CN100571850C - The recycling technology of molecular sieve adsorption product gas during neon isotope separates - Google Patents
The recycling technology of molecular sieve adsorption product gas during neon isotope separates Download PDFInfo
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- CN100571850C CN100571850C CNB031295886A CN03129588A CN100571850C CN 100571850 C CN100571850 C CN 100571850C CN B031295886 A CNB031295886 A CN B031295886A CN 03129588 A CN03129588 A CN 03129588A CN 100571850 C CN100571850 C CN 100571850C
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- gas
- molecular sieve
- product gas
- sieve adsorption
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Abstract
The present invention relates to the recycling technology of molecular sieve adsorption product gas in the neon isotope separation, molecular sieve adsorption gas adopts the segmentation desorb to reclaim 90～95% in this technology, reclaims gas and purifies the employing chemical method, removes O by metal Cu bits and sponge Ti
2, N
2, H
2, decontaminating column is vertically placed, two ends filling Cu bits, and the centre is a sponge Ti, CO
2Adopt NaOH solution to absorb, gas adopts the thermosiphon principle Natural Circulation in the decontaminating column, and gas purity can purify to 99% by 70～98%; Technology of the present invention is simple, and the purification efficiency height need not too much manually-operated, and cost-saved about 20%.
Description
Technical field
The present invention relates to thermal diffusion method segregational stability isotope
22The additional technology of Ne production technology, relate in particular to neon isotope separate in the recycling technology of molecular sieve adsorption product gas.
Background technology
In the prior art, still find no specially at the recovery of the too high product gas of impurity and the report of purification.
At thermal diffusion method segregational stability isotope
22During Ne produces,, cause still residual large-tonnage product gas in the final molecular sieve, thereby wasted large-tonnage product because of adopting molecular sieve low temperature purification impurity; Because system has little air to reveal unavoidably, cause O in the product simultaneously
2, N
2, CO
2Higher Deng impurity; In addition, also there are contingencies such as packing failure, product impurity is too high or abundance is defective in this separating technology.In order to guarantee that product purity is 99.99%, generally adopt the molecular sieve low temperature purification, but caused 20% product loss simultaneously.
Summary of the invention
Purpose of the present invention just provides the recycling technology of molecular sieve adsorption product gas in simple, easy to operate, the energy-conservation neon isotope separation of a kind of technology.
Purpose of the present invention can be achieved through the following technical solutions: the recycling technology of molecular sieve adsorption product gas during neon isotope separates is characterized in that this technology may further comprise the steps:
(1) recovery of molecular sieve adsorption product gas
The molecular sieve outlet of having adsorbed product gas is connected with the import that purifies bottle, slowly remove molecular sieve adsorption section liquid nitrogen, the molecular sieve cold-trap heats up gradually, the slow desorb of adsorbed gas, and introduce purification bottle, controlled pressure constant (atmospheric pressure), then entering the gas volume that purifies bottle equates with the volume of discharge water, liquid water in this purification bottle plays fluid-tight and metering effect, when reclaim gas reach the absorption cumulative volume 90～95% the time close and purify a bottle terminal valve, residual gas emptying in the molecular sieve;
(2) reclaim gas cleaning
It is impure higher to be recycled to the molecular sieve desorb product gas that purifies in the bottle, and purity is 70～98% moles, and impurity is mainly O
2, N
2, CO
2, adopt the decontaminating column that contains sponge Ti and Cu bits to purify desorb product gas by chemical method, reaction equation is:
4Cu+O
2→2Cu
2O
2Cu
2O+O
2→4CuO
Ti+O
2→TiO
2
Ti+H
2→TiH
2
Ti+N
2→TiN
2
Gas adopts thermosiphon principle in the decontaminating column, cold gas purifies the interior gaseous exchange of bottle to the decontaminating column bottom constantly through the upwards diffusion of decontaminating column of vertical placement, realizes circularly purifying, recovery gas in purifying bottle stops heating after reaching and purifying requirement, changes this gas over to the packaging system packing; Described decontaminating column is vertical the setting, its central filling sponge Ti, and two ends are the Cu bits, and the thermal source that described thermal siphon is adopted be and the corresponding vertically disposed electric furnace of decontaminating column, and the central temperature of this electric furnace is 700～1000 ℃, and two ends are 400～700 ℃.
