CN1154464A - Ultra high purity nitrogen and oxygen generator unit - Google Patents
Ultra high purity nitrogen and oxygen generator unit Download PDFInfo
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- CN1154464A CN1154464A CN 96118992 CN96118992A CN1154464A CN 1154464 A CN1154464 A CN 1154464A CN 96118992 CN96118992 CN 96118992 CN 96118992 A CN96118992 A CN 96118992A CN 1154464 A CN1154464 A CN 1154464A
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Abstract
A unit capable of simultaneously producing liquid nitrogen of ultra high purity and liquid oxygen of ultra high purity, is provided. The inside of a first rectification column 6 is demarcated to an upper rectifying part 12, a middle rectifying part 13 and a lower rectifying part 14. To the upper part 11 above the upper rectifying part 12 is connected a nitrogen condenser 8. A second rectification column 7 has a reboiler 24 provided under its rectifying part 22. Ultra high purity liquid nitrogen is recovered from between the upper rectifying part 12 and middle rectifying part 22 of the second rectification column 7, where it is brought in countercurrent contact with gas evaporated by the reboiler 24 provided below the rectifying part 22 so that lower boiling point components are separated therefrom. Thus, ultra high purity liquid oxygen is recovered from below the rectifying part 22 of the second rectification column 7.
Description
The present invention relates to a kind of rectifying column that utilizes from as the nitrogen for ultra-high purity, the oxygen generator unit that generate nitrogen for ultra-high purity and super high pure oxygen the air of unstripped gas simultaneously, be particularly related to a kind of concentration that can generate as the oxygen of impurity and be 10ppb or nitrogen for ultra-high purity still less with and purity be 99.999995% or the generating apparatus of higher super high pure oxygen, this kind device can be used for semiconductor fabrication.
It number is a kind of traditional nitrogen for ultra-high purity of describing in 296,651/1993 the Japanese patent application, the flow chart of oxygen generator unit that Fig. 5 shows open (KOKAI).In this figure, label 54 expression first order rectifying columns, 55 expression second level rectifying columns, 56 expression third level rectifying columns, 57 expression fourth stage rectifying columns, 58 expression nitrogen condensers, 53 expression main heat exchangers, 59 expression expansion turbine.
After raw air is compressed, removed carbon dioxide in air and moisture content, make its cooling by main heat exchanger 53 then, along with the liquefaction of raw air, a part of raw air is admitted to the lower space part 54e of first order rectifying column 54.The liquid phase part that enters the raw air of lower space part 54e accumulates in the bottom of lower space part 54e, and gas phase part along first order rectifying column 54 to rising, promptly successively by rectifying part 54d, middle rectifying part 54c and last rectifying part 54b down in case with the withdrawing fluid counter current contacting that mainly comprises liquid nitrogen that flows down from top.Like this, oxygen in the gas phase and mainly contain the component (hydrocarbon, nitrogen, xenon etc.) that boiling point is higher than oxygen boiling point and absorbed, the nitrogen in the withdrawing fluid and mainly contain boiling point and be evaporated out than the low-boiling component of nitrogen (neon, hydrogen, helium etc.) and enter gas phase simultaneously by withdrawing fluid.Like this, the high pure nitrogen that contains the low boiling component is collected among the upper space part 54a, and the oxygen-rich liquid air that contains the higher boiling component is collected at lower space partly among the 54e.
The high pure nitrogen that is collected among the upper space part 54a is sent into nitrogen condenser 58, so that it is cooled down, then the high-purity liquid nitrogen of condensation like this is re-used as withdrawing fluid and sends into rectifying part 54b, meanwhile, assembled the incoagulable gas of low boiling component and from system, discharged.
The oxygen-rich liquid air that a part is collected among the lower space part 54e enters expansion valve 61, and is depressurized in this valve so that obtain the low temperature oxygen, then this oxygen is sent into nitrogen condenser 58 as a kind of refrigerant.Then this oxygen of discharging from nitrogen condenser 58 enters expansion turbine 59, carries out discharging from system after the heat exchange in main heat exchanger 53.
