CN108159883B - Using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope - Google Patents
Using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope Download PDFInfo
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- CN108159883B CN108159883B CN201810051728.5A CN201810051728A CN108159883B CN 108159883 B CN108159883 B CN 108159883B CN 201810051728 A CN201810051728 A CN 201810051728A CN 108159883 B CN108159883 B CN 108159883B
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- propane
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/20—Separation by centrifuging
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Abstract
A method of using heptafluoro-propane as medium centrifugation separation of carbon isotope, comprising the following steps: purify natural heptafluoro-propane;By purified gaseous state heptafluoro-propane, it is passed through gas centrifuge, each relative molecular mass component in heptafluoro-propane will form different distributions in centrifugal force field, adjust feed flow, adjust essence, lean nozzle pressure, liquid nitrogen cold trap rewinding is used at fine fodder end, lean end respectively simultaneously, and maintains the air for reclaimer system to divide within 2Pa using vacuum pump;After system continuous operation to carbon isotope abundance distribution is stablized, concentration/dilution carbon isotope is obtained.Of the invention using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, low energy consumption, separation is larger, the large-scale production suitable for cascade form.Separating medium heptafluoro-propane is common extinguishing chemical, and the lean generated after centrifuge separation still can be used as extinguishing chemical normal use, and this method is used for the separation of carbon isotope, has technical feasibility.
Description
Technical field
The invention belongs to technical field of isotope separation, and in particular to a kind of same using heptafluoro-propane as medium centrifuge separation carbon
The method of position element.
Background technique
As stable isotope is in the fields such as Medical Devices, bio-pharmaceuticals, quantum communications, basic research application demand amount
Increase, for the product abundance and preparation method of stable isotope, higher requirements are also raised.Wherein, high abundance13C isotope
Field of medicaments mainly with [13C] form of urea contains urea in helicobacter pylori for the detection of helicobacter pylori
Enzyme, when tester takes [13C] urea when, [13C] urea is broken down into stomach13CO2, then by blood circulation by lung
Discharge.By whether containing in detection characteristics of contaminated respiratory droplets gas13CO2, so that it may judge whether infect helicobacter pylori.
Carbon has12C、13Two kinds of stable isotopes of C.The industrialized preparing process of carbon isotope is cryogenic rectification at present
There is the disadvantages of energy consumption is high, and requirement of shelter is tight, and industrialized production in method, rectification method13The chemical industry distillation technology of C isotope always by
Overseas enterprise is monopolized, and China not yet has industrialized production high abundance13The ability of C isotope.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide one kind is centrifugated carbon by medium of heptafluoro-propane
The method of isotope, at least one of to solve the above problems.
The present invention is achieved through the following technical solutions:
The present invention provides a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, which is characterized in that including
Following steps: (1) natural heptafluoro-propane is purified, its chemical purity is made to meet the centrifuge separation requirement of the medium;(2) after purifying
Gaseous state heptafluoro-propane, be passed through gas centrifuge, each relative molecular mass component in heptafluoro-propane is in centrifugal force field by shape
At different distributions, feed flow is adjusted, adjusts fine fodder nozzle, lean nozzle pressure, while making respectively at fine fodder end, lean end
The air for reclaimer system is maintained to divide within 2Pa with liquid nitrogen cold trap rewinding, and using vacuum pump;(3) it is continuously transported to system
After row is stablized to carbon isotope abundance distribution, concentration/dilution carbon isotope is obtained.
Preferably, in step (1), the chemical purity of purified gaseous state heptafluoro-propane is 99.99% or more.
Preferably, in step (2), the feed flow of the gas centrifuge is 22.5~34.5g/h, the gas centrifugation
The feed nozzle pressure of machine is 300~400Pa.
Preferably, in step (2), the fine fodder nozzle pressure is 1350~1500Pa, and the lean nozzle pressure is
2000~2150Pa.
Preferably, in step (3), system continuous operating time is more than sampling and the progress of using gas mass spectrograph after 1.5h
Component analysis, result to be analyzed collect carbon isotope after reaching requirement.
It can be seen from the above technical proposal that of the invention using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope
It has the advantages that
(1) low energy consumption, separation is larger, the large-scale production suitable for cascade form;
(2) separating medium heptafluoro-propane is common extinguishing chemical, and the lean generated after centrifuge separation still can be used as fire extinguishing
Agent normal use.