Recovery gas after the described purification is and contains micro-O
2, N
2, CO
2, Ar the neon isotope product, its purity is up to 99.9% mole, this product can reach more high-purity with the molecular sieve cryogenic absorption again, it is high-purity 〉=99.99% mole more.
CO in the recovery gas after the described purification
2When surpassing 0.1% mole, a certain amount of NaOH can be added the purification bottle, be made into the solution of 0.1～0.5 mol, to remove CO
2
In the recycling step of described molecular sieve adsorption product gas, can adopt cascade raising temperature, reclaim 90～95% moles adsorbed gas of preferential desorb.
The Cu/Ti length ratio of described decontaminating column is 1/6～1/2.
Cu in the described decontaminating column considers one or more replacements in available Fe, Zn, Ni, the Mg bits to be worth doing.
Described decontaminating column can be selected one or more for use, and this one or more decontaminating column can purify one bottle or purify several bottles simultaneously and reclaim gas.
Described technology also is applicable in He, Ar, Kr, the Xe rare gas and contains O
2, N
2, H
2, CO
2The purification of impurity.
The described liquid water that purifies in the bottle can replace with difficult volatile solvent paraffin oil.
Compared with prior art, the present invention has following beneficial effect and advantage:
1. technology of the present invention is simple, easy to operate, needs manually-operated during purification hardly, uses raw material cheapness, purification efficiency height, the selectivity height.
2. the present invention has remedied existing
22The product loss that molecular sieve purification causes during Ne isotopic separation product can reduce by about 20% product loss.
3. the present invention is equally applicable to contain O
2, N
2, H
2, CO
2Other gas cleaning of impurity.
4. the present invention adopts thermosiphon principle to realize natural back flow, need not any power consumption.
5. technology of the present invention is flexible, can adopt a decontaminating column to purify several bottles of gases simultaneously, also can adopt several decontaminating columns to purify.The cleanser kind and the amount of the every interior filling of decontaminating column all can change with concrete condition.Cleanser Cu considers metals such as available Fe, Zn, Ni, Mg bits to be worth doing and replaces, and can select one or more cleansers simultaneously for use.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
The invention will be further described below in conjunction with the accompanying drawings and the specific embodiments.
As shown in Figure 1, a kind of
22The recycling technology of molecular sieve adsorption product gas during Ne separates, this technology comprise molecular sieve adsorption product gas recovery, reclaim processing step such as gas cleaning; The flow chart of the recycling step of described molecular sieve adsorption product gas does not show that the equipment of described recovery gas cleaning step comprises purification bottle 1, circulating air import 2, sample tap (also being simultaneously product gas outlet after import of molecular sieve adsorption gas and the purification) 3, water filling port 4, electric furnace 5, Cu bits 6, sponge Ti 7, circulating air outlet 8, water (or alkali lye) 9, discharge outlet 10, decontaminating column 11; Described decontaminating column 11 is vertical the setting, its central filling sponge Ti 7, two ends are Cu bits 6, described electric furnace 5 is arranged on the both sides of this decontaminating column 11, and gas adopts thermosiphon principle in the decontaminating column 11, and cold gas is constantly through the upwards diffusion of the vertical decontaminating column of placing 11, purify bottle 1 interior gaseous exchange to decontaminating column 11 bottoms, realize circularly purifying, the recovery gas in purifying bottle 1 stops heating after reaching and purifying requirement, changes this gas over to the packaging system packing.
In once packing, 8500ml is arranged in the gas bottle
22The Ne abundance is 47.5% neon isotope product, and purity is 99% mole.Through packed behind the molecular sieve low temperature purification 8 * 800ml, purity be 99.99% mole 47.5%
22The Ne product.Molecular sieve adsorption 2100ml.When reclaiming molecular sieve adsorption gas, the segmentation desorb is reclaimed 2000ml to the purification bottle, residue 100ml emptying.So reclaim the inferior product that can obtain 8000ml impurity for 6 times and exceed standard (O wherein
21.21% mole, N
23.56% mole, CO
20.3% mole).The electric furnace of decontaminating column is opened, and gas circulation purifies.Purify column length 600mm, internal diameter 10mm, in fill sponge Ti 500mm, upper and lower respectively have a Cu bits 50mm.Sample analysis behind the 24h, product purity are higher than 99% mole of (O wherein
20.10% mole, N
20.31% mole, CO
20.05% mole).Access package assembling system packing obtains 8 * 800ml, purity and is 99.99% mole qualified products behind molecular sieve purification.With reclaim before compare, reduced by 17% mole loss.