In nitrogen condenser 58 condensation and the liquid nitrogen of sending into rectifying part 54b when its from rectifying partly the 54b when dirty with the uprising gas counter current contacting of mainly forming by nitrogen, further remove remaining low boiling component in the liquid nitrogen thus, thereby obtained ultra-pure liquid nitrogen.This ultra-pure liquid is assembled nitrogen in the storage liquid layer 54g between the rectifying part 54c in the middle of last rectifying part 54b kind.As ultra-pure liquid nitrogen, part in them is drawn out of, by expansion valve 63 decompressions, behind over-heat-exchanger, offering the system outside, and remainder flows through middle rectifying part 54c downwards further as withdrawing fluid as a kind of ultra-pure nitrogen product.
Another part oxygen-rich liquid air that is collected among the lower space part 54e enters expansion valve 62, in this valve, be depressurized and the part vaporization, thereby obtain a kind of solution-airmixture, then this solution-airmixture is sent into second level rectifying column 55 rectifying part 55b above.The gas phase of this solution-airmixture partly is collected among the upper space part 55a, and its liquid phase part passes through rectifying part 55b to dirty as withdrawing fluid, in 55b, contact with the back flow of gas that rises from below, increased the concentration of oxygen owing to having discharged lower boiling component, and be collected among the lower space part 55c.The reboiler 71 that a heating is collected at the liquid among the 55c of this space is housed in lower space part 55c,, and rises by rectifying part 55b so that the component (argon, carbon monoxide, nitrogen etc.) that makes boiling point be lower than oxygen boiling point evaporates with oxygen selectively.Like this, the liquid oxygen that contains high boiling component is collected among the lower space part 55c, and the gas that contains aerobic, nitrogen and low boiling component is collected among the upper space part 55a, and they discharge system from tower bottom and top of tower respectively then.
The oxygen that is collected in the gas phase part on the lower space part 55c liquid level of second level rectifying column 55 is admitted among the lower space part 56c of third level rectifying column 56.In this lower space part 56c, with withdrawing fluid (high-purity liquid oxygen) counter current contacting, the higher boiling component is absorbed by withdrawing fluid thus when the oxygen sent into rises through rectifying part 56b, and a part of oxygen in the while withdrawing fluid also is evaporated out.The condenser 81 that cooling and condensation are collected at the gas (high purity oxygen) among the upper space part 56a and the gas of institute's condensation are offered rectifying part 56b as withdrawing fluid is housed in the upper space part 56a of third level rectifying column 56.Like this, the liquid oxygen that contains a little higher boiling component accumulates among the lower space part 56c, and the high purity oxygen gas that contains a little low boiling component accumulates among the upper interval part 56a.The liquid oxygen that contains the higher boiling component that accumulates among the lower space part 56c is returned among the lower space part 55c of second level rectifying column 55.
The high purity oxygen gas that is collected at upper space part 56a is admitted on fourth stage rectifying column 57 among the mid portion 57c between the rectifying part 57b and following rectifying part 57d.In mid portion 57c, when the high purity oxygen gas sent into rises by last rectifying part 57b and withdrawing fluid (high-purity liquid oxygen) counter current contacting, oxygen is absorbed by withdrawing fluid thus, and the low boiling component in the while withdrawing fluid is evaporated.The condenser 82 that cooling and condensation are collected at the gas (high purity oxygen) among the upper space part 57a and the gas of this condensation are offered rectifying part 57b as described withdrawing fluid is housed in the upper space part 57a of fourth stage rectifying column 57.On the other hand, in lower space part 57e, a reboiler 72 that is used for heating the liquid (ultra-pure liquid oxygen) that is collected at lower space part 57e is installed, so that being lower than the component of oxygen boiling point, boiling point evaporates with oxygen selectively, and so the component of evaporation rises, successively by down rectifying part 57d and last rectifying part 57b so that with withdrawing fluid (high-purity liquid oxygen) counter current contacting.Like this, ultra-pure liquid oxygen is collected among the lower space part 57e, and the oxygen that has gathered the low boiling component accumulates among the upper space part 57a.The oxygen that is collected among the upper space part 57a will be discharged system from top of tower, and the ultra-pure liquid oxygen that is collected among the lower space part 57e will be recovered and offer the system outside as a kind of product.
