CN1233445C - Separation and purification method of medium abundance 22 Ne isotope - Google Patents
Separation and purification method of medium abundance 22 Ne isotope Download PDFInfo
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- CN1233445C CN1233445C CN 02151014 CN02151014A CN1233445C CN 1233445 C CN1233445 C CN 1233445C CN 02151014 CN02151014 CN 02151014 CN 02151014 A CN02151014 A CN 02151014A CN 1233445 C CN1233445 C CN 1233445C
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Abstract
The present invention relates to a separation and purification method of medium-abundance <22>Ne isotopes, which comprises the following steps that neon feed gas is led into cylindrical retention tower with a cooling device, a vertical heating cord arranged in the center of the tower is heated, the <20>Ne component is diffused upwards along the heating cord, the <22>Ne component is diffused downwards along a cold wall, and the <22>Ne components are collected, namely that medium-abundance <22>Ne gas is separated. The retention tower has 1 to 5 cascades which are connected with cold reflux tubes and hot reflux tubes, the retention tower is 4.5 to 20 meters high, the diameter of the cold wall is 5 to 30mm, the heating cord is 1 to 4mm in diameter and has a temperature of 450 to 900 DEG C, and internal pressure of the retention tower is from-200 to 200 mmHg. the present invention has the advantages that the present invention can continuously directly prepare the medium-abundance 40 to 60% <22>Ne gas, has low cost and simple technology, and the products can improve the purity by further eliminating a trace amount of O2, N2, CO2 and other impurities.
Description
Technical field
The present invention relates to a kind of
22The isotopic separating and purifying method of Ne relates to a kind of thermal diffusion method that adopts or rather and directly separates abundance in the purification
22The isotopic production method of Ne.
Background technology
Neon (Ne) is a kind of rare rare gas element, and three kinds of isotropic substances are arranged:
20Ne,
21Ne and
22Ne, wherein
20Ne accounts for 90.92%,
22Ne only accounts for a very little part.
In the prior art, 1956 " The Journal Of Chemical Physics " the 24th phase p167-168 have reported that the general thermal diffusion column of humans such as Clausius prepares more than 99%
22Ne and
20Ne and 13%
21Ne, making assist gas with deuterium methane then will
21Ne further is concentrated to 99.6%.He had successfully extracted 99.8% in 1940
20Ne and 99.7%
22Each 2.5 liters of Ne.
The Mound of United States Atomic Energy Commission laboratory report in 1969, they adopt four post level Four thermodiffusion tower cascades to separate neon isotope, can access 99.95%
20Ne, productive rate are 4.2 liters/day, 2.0%
210.56 liter/day of Ne, 99.8%
220.22 liter/day of Ne.This method prepares high abundance neon isotope gas, and productive rate is low, and the cycle is long.
In addition, the report that utilizes cryogenic rectification method to separate neon isotope is also arranged, but this method requires the temperature operation below 24.5K, need high low temperature technique, and investment greatly is not suitable for the production of small-scale neon isotope.
But it is abundant that aforesaid method all just prepares
22Ne gas, abundance in needs
22The occasion of Ne isotope gas must be with the high abundance that makes
22Ne with
20Ne is mixed in proportion, and giving needs abundance in the use
22The user of Ne gas makes troubles, and has increased cost, has also caused the waste of the energy.
Summary of the invention
The purpose of this invention is to provide abundance in a kind of preparation
22The isotopic method of Ne, this method has overcome the defective of aforesaid method, and the isotopic preparation of abundance Ne in can directly carrying out is produced abundance and is 40～60%
22Ne gas, technology of the present invention is simple, and production cost is lower.
The present invention realizes like this.A kind of middle abundance of the present invention
22The isotopic separating and purifying method of Ne is that the neon unstripped gas is fed the cylindrical diffusion column that has refrigerating unit, and diffusion column central authorities are provided with a vertical nichrome wire, and the heating nichrome wire is lighter in the neon unstripped gas
20The Ne component is along upwards diffusion of nichrome wire, and is heavier
22The Ne component spreads downwards along cold wall, collects heavier
22The Ne component promptly obtains isolating middle abundance
22Ne gas, described diffusion column has 1～5 cascade, there is hot and cold return line to be connected between cascade and the cascade, 4.5～20 meters of diffusion column tower heights, 5～30 millimeters of cold wall diameters, described nichrome wire diameter is 1～4 millimeter, and the temperature of nichrome wire is controlled at 450～900 ℃, and described diffusion column internal pressure is controlled at-200～200mmHg.