As shown in Figure 1, a kind of
22The recycling technology of molecular sieve adsorption product gas during Ne separates, this technology comprise molecular sieve adsorption product gas recovery, reclaim processing step such as gas cleaning; The flow chart of the recycling step of described molecular sieve adsorption product gas does not show that the equipment of described recovery gas cleaning step is identical with embodiment 1.
9000ml99% is arranged
22Ne purity is 95% neon isotope gas, and the 400mm sponge Ti is being housed, and purifies on the upper and lower decontaminating column that respectively has Cu to consider 100mm, internal diameter 10mm to be worth doing.Behind the 24h, purity reaches 98%, and 48h is 99%.Can get 8600ml99%
22Ne changes this gas over to packaging system, obtain 8 * 800ml, purity and be 99.99% 99%
22The Ne isotope product.
As shown in Figure 1, a kind of
22The recycling technology of molecular sieve adsorption product gas during Ne separates, this technology comprise molecular sieve adsorption product gas recovery, reclaim processing step such as gas cleaning; The flow chart of the recycling step of described molecular sieve adsorption product gas does not show that the equipment of described recovery gas cleaning step is identical with embodiment 1.
Reveal because of the tower cascade, cause in the gas bottle 9000ml head product impurity too high, purity is 90%.For reaching purity requirement, change this head product over to the purification bottle; Purify with inferior product and same decontaminating column of coupling of another bottle impurity too high (purity 95%).Column length 800mm, internal diameter 15mm are equipped with the 500mm sponge Ti, and upper and lower respectively have Cu to consider 100mm to be worth doing.Open the decontaminating column power supply, purity is 96% behind the 24h, can reach 99% behind the 72h.Change packaging system over to, adjust after the abundance directly packing, obtain qualified products.
As shown in Figure 1, a kind of
22The recycling technology of molecular sieve adsorption product gas during Ne separates, this technology comprise molecular sieve adsorption product gas recovery, reclaim processing step such as gas cleaning; The flow chart of the recycling step of described molecular sieve adsorption product gas does not show that the decontaminating column of described recovery gas cleaning step is by two series connection, and two electric furnaces heat respectively, and all the other are identical with embodiment 1.
It is 95% helium that 10 liters of purity are arranged, and wherein contains O
22.0%, N
22.1%, H
20.5%, CO
20.4%, on two decontaminating columns, purify, purify column length 100mm, internal diameter 10mm.Purifying the interior solution of bottle is 0.1MNaOH.First interior filling Cu/Zn, 400 ℃ of second filling sponge Ti of furnace temperature, 800 ℃ of furnace temperatures.Helium purity reaches 99.45% after purifying 24h, wherein contains O
20.1%, N
20.2%, H
20.05%, CO
20.1%.
Claims (9)
1. the recycling technology of molecular sieve adsorption product gas during neon isotope separates is characterized in that this technology may further comprise the steps:
(1) recovery of molecular sieve adsorption product gas
The molecular sieve outlet of having adsorbed product gas is connected with the import that purifies bottle, slowly remove molecular sieve adsorption section liquid nitrogen, the molecular sieve cold-trap heats up gradually, the slow desorb of adsorbed gas, and introduce the purification bottle, controlled pressure is constant, then enters the gas volume that purifies bottle and equates with the volume of discharge water, when reclaim gas reach the absorption cumulative volume 90～95% the time close and purify a bottle terminal valve, residual gas emptying in the molecular sieve;
(2) reclaim gas cleaning
It is impure higher to be recycled to the molecular sieve desorb product gas that purifies in the bottle, and purity is 70～98% moles, and impurity is mainly O
2, N
2, CO
2, adopt the decontaminating column that contains sponge Ti and Cu bits to purify desorb product gas by chemical method, reaction equation is:
4Cu+O
2→2Cu
2O
2Cu
2O+O
2→4CuO
Ti+O
2→TiO
2
Ti+H
2→TiH
2
Ti+N
2→TiN
2
Gas adopts thermosiphon principle in the decontaminating column, cold gas purifies the interior gaseous exchange of bottle to the decontaminating column bottom constantly through the upwards diffusion of decontaminating column of vertical placement, realizes circularly purifying, recovery gas in purifying bottle stops heating after reaching and purifying requirement, changes this gas over to the packaging system packing; Described decontaminating column is vertical the setting, its central filling sponge Ti, and two ends are the Cu bits, and the thermal source that described thermal siphon is adopted be and the corresponding vertically disposed electric furnace of decontaminating column, and the central temperature of this electric furnace is 700～1000 ℃, and two ends are 400～700 ℃.