Open (KOKAI) a kind of method that generates nitrogen (99.97%) and ultra-pure oxygen (99.998%) by two rectifying columns that number has been 105,088/1986 Japanese Patent Application Publication.According to this method, raw air is admitted to the bottom of first order rectifying column and the oxygen-rich liquid air extracted out above the equilibrium stage from the rectifying part lower end of first order rectifying column is admitted to the top of second level rectifying column, wherein nitrogen-rich gas is separated near the top of first order rectifying column, and separates (Fig. 2 that sees communique) above the equilibrium stage of ultra-pure oxygen from the lower end of second level rectifying column rectifying part.
Although open (KOKAI) number is 296, the device of 651/1993 Japanese Patent Application Publication has can be by the advantage that unstrpped gas is liquefied and rectifying only produces nitrogen for ultra-high purity and super high pure oxygen from a device, but it also has some shortcomings, as four rectifying columns of needs, and make pipe-line system and operating condition complicated owing to be provided with a plurality of condensers and reboiler.And disclose (KOKAI) number is that the method for 105,088/1986 Japanese Patent Application Publication can not generate nitrogen for ultra-high purity simultaneously.
Consider the problems referred to above, the present invention is intended to propose a kind of device that can utilize simple device to generate nitrogen for ultra-high purity and super high pure oxygen simultaneously.
Nitrogen for ultra-high purity of the present invention, oxygen generator unit comprise:
First order rectifying column, by from top to bottom order, this tower has first upper space part, goes up the rectifying part, middle rectifying part, the rectifying part and the first lower space part down;
Second level rectifying column, it has second upper space part, rectifying part and the second lower space part;
Utilize and to carry out with refrigerant that indirect heat exchange is cooled off raw air and the air that will so cool off offers the following main heat exchanger of the described part of rectifying down;
High-purity liquid nitrogen is supplied with the described top high-purity liquid nitrogen supply pipe of going up the rectifying part as withdrawing fluid;
Be used for cooling off the nitrogen condenser of the high pure nitrogen that is collected at first upper space part, this condenser within it chilled high-purity liquid nitrogen as the part of withdrawing fluid supply with go up the rectifying part above, and incoagulable gas is discharged system;
Be used for making first expansion valve of the oxygen-rich liquid air decompression that is collected at first lower space part, the oxygen that this valve will generate is within it supplied with nitrogen condenser as refrigerant;
Be used for being provided at the oxygen that nitrogen condenser is made refrigerant, herein oxygen discharged the oxygen pipe of giving main heat exchanger as refrigerant then;
Be used for from reclaiming nitrogen for ultra-high purity carrier pipe between last rectifying part and the middle rectifying part as a part of withdrawing fluid of ultra-pure liquid nitrogen;
Be used to make from second expansion valve of the partial reflux liquid decompression that enters between middle rectifying part and the following rectifying part, the rectifying that the solution-airmixture that this valve will generate is within it supplied with second rectifying column partly above;
Be arranged in second lower space part be used to heat be collected at second lower space part liquid so that the reboiler that its part is evaporated;
Be used for to be collected at the gas discharge pipe that second upper space gas is partly discharged system; And
Be used for reclaiming super high pure oxygen carrier pipe as the liquid that is collected at second lower space part of ultra-pure liquid oxygen.
