, and the D abundance of depleted water is 85ppm in the phegma storage tank.
The quantum of output 4.7 gram/hr of heavy oxygen water, oxygen-18 abundance is greater than 98%.
Embodiment 6
With natural water is raw material, D abundance 150ppm, flow with 500kg/hr enters first order rectifying column from cat head, 4000 of the theoretical cam curves of heavy oxygen water separation device, the operating pressure of rectifying columns at different levels is 760mmHg (absolute pressure), 100 ℃ of tower top temperatures, final stage rectifier bottoms heavy oxygen aquatic products produced quantity is 7.2g/hr, in the phegma storage tank, add natural water, make the inventory in the storage tank reach 1000kg, stop the charging and the cat head extraction of first order rectifying column then simultaneously, change first order rectifying column into total reflux operation, the condensate stream at first order rectifying column top is through the phegma storage tank, with liquid delivery pump phegma is imported in the tower, the flow of phegma equates that with the flow of overhead condensation liquid the time of staying of material is 2hr in the phegma storage tank at this moment, control infinite reflux running time is 36hr, and the D abundance of depleted water is 105ppm in the phegma storage tank.
The quantum of output 10 gram/hr of heavy oxygen water, oxygen-18 abundance is greater than 50%.
All quote in this application as a reference at all documents that the utility model is mentioned, just quoted as a reference separately as each piece document.Should be understood that in addition after having read foregoing of the present utility model, those skilled in the art can make various changes or modifications the utility model, these equivalent form of values fall within the application's appended claims institute restricted portion equally.