2. the recycling technology of molecular sieve adsorption product gas is characterized in that the recovery gas after the described purification is and contains micro-O during neon isotope according to claim 1 separated
2, N
2, CO
2, Ar the neon isotope product, this product reaches more high-purity with the molecular sieve cryogenic absorption again.
3. the recycling technology of molecular sieve adsorption product gas is characterized in that CO in the recovery gas after the described purification during neon isotope according to claim 1 separated
2When surpassing 0.1% mole, a certain amount of NaOH is added the purification bottle, be made into the solution of 0.1～0.5 mol, to remove CO
2
4. the recycling technology of molecular sieve adsorption product gas during neon isotope according to claim 1 separates, it is characterized in that, in the recycling step of described molecular sieve adsorption product gas, adopt cascade raising temperature, reclaim 90～95% moles adsorbed gas of preferential desorb.
5. the recycling technology of molecular sieve adsorption product gas is characterized in that the Cu/Ti length ratio of described decontaminating column is 1/6～1/2 during neon isotope according to claim 1 separated.
6. the recycling technology of molecular sieve adsorption product gas is characterized in that during neon isotope according to claim 1 separated, one or more replacements in the Cu crumb Fe in the described decontaminating column, Zn, Ni, the Mg bits.
7. the recycling technology of molecular sieve adsorption product gas is characterized in that described decontaminating column is selected one or more for use during neon isotope according to claim 1 separated, and this one or more decontaminating column purifies one bottle or purify several bottles simultaneously and reclaim gas.
8. the recycling technology of molecular sieve adsorption product gas is characterized in that described technology also is applicable in He, Ar, Kr, the Xe rare gas and contains O during neon isotope according to claim 1 separated
2, N
2, H
2, CO
2The purification of impurity.
9. the recycling technology of molecular sieve adsorption product gas is characterized in that during neon isotope according to claim 1 separated, and the described liquid water that purifies in the bottle replaces with difficult volatile solvent paraffin oil.
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|---|---|---|---|
| CNB031295886A CN100571850C (en) | 2003-06-30 | 2003-06-30 | The recycling technology of molecular sieve adsorption product gas during neon isotope separates |
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|---|---|---|---|
| CNB031295886A CN100571850C (en) | 2003-06-30 | 2003-06-30 | The recycling technology of molecular sieve adsorption product gas during neon isotope separates |
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|---|---|
| CN1565711A CN1565711A (en) | 2005-01-19 |
| CN100571850C true CN100571850C (en) | 2009-12-23 |
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| CN103977707B (en) * | 2014-05-27 | 2016-08-24 | 中国科学院青海盐湖研究所 | The method utilizing modified MCM-41 molecular sieve adsorption Separation of boron isotopes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087319A (en) * | 1992-11-19 | 1994-06-01 | 化学工业部上海化工研究院 | The preparation method of low pressure high pure hydrogen nitrogen mixed gas |
| US6572681B1 (en) * | 1998-07-22 | 2003-06-03 | Air Products And Chemicals, Inc. | Purification of gases |
-
2003
- 2003-06-30 CN CNB031295886A patent/CN100571850C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087319A (en) * | 1992-11-19 | 1994-06-01 | 化学工业部上海化工研究院 | The preparation method of low pressure high pure hydrogen nitrogen mixed gas |
| US6572681B1 (en) * | 1998-07-22 | 2003-06-03 | Air Products And Chemicals, Inc. | Purification of gases |
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|---|---|
| CN1565711A (en) | 2005-01-19 |
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Granted publication date: 20091223 Termination date: 20120630 |