The method of utilizing this device to generate nitrogen for ultra-high purity and super high pure oxygen simultaneously will be described below.
Be provided for through the raw air that in main heat exchanger, cools down below the following rectifying part of first order rectifying column with the indirect heat exchange of refrigerant.On the other hand, as the high-purity liquid nitrogen of withdrawing fluid by the high-purity liquid nitrogen supply pipe from the system outside supply to first order rectifying column last rectifying part above.
The raw air that is infeeded rises along first order rectifying column, promptly successively by rectifying part, middle rectifying part and last rectifying part down so that with the withdrawing fluid counter current contacting that mainly contains liquid nitrogen that flows down from above.Like this, the component (hydrocarbon, nitrogen, xenon etc.) that oxygen in the gas phase and the boiling point that mainly contains are higher than oxygen boiling point is absorbed by withdrawing fluid, and simultaneously nitrogen in the withdrawing fluid and the boiling point that mainly the contains component (neon, hydrogen, helium etc.) that is lower than the nitrogen boiling point is evaporated out and enters gas phase.Like this, the high pure nitrogen that comprises the low boiling component is collected at the first upper space part, and the oxygen-rich liquid air that comprises the higher boiling component is collected at the first lower space part.
The high pure nitrogen that is collected in first upper space part is admitted to nitrogen condenser, so that it is cooled down, then so the high-purity liquid nitrogen that gets off of condensation by once more as the part of withdrawing fluid deliver to the rectifying part above, the incoagulable gas that the while has wherein been gathered the low boiling component is exhausted from system.
The oxygen-rich liquid air that is collected in first lower space part is admitted to first expansion valve, and the oxygen-rich liquid air is depressurized so that obtain the low temperature oxygen in this valve, and this oxygen will be admitted to nitrogen condenser as refrigerant then.The oxygen that to make refrigerant in nitrogen condenser offers main heat exchanger by the oxygen pipe again, and in this heat exchanger, oxygen cools off raw air as refrigerant, is exhausted from system at last.
Be admitted to the high-purity liquid nitrogen above the rectifying part and the high-purity liquid nitrogen and the uprising gas counter current contacting of mainly forming of condensation in nitrogen condenser as withdrawing fluid by nitrogen, so as high-purity liquid nitrogen from flow down through on the further wherein remaining low boiling component of release during the rectifying part.High-purity liquid nitrogen enters between rectifying part and the middle rectifying part then.Like this, the flow through high purity nitrogen of nitrogen for ultra-high purity carrier pipe of a part is recovered as a kind of ultra-pure liquid nitrogen product, and the high-purity liquid nitrogen of remainder flows downwards through middle rectifying part as withdrawing fluid.Again with a part of withdrawing fluid from extracting out between middle rectifying part and the following rectifying part and be admitted to second expansion valve, and remaining withdrawing fluid flows downwards through rectifying part down so as to absorb the higher boiling component in the raw air and be collected at last first lower space partly in.
Be admitted to that becoming in second expansion valve removed that the withdrawing fluid of the liquid air of higher boiling component is depressurized by second expansion valve and the part evaporation, so that the acquisition solution-airmixture, then this solution-airmixture is offered second level rectifying column the rectifying part above.The gas phase of this solution-airmixture partly is collected at the upper space part, and its liquid phase part flows downwards through rectifying part as withdrawing fluid so that by discharging the low boiling component with counter current contacting from following uprising gas and improving the concentration of oxygen, is collected at the lower space part then.Partly be provided with one in lower space and be used for heating the reboiler that is collected at the liquid in the lower space part, therefore its boiling point component (argon, carbon monoxide, nitrogen etc.) of being lower than oxygen boiling point is evaporated with oxygen selectively, and the component of so evaporation rises and through the rectifying part.The result contains the nitrogen that its boiling point is lower than the component of oxygen boiling point and is collected at the upper space part, and is exhausted from system from the top through flue gas leading, and ultra-pure liquid oxygen is collected at the lower space part, is recovered through the super high pure oxygen carrier pipe as a kind of product then.
