CN108404667B - Method for centrifugal separation of carbon isotope by using methyl iodide as medium - Google Patents
Method for centrifugal separation of carbon isotope by using methyl iodide as medium Download PDFInfo
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- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 43
- 238000000926 separation method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 58
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000012141 concentrate Substances 0.000 claims abstract description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 238000009826 distribution Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000012530 fluid Substances 0.000 claims abstract description 6
- 238000004949 mass spectrometry Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 description 6
- 238000005372 isotope separation Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- OKTJSMMVPCPJKN-OUBTZVSYSA-N Carbon-13 Chemical compound [13C] OKTJSMMVPCPJKN-OUBTZVSYSA-N 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- OKTJSMMVPCPJKN-IGMARMGPSA-N Carbon-12 Chemical compound [12C] OKTJSMMVPCPJKN-IGMARMGPSA-N 0.000 description 3
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 241000590002 Helicobacter pylori Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-OUBTZVSYSA-N Urea-13C Chemical compound N[13C](N)=O XSQUKJJJFZCRTK-OUBTZVSYSA-N 0.000 description 1
- -1 air and water vapor Chemical compound 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000003759 clinical diagnosis Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000012938 design process Methods 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000036267 drug metabolism Effects 0.000 description 1
- 229940037467 helicobacter pylori Drugs 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- ZCYVEMRRCGMTRW-IGMARMGPSA-N iodine-127 atom Chemical compound [127I] ZCYVEMRRCGMTRW-IGMARMGPSA-N 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/20—Separation by centrifuging
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method for centrifugally separating carbon isotopes by taking methyl iodide as a medium comprises the following steps: purifying light impurities in the methyl iodide raw material to ensure that the chemical purity of the light impurities meets the centrifugal separation requirement of the methyl iodide; introducing the purified gaseous methyl iodide into a gas centrifuge, adjusting the feed flow and the pressure of a concentrate pipe orifice and a lean pipe orifice of the gas centrifuge, and respectively separating concentrate and lean from the concentrate pipe orifice and the lean pipe orifice; and maintaining stable fluid parameters of the methyl iodide feeding material, the concentrate and the lean material, and respectively collecting the concentrate and the lean material with stable carbon isotope abundance distribution through a liquid nitrogen cold trap after the gas centrifugal machine continuously runs until the carbon isotope abundance distribution in the gas centrifugal machine is stable. The method has the advantages of low energy consumption, large separation coefficient and no isotope interference except carbon element in the working medium, and is suitable for cascade-form large-scale production.
Description
Technical Field
The invention relates to the technical field of isotope separation preparation, in particular to a method for centrifugally separating carbon isotopes by taking methyl iodide as a medium.
Background
Carbon has two naturally stable isotopes: carbon-12 (98.9%), carbon-13 (1.1%). In recent years, carbon-13 has become more and more widely used in agriculture ecology, drug metabolism, medical diagnosis and the like, and especially, the breath Test (UBT) for enriching carbon-13 urea has become a main means for clinical diagnosis of helicobacter pylori. The domestic market of the carbon-13-enriched urea breath test is in a growing stage and has the development potential advantage, so that economic and efficient carbon isotope separation preparation methods are more and more concerned.
The principle of the gas centrifugation method is that the radial pressure intensity distribution formed by components with different relative molecular masses in the centrifugal force field of the gas centrifuge is different, so that the relative separation among the components is realized, and the absolute separation among isotopes is not realized. Through the parallel connection and the serial connection of the separation units, a centrifugal separation cascade is formed, and a high-abundance product can be obtained. The structure of the gas centrifuge is one feed and two discharge, wherein light components are enriched at a concentrate end, and heavy components are enriched at a lean end. The gas centrifugal separation effect is influenced by many aspects, including influences such as physical property parameter, centrifuge structure parameter, centrifugation fluid parameter of working medium, because gas centrifuge is applied to the particularity of uranium enrichment production, some performance parameters are in secret state.