The present invention adopts thermal diffusion method segregational stability isotropic substance
22Ne and
20Ne, neon unstripped gas are that steel cylinder is adorned high-purity neon, through the voltage stabilizing of voltage stabilizing gas holder, enter the cylindrical diffusion column that has refrigerating unit, diffusion column central authorities are provided with vertical nichrome wire, energising heating nichrome wire, the logical recirculated water cooling of diffusion column refrigerating unit, temperature of cooling water is below 30 ℃.Under heat effect, lighter in the neon isotope gas
20The Ne component slowly upwards spreads in tower central authorities along nichrome wire, and heavier
22Ne then is subjected to slowly diffusion downwards of outer wall water coolant effect, through diffusion after a while,
20Ne and
22Ne is enriched in the two ends of diffusion column respectively, collects heavier
22The Ne component promptly obtains middle abundance
22Ne gas.
Method of the present invention can be formed several cascades by diffusion column to be increased
22The output of Ne can have 1～5 cascade, preferred 3～5 cascades.Each cascade can have 1～5 diffusion column to compose in parallel.There is hot and cold return line to be connected between cascade and the cascade, neon refluxes by thermosyphon action, return line heat pipe diameter is 10～20 millimeters, cold pipe diameter is 5～10 millimeters, the return line heat pipe is provided with heating unit outward so that return line keeps certain temperature, temperature is controlled at 25～330 ℃, preferred 50～150 ℃ in the return line heat pipe.Through stage trapping, lighter like this
20Ne and heavier
22Ne is enriched in respectively in the two ends diffusion column of cascade, separates the purpose of purifying thereby reach.
In addition, also the number cover system can be connected mutually, the tail gas of last system can further improve the utilization ratio of unstripped gas as the unstripped gas of next system, is independent of each other each other, has avoided owing to the situation that causes total system all must stop is leaked in certain.
4.5～20 meters of the described diffusion column tower heights of the inventive method, preferred 6～10 meters, 5～30 millimeters of the cold wall diameters of tower.
The described nichrome wire temperature of the inventive method is controlled at 450～900 ℃, preferred 500～700 ℃; The nichrome wire diameter is 1～4 millimeter; The diffusion column internal pressure is controlled at-200～200mmHg, and is preferred-100～50mmHg.
Before the first cascade diffusion column, an extraction column is arranged, be used to separate light impurities, as H
2, He and part
20Ne, and improve the unstripped gas utilization ratio, in the end behind the cascade diffusion column impurity tower is arranged, be used to get rid of O
2, N
2, CO
2Deng heavy seeds.
Abundance during method of the present invention can prepare
22Ne gas, the abundance scope can change in 40～60% abundance.The discharging of product gas adopts draining to get the gas method.After the general a couple of days of driving, total system reaches the stable equilibrium, can begin continuous discharging.When just beginning discharging, can (L be a diffusion column cascade total length, m) determines initial load, then by analyzing every day according to (40～45) * L milliliter/sky
22The abundance of Ne gas changes regulates load, when measuring the abundance value and depart from set(ting)value, suitably regulate load what can obtain certain abundance
22Ne gas.In case system balancing, stably discharging.
Method facility investment of the present invention is little, expands the scale of production easily.Can make up according to the series-parallel connection of number, size and the diffusion column of the requirement of turnout design diffusion column increases
22The Ne turnout.
Separate the middle abundance that obtains for further improving
22The Ne gas purity, the present invention also can further remove the employing of the product gas after separating molecular sieve micro-O wherein under liquid nitrogen temperature
2, N
2, CO
2Deng impurity.Molecular screening 4A and 5A molecular sieve, place retort furnace at 500～600 ℃ of activation glass cold-trap of packing into after 3 hours, before each the use, molecular sieve need be 300～400 ℃ of following vacuum activation 3 hours, the vial of splendid attire product also need vacuumize under 300～400 ℃ 3 hours, the packing of product should (approximately-30mmHg), encapsulate by sintered glass product bottle inlet mouth in little negative pressure.Process purifies like this
22The Ne purity of product gas can reach 99.99%.