In said apparatus, be utilized as device from the cold of the outside high-purity liquid nitrogen of introducing (withdrawing fluid) of system through the high-purity liquid nitrogen supply pipe and move necessary low-temperature receiver.Yet replace this low-temperature receiver also can in system, produce cold.In this case, an expansion turbine should be set, and in nitrogen condenser, be used as oxygen that refrigerant discharges then thus by the expansion turbine decompression, so that the temperature of oxygen is descended, and send into described main heat exchanger as refrigerant and cool off raw air.
By the also cold of recyclable ultra-pure liquid nitrogen of the 3rd expansion valve is set.In this case, by described nitrogen for ultra-high purity carrier pipe ultra-pure liquid nitrogen being sent into the 3rd expansion valve reduces pressure, and so the ultra-pure nitrogen of low temperature that generates is used as a part of refrigerant in the described nitrogen condenser, offers the system outside as product then.
In addition, raw air can be used as the thermal source of the reboiler in second lower space part that is arranged on second level rectifying column.In this case, the part material air is partly introduced reboiler as thermal source from first lower space, and the raw air through cooling and condensation turns back to the described first lower space part then.
Be collected at the thermal source that high pure nitrogen in first upper space part of first order rectifying column also can be further used as the reboiler in second lower space part that is arranged on second level rectifying column.In this case, the part high pure nitrogen is partly introduced reboiler as thermal source from first upper space, and the high-purity liquid nitrogen through cooling and condensation is provided for the rectifying part as a part of withdrawing fluid then.
And the amount for the withdrawing fluid of the following rectifying part of adjusting the first order rectifying column of flowing through is provided with a flow control valve.By this flow control valve, a part of withdrawing fluid is extracted and is directly entered out the first lower space part between middle rectifying part and following rectifying part.By flow through the down amount of withdrawing fluid of rectifying part of adjusting, can regulate the oxygen concentration in the liquid air of waiting to enter second rectifying column.
Fig. 1 shows the flow chart of an example of nitrogen for ultra-high purity based on the present invention, oxygen generator unit.In the figure, label 5 expression main heat exchangers, 6 expression first order rectifying columns, 7 expression second level rectifying columns, 8 expression nitrogen condensers, 11 expressions, the first upper space part, the rectifying part is gone up in 12 expressions, rectifying part in the middle of 13 expressions, 14 expressions are the rectifying part down, 15 expressions, the first lower space part, 21 expressions, the second upper space part, 22 expression rectifying parts, 23 expressions, the second lower space part, 24 expression reboilers, 31 expressions, first expansion valve, 32 expressions, second expansion valve, 33 expressions the 3rd expansion valve, 34 expressions the 4th expansion valve, 40 expression hot boxes, 100 expression high-purity liquid nitrogen supply pipes, 109 expression nitrogen for ultra-high purity carrier pipes, 110 expression super high pure oxygen carrier pipes, 117 expression oxygen pipes, 118 expression flue gas leadings.
First order rectifying column 6 from toply have the first upper space part 11 successively, go up rectifying part 12, middle rectifying part 13, the rectifying part 14 and the first lower space part 15 down, be useful on the storage part 16 of storage withdrawing fluid on last rectifying part 12, the following storage part 18 that is used on storage withdrawing fluid between last rectifying part 12 and the middle rectifying part 13 storage part 17 and is used for storage withdrawing fluid between middle rectifying part 13 and following rectifying part 14 in addition.Second level rectifying column 7 has the second upper space part 21, rectifying part 22 and the second lower space part 23.Raw air path in the main heat exchanger 5 is connected to the first lower space part 15 by pipeline 105.High-purity liquid nitrogen supply pipe 100 is connected to storage part 16, so that provide high-purity liquid nitrogen to be used as withdrawing fluid from the system outside.