The separation and preparation method of the carbon isotope mainly comprises a low-temperature rectification method, a chemical exchange method, a gas centrifugation method and the like, wherein the low-temperature rectification method forms industrial production abroad, the production capacity of the carbon-13 enrichment can reach 700kg/a internationally, and the main production place is the United states. The separation and preparation research of domestic carbon isotopes has been carried out for many years, and Shanghai chemical research institute is working on the industrialization of the low-temperature rectification method; the engineering physical system of Qinghua university successively uses n-octane and freon-11 as working media to implement gas centrifugal separation of carbon isotope. In addition, no other published documents about the carbon isotope separation preparation method at home and abroad are published. However, the above-mentioned gas centrifugal separation methods of carbon isotopes all have the problem of requiring multi-element separation, and the separation coefficient is relatively small, which brings higher equipment cost when used for cascade production, and the cascade design process is also more complicated.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide a method for centrifugally separating carbon isotopes using methyl iodide as a medium, so as to at least partially solve at least one of the above-mentioned technical problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for centrifugally separating carbon isotopes by taking methyl iodide as a medium comprises the following steps:
step A: purifying light impurities in the methyl iodide raw material to ensure that the chemical purity of the light impurities meets the centrifugal separation requirement of the methyl iodide;
and B: introducing the purified gaseous methyl iodide into a gas centrifuge, adjusting the feed flow and the pressure of a concentrate pipe orifice and a lean pipe orifice of the gas centrifuge, and respectively separating concentrate and lean from the concentrate pipe orifice and the lean pipe orifice;
and C: and maintaining stable fluid parameters of methyl iodide feeding, concentrate and lean materials, and respectively collecting the concentrate and lean materials with stable carbon isotope abundance distribution through a liquid nitrogen cold trap after the gas centrifugal machine continuously runs until the carbon isotope abundance distribution in the gas centrifugal machine is stable.
Preferably, in the step a, the chemical purity of the purified methyl iodide raw material reaches more than 99.5%.
Preferably, in the step B, the feed flow of the gas centrifuge is 11.5-19.5 g/h, the split ratio is 0.4-0.6, and the pressure of the concentrate nozzle and the pressure of the lean nozzle of the gas centrifuge are both 175-300 Pa.
Preferably, in step C, the gas centrifuge is continuously operated for 1.5 hours or more to stabilize the distribution of the abundance of carbon isotopes therein.
Preferably, step C further comprises the step of performing mass spectrometry on the concentrate and the barren material to obtain a separation coefficient: adjusting ion source parameters of the gas mass spectrometer to (CH)3I)+The ion cluster is an analysis object, so that the carbon isotope content of the concentrate and the lean is accurately analyzed to calculate the separation system.
Preferably, the gas centrifuge is stand-alone or staged inline.
Based on the technical scheme, the invention has the following beneficial effects:
(1) the invention takes the methyl iodide as a working medium, can avoid the problem of complex multi-element separation as the condition that isotope interference except carbon element does not exist, has advantages in the aspects of centrifugal separation production cascade design and optimization, and has stronger technical feasibility and certain economical efficiency.
(2) The method has the advantages that the methyl iodide is used as a working medium, working parameters such as pressure intensity, flow rate and the like of the gas centrifuge are reasonably adjusted, the single-machine separation coefficient reaches 1.11, the method is suitable for cascade-form large-scale production, the obtained lean material and the raw material are only different in abundance, and the recovery and the continuous use of the lean material as a chemical reagent are not influenced at all, so the method has certain market application value.
(3) Compared with the current industrial production method of carbon isotopes, namely a low-temperature rectification method, the carbon isotope separation method has lower energy consumption.
Drawings
FIG. 1 is a schematic structural diagram of a system for centrifugal separation of carbon isotopes using methyl iodide as a medium according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for centrifugal separation of carbon isotopes using methyl iodide as a medium according to an embodiment of the present invention;
FIG. 3 shows the results of mass spectrometry for separation of methyl iodide using a single column in example 1 of the present invention.
In the above figures, the reference numerals have the following meanings:
1-gas centrifuge; 2-a lean material tank; 3-a concentrate tank; 4-liquid nitrogen cold trap; 5, a sampler; 6-gas mass spectrometer; 7-vacuum pump.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
For separating carbon isotopes by gas centrifugation, a working medium is one of the key elements, and the working medium for gas centrifugation generally satisfies the following three conditions:
1) the product can be kept stable and not decomposed at the temperature lower than 300 ℃;
2) a relative molecular mass of not less than 70;
3) at normal temperature, the saturated vapor pressure is not less than 665 Pa.