Of the present invention
22The isotopic separating and purifying method of Ne compared with prior art has the following advantages:
One, of the present invention
22The isotopic separating and purifying method technology of Ne is simple, can be at normal temperatures abundance in the direct production continuously
22Ne gas has avoided other thermal diffusion method to prepare high abundance earlier
22Ne and
20Ne isotope gas, and then the unreasonable method of mixing distribution have reduced production cost.
Two, method easy handling of the present invention is pollution-free, expands the scale of production easily, and reduced investment does not have undue requirement to working condition, has avoided the high facility investment of cryogenic rectification method, and to the harsh requirement of environment, material, working condition.
Three, adopt the product gas of the inventive method preparation also can adopt molecular sieve under liquid nitrogen temperature, to remove wherein micro-O
2, N
2, CO
2Deng impurity, further improve the purity of product gas.
Four, method cascaded design of the present invention does not increase cascade quantity by increasing diffusion column quantity and increases productive rate.
Description of drawings
Fig. 1 is the neon diffusion column structural representation of the inventive method.
Fig. 2 is an embodiment 7 tower level Four connection neon diffusion column system architecture synoptic diagram of the inventive method.
Shown in the number in the figure:
The 1-nichrome wire, the cold wall of 2-, 3-cooling water jecket, the 4-cold reflux mouth of pipe, 5-weight, 6-entrance of cooling water, 7-thief hole, the 8-thermal backflow mouth of pipe, 9-cooling water outlet, 10-diffusion column, 11-cold reflux pipe, 12-hot reflux condenser.
Embodiment
To further set forth the present invention by detailed description below, but embodiment not a limitation of the present invention to the specific embodiment of the inventive method.
Embodiment 1:
One cover, 7 tower level Four connection neon diffusion column apparatus system.First cascade is composed in parallel by 2 towers, and all the other each 1 towers of level Four connection are formed.Tower height is 6m, and the cold wall diameter of tower is respectively 13.5,13.9,14.5,17.2,18.6,19.4mm it is 1 millimeter nichrome wire that there is a diameter in the central authorities of tower, has hot and cold return line to be connected between tower and the tower, return line diameter 5mm, the heating nichrome wire, temperature is 600 ℃, the diffusion column internal pressure is 50mmHg, temperature in the hot reflux condenser is 100 ℃, and temperature of cooling water is 25 ℃.With abundance is that 9.22% Ne unstripped gas feeds diffusion column, after 5 days,
22The Ne abundance can reach 60%.If the discharging abundance is 60%
22Ne gas can produce 600 milliliters every day, if the discharging abundance is 50%
22Ne gas can produce 800 milliliters every day, if the discharging abundance is 40%
22Ne gas can be produced 1000 milliliters every day.Purity of product gas can reach 99%.
Embodiment 2:
The series connection of two 5 tower level Four connection neon diffusion column apparatus systems.Tower height is 10m, the cold wall diameter of tower is 30mm, it is 1.5 millimeters nichrome wire that there is a diameter in the central authorities of tower, there is hot and cold return line to be connected between tower and the tower, return line diameter 8mm, heating nichrome wire, temperature is 500 ℃, the diffusion column internal pressure is-50mmHg, and the temperature in the hot reflux condenser is 50 ℃, and temperature of cooling water is 25 ℃.With abundance is that 9.22% Ne unstripped gas feeds diffusion column, after 5 days,
22The Ne abundance can reach 60%.If the discharging abundance is 60%
22Ne gas can produce 1800 milliliters every day, if the discharging abundance is 50%
22Ne gas can produce 2200 milliliters every day, if the discharging abundance is 40%
22Ne gas can be produced 2500 milliliters every day.Purity of product gas can reach 99%.