The entrance side of nitrogen condenser 8 links to each other with the top of the first upper space part 21 by pipe 106, and it is discharged side and links to each other with storage part 16 with high-purity liquid nitrogen supply pipe 100 by managing 107.The discharge side of nitrogen condenser 8 also links to each other with pipe 119, so that by a gas-liquid separator (not shown) incoagulable gas is discharged system.The first refrigerant supply side of nitrogen condenser 8 links to each other with the bottom of the first lower space part 15 by pipe 108, and described pipeline 108 is provided with first expansion valve 31.First refrigerant of nitrogen condenser 8 is discharged side and is linked to each other with main heat exchanger 5 by oxygen pipe 117, and described pipeline 117 is provided with the 4th expansion valve 34.The second refrigerant supply side of nitrogen condenser 8 links to each other with last storage part 17 by nitrogen for ultra-high purity carrier pipe 109, and described nitrogen for ultra-high purity carrier pipe is provided with the 3rd expansion valve 33.Second refrigerant of nitrogen condenser 8 is discharged side and is linked to each other with main heat exchanger 5 by pipe 111.
Following storage part 18 links to each other with the top of rectifying part 22 of second level rectifying column 7 by pipe 114, and described pipeline 114 is provided with second expansion valve 32.
In the second lower space part 23, be provided with a reboiler 24.The thermal medium supply side of described reboiler 24 links to each other with the first lower space part 15 by pipe 115, and its thermal medium waste side links to each other with the first lower space part 15 by managing 116.The top of the second upper space part 21 links to each other with oxygen pipeline 117 through flue gas leading 118.The second lower space part 23 links to each other with super high pure oxygen carrier pipe 110.
In addition, the pipeline and the valve of first order rectifying column 6, second level rectifying column 7, nitrogen condenser 8, main heat exchanger 5 and connection each several part all are contained in the hot box 40.
To describe below and utilize this device to generate the method for nitrogen for ultra-high purity and nitrogen for ultra-high purity.
By after the dedusting of filter (not shown), be compressed to about 8.4kg/cm at raw air by compressor 1
2The pressure of G.In being filled with the carbon monoxide of oxidation catalyst/hydrogen converter 2, hydrogen, carbon monoxide and hydrocarbon contained in the raw air are oxidized continuously, be cooled by refrigerator 3 raw airs, from raw air, remove carbon dioxide and moisture content by carbon dioxide removal/drying device 4a or 4b then.Afterwards by in main heat exchanger 5, raw air being cooled to approximately-167 ℃ with the indirect heat exchange of refrigerant, by pipeline 105 raw air is offered by partial liquefaction along with raw air first order rectifying column 6 following rectifying part 14 below.On the other hand, will be used for the high-purity liquid nitrogen of withdrawing fluid (also can make low-temperature receiver) by the storage part 16 of high-purity liquid nitrogen supply pipe 100 above the system outside infeeds the last rectifying part 12 that is arranged in first order rectifying column 6.
Infeed liquid phase part in the raw air of first order rectifying column 6 and be collected at the bottom of the first lower space part 15, its gas phase part rises along first order rectifying column, promptly successively by down rectifying part 14, middle rectifying part 13 and last rectifying part 12, so as with the main withdrawing fluid counter current contacting of forming by liquid nitrogen from flowing down.Like this, the component that oxygen in the gas phase and boiling point are higher than oxygen boiling point (methane, nitrogen, xenon etc.) is dissolved in the withdrawing fluid, and nitrogen and the boiling point in the withdrawing fluid is evaporated out and enters gas phase than the low-boiling component of nitrogen (neon, hydrogen, helium etc.) simultaneously.The high pure nitrogen that the result contains the low boiling component is collected in the first upper space part 11, and the oxygen-rich liquid air that contains the higher boiling component is collected in the first lower space part 15.