Iodomethane (CH)3I) The relative molecular mass is 141.94, the pyrolysis is difficult, the saturated vapor pressure at room temperature is about 50kPa, the requirement of a gas centrifugal method on a working medium is met, and meanwhile, the preparation of the iodomethane serving as a common chemical reagent has a stable and mature process, which is also an advantage condition for selecting the iodomethane as the working medium.
The present invention provides a method for centrifugally separating carbon isotope by using methyl iodide as medium, and is characterized by that the natural stable isotope of iodine is only one iodine-127, and the natural abundance of deuterium as hydrogen isotope is very low (0.0115%), and it can completely consider that the working medium methyl iodide is binary separated, and two components are respectively12CH3I and13CH3and the corresponding relative molecular masses are 142 and 143, so that the problem of introducing multi-element separation is avoided, and a good carbon isotope separation effect is achieved.
The method can be realized by utilizing the existing gas centrifugal separation system, the structure of the gas centrifugal separation system is shown in figure 1, and the gas centrifugal separation system comprises a gas centrifugal machine 1, a material supply and taking unit, a lean material tank 2, a fine material tank 3, a liquid nitrogen cold trap 4, a material taking device 5 and a vacuum pump 7, wherein:
the structure of gas centrifuge 1 is conventional structure in this technical field, get the material unit through supplying and carry methyl iodide in order to carry out carbon isotope separation to gas centrifuge 1, lean material, the beneficiated burden that separates through gas centrifuge 1 are got the material unit through supplying respectively and are carried to lean material jar 2 and beneficiated burden jar 3 in, lean material jar 2 and beneficiated burden jar 3 set up in liquid nitrogen cold trap 4, in order to cool off the beneficiated burden material and lean material and collect, vacuum pump 7 is connected to supplying and gets the material unit, in order to maintain the air partial pressure that supplies to get the material unit at certain extent.
FIG. 2 is a flow chart of a method for centrifugal separation of carbon isotopes using methyl iodide as a medium according to an embodiment of the present invention. As shown in fig. 2, the present invention provides a method for centrifugally separating carbon isotopes by using methyl iodide as a medium, comprising:
step A: purifying light impurities in the methyl iodide raw material to ensure that the chemical purity of the light impurities meets the centrifugal separation requirement of the methyl iodide;
wherein, the light impurities are the term of art, and refer to impurities with much smaller molecular weight relative to the working medium, such as impurities with molecular weight below 50% of the molecular weight of the working medium; the light impurities are impurities with much smaller molecular weight relative to the raw material of the methyl iodide, mainly air and water vapor, and the natural methyl iodide raw material, namely the methyl iodide raw material under natural abundance, can be purified by using a mixture of liquid nitrogen and 'liquid nitrogen-absolute ethyl alcohol' as a coolant and utilizing the difference of saturated vapor pressure of methyl iodide and light impurities to ensure that the chemical purity of the methyl iodide reaches more than 99.5 percent so as to meet the requirement of gas centrifugal separation.
And B: introducing the purified gaseous methyl iodide into a gas centrifuge, adjusting the feed flow and the pressure of a concentrate pipe orifice and a lean pipe orifice of the gas centrifuge, and respectively separating concentrate and lean from the concentrate pipe orifice and the lean pipe orifice;
by way of example, the gas centrifuge 1 used in the present invention is a stand-alone gas centrifuge, a feeding hole plate is arranged in the feeding and extracting unit, and is connected to the gas centrifuge 1 through a pipeline, and methyl iodide can be introduced into the gas centrifuge 1 through the feeding hole plate at a feeding flow rate of 11.5-19.5 g/h; the pipeline connecting the material supply and taking unit and the gas centrifuge is also provided with a valve, the flow split ratio is adjusted to be 0.4-0.6 through the valve, the pressure of the concentrate pipe orifice and the lean pipe orifice is 175-300 Pa, and the high separation coefficient of the carbon isotopes can be ensured under the condition.
In the separation process, the vacuum pump 7 is used for maintaining the air partial pressure of the material supplying and taking unit within 2Pa, and the liquid nitrogen cold trap is used for collecting the concentrate and the lean material respectively.