Detailed description of the invention
Fig. 1 is in one embodiment of the invention using heptafluoro-propane as the separation principle of the method for medium centrifugation separation of carbon isotope
Schematic diagram;
Fig. 2 is the mass spectrometry results figure that single machine separates heptafluoro-propane in one embodiment of the invention;
[figure elements explanation]
1- pressurizing vessel;2- feed material bottle;
3- centrifuge;4- fine fodder sampler;
5- lean sampler;6- fine fodder material bottle;
7- lean material bottle;8- vacuum pump;
9- liquid nitrogen cold trap;10- liquid nitrogen cold trap.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
The present invention provides a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, comprising the following steps: net
Change natural heptafluoro-propane;By purified gaseous state heptafluoro-propane, it is passed through gas centrifuge, each average molecular matter in heptafluoro-propane
Amount component will form different distributions in centrifugal force field, adjusts feed flow, adjusts essence, lean nozzle pressure, simultaneously respectively
Fine fodder end, lean end use liquid nitrogen cold trap rewinding, and using vacuum pump maintain for reclaimer system air partial pressure 2Pa with
It is interior;After system continuous operation to carbon isotope abundance distribution is stablized, concentration/dilution carbon isotope is obtained.It is of the invention with
Heptafluoro-propane be medium centrifugation separation of carbon isotope method low energy consumption, separation is larger, the scale suitable for cascade form
Metaplasia produces.Separating medium heptafluoro-propane is common extinguishing chemical, and the lean generated after centrifuge separation still can be used as extinguishing chemical just
It is often used, this method is used for the separation of carbon isotope, has technical feasibility.
Specifically, the present invention provides a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, and feature exists
In, comprising the following steps: (1) natural heptafluoro-propane is purified, its chemical purity is made to meet the centrifuge separation requirement of the medium;(2)
By purified gaseous state heptafluoro-propane, it is passed through gas centrifuge, each relative molecular mass component in heptafluoro-propane is in centrifugal force
Different distributions will be formed in, feed flow is adjusted, adjust fine fodder nozzle, lean nozzle pressure, at the same respectively fine fodder end,
Lean end uses liquid nitrogen cold trap rewinding, and maintains the air for reclaimer system to divide within 2Pa using vacuum pump;(3) wait be
After continuous operation of uniting is stablized to carbon isotope abundance distribution, concentration/dilution carbon isotope is obtained.
In step (1), the chemical purity of purified gaseous state heptafluoro-propane is 99.99% or more.
In step (2), the feed flow of the gas centrifuge is 22.5~34.5g/h, the confession of the gas centrifuge
Expects pipe mouth pressure is 300~400Pa;The fine fodder nozzle pressure is 1350~1500Pa, and the lean nozzle pressure is 2000
~2150Pa.
In step (3), system continuous operating time is more than sampling and using gas mass spectrograph progress component point after 1.5h
Analysis, result to be analyzed collect carbon isotope after reaching requirement.
Below in conjunction with specific embodiments and the drawings, the same position of carbon is centrifugated by medium of heptafluoro-propane to provided by the invention
The method of element is described in further detail.
Fig. 1 is in one embodiment of the invention using heptafluoro-propane as the separation principle of the method for medium centrifugation separation of carbon isotope
Schematic diagram.As shown in Figure 1, separator includes pressurizing vessel 1, feed material bottle 2, centrifuge 3, fine fodder sampler 4, lean sampling
Device 5, fine fodder material bottle 6, lean material bottle 7, vacuum pump 8, liquid nitrogen cold trap 9 and liquid nitrogen cold trap 10.
In the present embodiment centrifuge 3 be domestic special gas centrifugal separation equipment, have low energy consumption, single machine separation compared with
Big feature.
When carrying out isotopic separation using gas centrifuge, it is necessary to meet following condition for working media: (1) average molecular matter
Amount is not less than 70;(2) saturated vapour pressure at normal temperature is not less than 665Pa;(3) thermal stability is good, does not send out at 300 DEG C or less
Solution estranged.
The molecular formula of heptafluoro-propane is C3HF7, molecular weight 170.03 is at normal temperatures and pressures colorless and odorless gas, chemistry
Property is stablized, nontoxic non-corrosive.The density of gas is 1.403g/cm3, the saturated vapour pressure at 25 DEG C is about 450kPa.
Heptafluoro-propane is common fire-suppressant gas, is easy to obtain on a large scale and at low cost, has obvious warp compared to other fluorides
Ji advantage.For natural heptafluoro-propane, heptafluoro-propane as coolant, is utilized using liquid nitrogen and " liquid nitrogen-dehydrated alcohol " mixture
With the difference of light impurity saturated vapour pressure, repeatedly fractionation purification is carried out to natural heptafluoro-propane, its chemical purity can be promoted
To 99.99% or more.
The pipeline adjusted for reclaimer system connects, so that the connection of system is under normal operating conditions.It adjusts and supplies
Expect orifice plate, purified heptafluoro-propane is fed into gas centrifuge with the feed flow of 22.66g/h, to guarantee feed flow
Stability has been connected in parallel the biggish pressurizing vessel of volume at feed material bottle.The valve for reclaimer system is adjusted, so that
Nozzle pressure is fed in 300Pa or so, fine fodder nozzle pressure is in 1450Pa or so, and lean nozzle pressure is in 2000Pa or so, together
When rewinding is carried out using liquid nitrogen cold trap at essence, lean end respectively, and will be maintained for the vacuum degree of reclaimer system using vacuum pump
Within 2Pa.After adjusting to every fluid parameter, make system continuous and steady operation at least 1.5h, uses liquid at essence, lean end
Nitrogen cold-trap feeding can get the stable heptafluoro-propane feeding sample of abundance at this time.