The high pure nitrogen that contains the low boiling component that accumulates in the first upper space part 11 is admitted in the nitrogen condenser 8 by pipeline 106, so that it is cooled down by indirect heat exchange with refrigerant, and by manage 107 and high-purity liquid nitrogen supply pipe 100 high-purity liquid nitrogen that condensation like this is got off turn back in the storage part 16 above the rectifying part 12 as partial reflux liquid, the incoagulable gas that has gathered the low boiling component simultaneously is exhausted from system by pipeline 119.
The temperature that is collected at the first lower space part, 15 bottoms is that about-168 ℃ part oxygen-rich liquid air is introduced into first expansion valve 31 by pipeline 108, and the oxygen-rich liquid air is depressurized to about 3.2kg/cm in this valve
2G also is provided for nitrogen condenser 8 as refrigerant.By the 4th expansion valve 34, the oxygen of employed temperature about-175 ℃ is further depressurized to 0.3kg/cm
2G, and enter main heat exchanger 5 through oxygen pipe 117, oxygen cools off raw air as refrigerant in this heat exchanger.Further be exhausted from system behind the regeneration gas as carbon dioxide removal/drying device 4a or 4b at oxygen.
The high-purity liquid nitrogen of the high-purity liquid nitrogen of the top storage part 16 of rectifying part 12 and condensation in nitrogen condenser 8 and the uprising gas counter current contacting of mainly forming in the supply by nitrogen, so that they flow down through on obtain ultra-pure liquid nitrogen by the wherein remaining low boiling component of further release during rectifying part 12, and this ultra-pure liquid nitrogen be collected between last rectifying part 12 and middle rectifying part 13 in the storage part 17.Like this, a part of ultra-pure liquid nitrogen is extracted and is admitted to out the 3rd expansion valve 33 through nitrogen for ultra-high purity carrier pipe 109 from storage part 17, and remaining ultra-pure liquid nitrogen further flows through middle rectifying part 13 downwards as withdrawing fluid.The ultra-pure liquid nitrogen that enters the 3rd expansion valve 33 is depressurized, and is approximately 6.8kg/cm so that obtain pressure
2G, temperature are about ultra-pure nitrogen of-173 ℃, and this ultra-pure nitrogen is admitted to nitrogen condenser 8 as described a part of refrigerant.Go into main heat exchanger 5 by the nitrogen for ultra-high purity pneumatic transmission that pipeline 111 will take out from nitrogen condenser 8, ultra-pure here nitrogen is used as part refrigerant and cools off raw air, 113 it is offered the system outside as ultra-pure nitrogen product by the road then.
Part withdrawing fluid is collected in the following storage part 18 between middle rectifying part 13 and following rectifying part 14, these withdrawing fluids have become the liquid air of having removed the higher boiling component, and the rectifying part 14 of further flowing through down downwards is so that the higher boiling component in the absorption raw air, accumulate in then in the first lower space part 15, and another part of withdrawing fluid 114 is drawn out of and enters second expansion valve 32 by the road.This part withdrawing fluid that enters second expansion valve 32 is depressurized to about 0.3kg/cm
2The pressure of G and part evaporation are about-190 ℃ solution-airmixture so that obtain temperature, this solution-airmixture be provided to second level rectifying column 7 rectifying part 22 above.The gas phase of solution-airmixture partly is collected in the second upper space part 21, and liquid phase part is as the withdrawing fluid rectifying part 22 of flowing through downwards, so that by contact the concentration that discharges the low boiling component and improve oxygen with the back flow of gas that rises from below, this liquid phase part is collected in the second lower space part 23 then.In second lower space 23, be provided with a reboiler 24, here 115 raw airs of sending into from the first lower space part 15 heat the liquid that is collected at the second lower space part 23 as thermal source by the road, therefore the boiling point component (argon, carbon monoxide, nitrogen etc.) lower than oxygen boiling point selectively evaporated with oxygen, and the component of so evaporation rises by rectifying part 22.In addition, the raw air that has used as thermal source in reboiler 24 is condensed and turns back in the first lower space part 15 by pipeline 116.