And C: and maintaining stable fluid parameters of the methyl iodide feeding material, the concentrate and the lean material, and obtaining the concentrate and the lean material containing the concentrated/depleted carbon isotopes after the gas centrifuge continuously operates until the distribution of the carbon isotope abundance is stable.
Preferably, the gas centrifuge is operated for more than 1.5 hours after the flow parameters of the methyl iodide feeding material, the concentrate and the lean material are stabilized, so that the carbon isotope graduation distribution in the gas centrifuge is stable;
the method also comprises the steps of sampling the concentrate and the lean material and performing mass spectrometry by using a gas mass spectrometer to calculate the separation coefficient. Wherein the step of performing mass spectrometry on the concentrate and the barren material comprises: adjusting ion source parameters of the gas mass spectrometer to (CH)3I)+The ion clusters are the analysis objects, so that the carbon isotope content of the concentrate and the lean material is accurately analyzed.
The technical scheme of the invention is further illustrated by the following specific examples:
example 1
The purified gaseous methyl iodide is introduced into a single-machine gas centrifuge at a feeding flow of about 15g/h by adjusting a feeding orifice plate, the pressure of the orifices of fine and lean materials of the centrifuge is adjusted to be about 230Pa by a valve of a feeding and taking unit, the flow division ratio is 0.5, the gas centrifuge needs to continuously and stably operate for more than 1.5 hours after the fluid parameters of the methyl iodide feeding, the fine and lean materials reach a stable state, then liquid nitrogen cold traps are used for receiving the materials at the fine material tank and the lean material tank respectively, and a vacuum pump is used for maintaining the air partial pressure of the feeding and taking unit within 2Pa in the separation process.
The separation coefficient is obtained by analyzing the sample, and the calculation formula is as follows: gamma ═ Cp/(1-Cp)]/[Cw/(1-Cw)]Wherein γ is the separation coefficient, CpAbundance of carbon-12 in the concentrate, CwIs the abundance of carbon-12 in the lean material. The results of the stand-alone centrifugation of this example are shown in figure 3,and calculating according to the mass spectrum analysis result to obtain a single-machine separation coefficient of 1.11. In the prior art, the single-machine separation coefficient of separating the carbon isotopes by taking normal octane as a medium is 1.08, and the single-machine separation coefficient of separating the carbon isotopes by taking Freon as a medium is 1.08.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method of centrifugally separating carbon isotopes, comprising:
step A: purifying light impurities in the methyl iodide raw material to ensure that the chemical purity of the light impurities meets the centrifugal separation requirement of the methyl iodide;
and B: introducing the purified gaseous methyl iodide serving as a medium into a gas centrifuge, adjusting the feed flow and the pressure of a concentrate pipe orifice and a lean pipe orifice of the gas centrifuge, and respectively separating concentrate and lean from the concentrate pipe orifice and the lean pipe orifice;
and C: and maintaining stable fluid parameters of methyl iodide feeding, concentrate and lean materials, and respectively collecting the concentrate and lean materials with stable carbon isotope abundance distribution through a liquid nitrogen cold trap after the gas centrifugal machine continuously runs until the carbon isotope abundance distribution in the gas centrifugal machine is stable.
2. The method of claim 1, wherein in step a, the chemical purity of the purified methyl iodide feedstock is greater than 99.5%.
3. The method according to claim 1, wherein in the step B, the feed flow of the gas centrifuge is 11.5-19.5 g/h, the split ratio is 0.4-0.6, and the pressure of the concentrate nozzle and the lean nozzle of the gas centrifuge is 175-300 Pa.
4. The method of claim 1, wherein in step C, the gas centrifuge is continuously operated for 1.5 hours or more to stabilize the distribution of the abundance of carbon isotopes therein.
5. The method of claim 1, wherein step C further comprises the step of performing mass spectrometry on the fine material and the lean material to obtain separation coefficients: adjusting ion source parameters of a gas mass spectrometer to (CH)3I)+The ion cluster is an analysis object, so that the carbon isotope content of the concentrate and the lean material is accurately analyzed to calculate the separation coefficient.
6. The method of claim 1, wherein the gas centrifuge is stand-alone or staged inline.
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| CN100569344C (en) * | 2008-03-17 | 2009-12-16 | 清华大学 | With the normal octane is the method for medium centrifugation separation of carbon isotope |
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