CN108159883A - 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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- CN108159883A CN108159883A CN201810051728.5A CN201810051728A CN108159883A CN 108159883 A CN108159883 A CN 108159883A CN 201810051728 A CN201810051728 A CN 201810051728A CN 108159883 A CN108159883 A CN 108159883A
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- heptafluoro
- 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
It is a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, include 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, simultaneously respectively at fine fodder end, lean end using liquid nitrogen cold trap rewinding, and the air for reclaimer system is maintained to divide within 2Pa using vacuum pump；After system continuous operation to carbon isotope abundance distribution is stablized, the carbon isotope of concentration/dilution is obtained.The present invention using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, low energy consumption, separation is larger, suitable for the large-scale production of cascade form.Separating medium heptafluoro-propane is common extinguishing chemical, and the lean generated after centrifugation can still be used as extinguishing chemical normal use, 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 centrifugation carbon
The method of position element.
Background technology
As stable isotope is in the fields such as Medical Devices, bio-pharmaceuticals, quantum communications, basic research application demand amount
Increase, higher requirement is also proposed for the product abundance and preparation method of stable isotope.Wherein, high abundance13C isotopes
Field of medicaments mainly with [13C] urea form, for the detection of helicobacter pylori, contain urea in helicobacter pylori
Enzyme, when tester takes [13C] urea when, [13C] urea is broken down into stomach13CO2, then by blood circulation by lung
Discharge.Whether contained by detecting in characteristics of contaminated respiratory droplets gas13CO2, it is possible to 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
The shortcomings of method, rectification method is big there are energy consumption, and requirement of shelter is tight, and industrialized production13The chemical industry distillation technology of C isotopes always by
Overseas enterprise is monopolized, and China not yet has industrialized production high abundance13The ability of C isotopes.
Invention content
In view of the deficiencies of the prior art, the purpose of the present invention is to provide one kind carbon is centrifuged 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 centrifugation 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
Into different distributions, feed flow is adjusted, adjusts fine fodder nozzle, lean nozzle pressure, while make 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) treat that system is continuously transported
After row is stablized to carbon isotope abundance distribution, the carbon isotope of concentration/dilution is obtained.
Preferably, in step (1), the chemical purity of purified gaseous state heptafluoro-propane is more than 99.99%.
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 sampled and is simultaneously carried out using mass spectrometer more than 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 the present 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, suitable for the large-scale production of cascade form；
(2) separating medium heptafluoro-propane is common extinguishing chemical, and the lean generated after centrifugation can still be used as fire extinguishing
Agent normal use.
Description of the drawings
Fig. 1 is the separation principle using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope in one embodiment of the invention
Schematic diagram；
Fig. 2 is the mass spectrometry results figure that unit detaches heptafluoro-propane in one embodiment of the invention；
【Figure elements explanation】
1- pressurizing vessels；2- feed material bottles；
3- centrifuges；4- fine fodder samplers；
5- lean samplers；6- fine fodder material bottles；
7- lean material bottles；8- vacuum pumps；
9- liquid nitrogen cold traps；10- liquid nitrogen cold traps.
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.
Present invention offer is a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, includes the following steps：Only
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
At fine fodder end, lean end using liquid nitrogen cold trap rewinding, and using vacuum pump maintain air partial pressure for reclaimer system 2Pa with
It is interior；After system continuous operation to carbon isotope abundance distribution is stablized, the carbon isotope of concentration/dilution is obtained.The present invention with
Low energy consumption, separation is larger for the method for medium centrifugation separation of carbon isotope for heptafluoro-propane, suitable for the scale of cascade form
Metaplasia is produced.Separating medium heptafluoro-propane is common extinguishing chemical, and the lean generated after centrifugation can still be used as extinguishing chemical just
It often uses, 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 including the following steps：(1) natural heptafluoro-propane is purified, its chemical purity is made to meet the centrifugation 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
To form different distributions in, adjust feed flow, adjust fine fodder nozzle, lean nozzle pressure, at the same respectively fine fodder end,
Lean end uses liquid nitrogen cold trap rewinding, and the air for reclaimer system is maintained to divide within 2Pa using vacuum pump；(3) wait be
After continuous operation of uniting is stablized to carbon isotope abundance distribution, the carbon isotope of concentration/dilution is obtained.
In step (1), the chemical purity of purified gaseous state heptafluoro-propane is more than 99.99%.
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 samples more than after 1.5h and simultaneously carries out component point using mass spectrometer
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 centrifuged by medium of heptafluoro-propane to provided by the invention
The method of element is described in further detail.
Fig. 1 is the separation principle using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope in one embodiment of the invention
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, unit separation compared with
The characteristics of big.
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 temperatures is not less than 665Pa；(3) thermal stability is good, is not sent out below 300 DEG C
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 cooling agent, is utilized using liquid nitrogen and " liquid nitrogen-absolute ethyl 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 more than 99.99%.
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 ensure feed flow
Stability has been connected in parallel a larger pressurizing vessel of volume at feed material bottle.Adjust the valve for reclaimer system 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 treating that every fluid parameter is adjusted, make system continuous and steady operation at least 1.5h, liquid is used at essence, lean end
Nitrogen cold-trap feeding can obtain the heptafluoro-propane feeding sample of abundance stabilization 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 two kinds of H and D to stablize 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 detaches.
The isotope composition of 1 natural heptafluoro-propane of table
| 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 parameter of mass spectrometer is adjusted so that C3HF7It is struck off one
A F-Ion obtains (C3HF6)+Ion cluster, so as to measure to obtain the mole percent variation of heptafluoro-propane different molecular weight component
Situation.The mass spectrometry results of gas centrifugation unit separating experiment are as shown in Fig. 2, wherein abscissa represents the phase of heptafluoro-propane
To molecular mass.Using binary separation theorem, mass spectrometry results are carried out with certain processing, the base of heptafluoro-propane can be obtained
This head to tail separationfactor is 1.12, illustrates to carry out the feasibility of carbon isotope separation using this method.
In conclusion the present invention using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, low energy consumption, segregative line
Number is larger, suitable for the large-scale production of cascade form.Separating medium heptafluoro-propane is common extinguishing chemical, is produced after centrifugation
Raw lean can still 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 the purpose of the present invention, technical solution and advantageous effect further in detail
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 the protection of the present invention
Within the scope of.
Claims (5)
- It is 1. a kind of using heptafluoro-propane as the method for medium centrifugation separation of carbon isotope, which is characterized in that include the following steps：(1) natural heptafluoro-propane is purified, its chemical purity is made to meet the centrifugation 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, feed flow is adjusted, adjusts fine fodder nozzle, lean nozzle pressure, while exist respectively Fine fodder end, lean end maintain the air for reclaimer system to divide within 2Pa using liquid nitrogen cold trap rewinding, and using vacuum pump；(3) after system continuous operation to carbon isotope abundance distribution is stablized, the carbon isotope of concentration/dilution is obtained.
- It is 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 more than 99.99%.
- It is 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.
- It is 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.
- It is 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 samples more than after 1.5h and simultaneously carries out component analysis, knot to be analyzed using mass spectrometer Fruit collects carbon isotope after reaching requirement.
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Cited By (2)
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| CN108939921A (en) * | 2018-09-05 | 2018-12-07 | 清华大学 | Membrane separation device and method for carbon isotope separation |
| CN111036077A (en) * | 2019-12-13 | 2020-04-21 | 清华大学 | Method for preparing high-abundance carbon-13 isotope by using ethylene and carbon dioxide as media |
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