Embodiment 3:
One cover, 10 towers, three cascade neon diffusion column apparatus systems.Tower height is 8m, the cold wall diameter of tower is 30mm, it is 4 millimeters nichrome wire that there is a diameter in the central authorities of tower, there is hot and cold return line to be connected between tower and Tata and the tower, return line diameter 10mm, heating nichrome wire, temperature is 800 ℃, the diffusion column internal pressure is-10mmHg, and the temperature in the hot reflux condenser is 150 ℃, and temperature of cooling water is 25 ℃.With abundance is that 9.22% Ne unstripped gas feeds diffusion column, after 5 days,
22The Ne abundance can reach 60%.If the discharging abundance is 60%
22Ne gas can produce 2200 milliliters every day, if the discharging abundance is 50%
22Ne gas can produce 3000 milliliters every day, if the discharging abundance is 40%
22Ne gas can be produced 3800 milliliters every day.Purity of product gas can reach 99%.
Claims (9)
1, a kind of middle abundance
22The isotopic separating and purifying method of Ne is characterized in that this method is that the neon unstripped gas is fed the cylindrical diffusion column that has refrigerating unit, and diffusion column central authorities are provided with a vertical nichrome wire, and the heating nichrome wire is in the neon unstripped gas
20The Ne component upwards spreads along nichrome wire,
22The Ne component spreads downwards along cold wall, collects
22The Ne component promptly obtains isolating middle abundance
22Ne gas, under liquid nitrogen temperature, remove impurity with molecular sieve, described diffusion column has 1～5 cascade, there is hot and cold return line to be connected between cascade and the cascade, 4.5～20 meters of diffusion column tower heights, 5～30 millimeters of cold wall diameters, described nichrome wire diameter is 1～4 millimeter, the temperature of nichrome wire is controlled at 450～900 ℃, and described diffusion column internal pressure is controlled at-200～200mmHg.
2, the method for claim 1 is characterized in that described diffusion column has 3～5 cascades, and every grade is associated with 1～5 diffusion column parallel connection.
3, the method for claim 1 is characterized in that 6～10 meters of described diffusion column tower heights.
4, the method for claim 1 is characterized in that the temperature of described nichrome wire is controlled at 500～700 ℃.
5, the method for claim 1 is characterized in that described diffusion column internal pressure is controlled at-100～50mmHg.
6, the method for claim 1 is characterized in that temperature is controlled at 25～330 ℃ in the described return line heat pipe.
7, the method for claim 1 is characterized in that described return line heat pipe diameter is 10～20 millimeters, and cold pipe diameter is 5～10 millimeters.
8, the method for claim 1 is characterized in that described molecular sieve is 4A and 5A molecular sieve.
9, method as claimed in claim 8 is characterized in that described molecular sieve activates 3 hours down at 500～600 ℃, activates 3 hours in 300～400 ℃ of following vacuum then before each the use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02151014 CN1233445C (en) | 2002-12-04 | 2002-12-04 | Separation and purification method of medium abundance 22 Ne isotope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02151014 CN1233445C (en) | 2002-12-04 | 2002-12-04 | Separation and purification method of medium abundance 22 Ne isotope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1513587A CN1513587A (en) | 2004-07-21 |
| CN1233445C true CN1233445C (en) | 2005-12-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02151014 Expired - Fee Related CN1233445C (en) | 2002-12-04 | 2002-12-04 | Separation and purification method of medium abundance 22 Ne isotope |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102851516B (en) * | 2012-09-29 | 2015-04-01 | 广东雪莱特光电科技股份有限公司 | Amalgam purifying method and container |
| CN106052302B (en) * | 2016-08-03 | 2019-01-18 | 上海启元气体发展有限公司 | One kind is separated from neon22The method of Ne |
| CN106196884B (en) * | 2016-08-03 | 2019-03-08 | 上海启元空分技术发展股份有限公司 | One kind is separated from neon21The method of Ne |
| CN106052301B (en) * | 2016-08-03 | 2019-01-18 | 上海启元气体发展有限公司 | A method of separating 20Ne from neon |
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2002
- 2002-12-04 CN CN 02151014 patent/CN1233445C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1513587A (en) | 2004-07-21 |
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Granted publication date: 20051228 Termination date: 20111204 |