Before feeding analysis, the isotopics of natural heptafluoro-propane are analyzed first.Natural carbon has12C
With13Two kinds of stable isotopes of C, natural abundance is respectively 98.9% and 1.1%.Natural protium has a H and two kinds of D are stablized same position
Element, natural abundance are respectively 99.985% and 0.015%, approximate protium can be considered as single isotopic element.Natural fluorine
Element only has a kind of stable isotope19F.The isotopics of heptafluoro-propane molecule and its natural abundance are shown in Table 1.Separating medium
C3HF7Isotope composition have 4 kinds, but since the constituent content that mass number is 172 and 173 is extremely low, can be approximately by heptafluoro-propane
Binary separation.
The isotope composition of the natural heptafluoro-propane of table 1
Molecular composition | Molecular weight | In natural C3HF7Middle content (%) |
12C12C12CHF7 | 170 | 96.71 |
13C12C12CHF7 | 171 | 3.25 |
13C13C12CHF7 | 172 | 0.04 |
13C13C13CHF7 | 173 | - |
When being analyzed using mass spectrometer feeding, the mass spectrometric parameter of regulating gas, so that C3HF7It is struck off one
A F-Ion obtains (C3HF6)+Ion cluster, so that measurement obtains the mole percent variation of heptafluoro-propane different molecular weight component
Situation.The mass spectrometry results of gas centrifugation single machine separating experiment are as shown in Fig. 2, wherein abscissa indicates the phase of heptafluoro-propane
To molecular mass.Using binary separation theorem, mass spectrometry results are carried out with certain processing, the base of available heptafluoro-propane
This head to tail separationfactor is 1.12, illustrates the feasibility that carbon isotope separation is carried out using this method.
In conclusion of the invention, using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, low energy consumption, segregative line
Larger, the large-scale production suitable for cascade form of number.Separating medium heptafluoro-propane is common extinguishing chemical, is produced after centrifuge separation
Raw lean still can be used as extinguishing chemical normal use, and this method is used for the separation of carbon isotope, has technical feasibility.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (5)
1. a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, which comprises the following steps:
(1) natural heptafluoro-propane is purified, its chemical purity is made to meet the centrifuge separation requirement of the medium;
(2) by purified gaseous state heptafluoro-propane, it is passed through gas centrifuge, each relative molecular mass component in heptafluoro-propane exists
Different distributions will be formed in centrifugal force field, is adjusted feed flow, is adjusted fine fodder nozzle, lean nozzle pressure, while existing respectively
Fine fodder end, lean end use liquid nitrogen cold trap rewinding, and maintain the air for reclaimer system to divide within 2Pa using vacuum pump;
(3) after system continuous operation to carbon isotope abundance distribution is stablized, concentration/dilution carbon isotope is obtained.
2. according to claim 1 using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, it is characterised in that: step
Suddenly in (1), the chemical purity of purified gaseous state heptafluoro-propane is 99.99% or more.
3. according to claim 1 using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, it is characterised in that: step
Suddenly in (2), the feed flow of the gas centrifuge is 22.5~34.5g/h, the feed nozzle pressure of the gas centrifuge
For 300~400Pa.
4. according to claim 1 using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, it is characterised in that: step
Suddenly in (2), the fine fodder nozzle pressure is 1350~1500Pa, and the lean nozzle pressure is 2000~2150Pa.
5. according to claim 1 using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, it is characterised in that: step
Suddenly in (3), system continuous operating time is more than sampling and the progress component analysis of using gas mass spectrograph after 1.5h, knot to be analyzed
Fruit collects carbon isotope after reaching requirement.
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Citations (4)
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RU2144421C1 (en) * | 1998-03-10 | 2000-01-20 | Государственное предприятие Научно-исследовательский институт электрофизической аппаратуры имени Д.В.Ефремова | Method of producing highly enriched isotope 13c |
CN101244366A (en) * | 2008-03-17 | 2008-08-20 | 清华大学 | Method for centrifugation separation of carbon isotope with n-octane as medium |
CN102405089A (en) * | 2009-02-20 | 2012-04-04 | Hrd有限公司 | Apparatus and method for gas separation |
CN107441933A (en) * | 2017-08-09 | 2017-12-08 | 清华大学 | A kind of method for centrifuging titanium isotope |
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RU2144421C1 (en) * | 1998-03-10 | 2000-01-20 | Государственное предприятие Научно-исследовательский институт электрофизической аппаратуры имени Д.В.Ефремова | Method of producing highly enriched isotope 13c |
CN101244366A (en) * | 2008-03-17 | 2008-08-20 | 清华大学 | Method for centrifugation separation of carbon isotope with n-octane as medium |
CN102405089A (en) * | 2009-02-20 | 2012-04-04 | Hrd有限公司 | Apparatus and method for gas separation |
CN107441933A (en) * | 2017-08-09 | 2017-12-08 | 清华大学 | A kind of method for centrifuging titanium isotope |
Non-Patent Citations (1)
Title |
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