At last, contain the nitrogen that its boiling point is lower than the component of oxygen boiling point and be collected in the second upper space part 21, ultra-pure liquid oxygen is collected in the second lower space part 23.The nitrogen that is collected in the second upper space part 21 joins from the top through flue gas leading 118 and oxygen pipe 117, enter main heat exchanger 5 as refrigerant then, be collected at ultra-pure liquid oxygen in the second lower space part 23 simultaneously and be used as a kind of product and be recovered through super high pure oxygen carrier pipe 110.
Fig. 2 shows the flow chart of another example of nitrogen for ultra-high purity based on the present invention, oxygen generator unit.In this figure, label 50 is represented an expansion turbine.In this example, the entrance side of expansion turbine 50 is linked to each other with oxygen exit portion on main heat exchanger 5 pipelines, partly link to each other with the refrigerant inlet of main heat exchanger 5 by the outlet side of pipeline 122 with expansion turbine 50 by pipeline 121.In addition, in this device, do not provide pipe (among Fig. 1, being equivalent to pipeline 100) and flue gas leading 118 to join with pipe 122 as the supply high-purity liquid nitrogen of low-temperature receiver (yet can be used as withdrawing fluid) from the system outside to first order rectifying column.In addition to these, the device of describing among the device in this example and Fig. 1 has identical structure.
Be collected at a part of oxygen-rich liquid air that its temperature in the first lower space part 15 is approximately-168 ℃ and be admitted to first expansion valve 31 through pipeline 108, the oxygen-rich liquid air is depressurized to 3.2kg/cm in this valve
2G, and then it is sent in the nitrogen condenser 8 as refrigerant.After will used oxygen with about-175 ℃ temperature by oxygen pipeline 117 sending into main heat exchanger 5 here, oxygen is discharged from the pipeline of main heat exchanger 5 also with temperature approximately-150 ℃ and 121 is entered expansion turbine 50 by the road.Make its pressure reduce to about 0.3kg/cm through expansion turbine 50
2G and its temperature are reduced to approximately, and-180 ℃ oxygen 122 enters main heat exchanger 5 so that be used for cooling off raw air once more by the road.Owing to be provided with expansion turbine 50, make to have device in the system and move necessary cold, and needn't provide high-purity liquid nitrogen to be used as low-temperature receiver (also making withdrawing fluid) from the system outside.
Fig. 3 shows the flow chart of the 3rd example of nitrogen for ultra-high purity based on the present invention, oxygen generator unit.In this example, the thermal medium supply side that is arranged on the reboiler 24 in the second lower space part 23 of second level rectifying column 7 131 links to each other with pipeline 106 by the road, described pipeline is given nitrogen condenser 8 with high pure nitrogen from the first upper space part 21 of first order rectifying column 6, and the thermal medium of reboiler 24 is discharged side and 132 linked to each other with high-purity liquid nitrogen feeding pipe 100 by the road.
The 131 a part of high pure nitrogens from 11 discharges of the first upper space part are used as the thermal source the reboiler 24 by the road, so that be cooled, and by pipeline 132 and high-purity liquid nitrogen supply pipe 100, so the high-purity liquid nitrogen that gets off of condensation is used as partial reflux liquid and turns back in the top storage part 16 of rectifying part 12.
Fig. 4 shows the flow chart of the 4th example of nitrogen for ultra-high purity based on the present invention, oxygen generator unit.In this example, the following storage part 18 between middle rectifying part 13 and following rectifying part 14 links to each other mutually by pipeline 141 with the first lower space part 15, and described pipeline 141 is provided with a flow control valve 60.
Send into the first lower space part 15 by directly leaning on flow control valve 60 from the partial reflux liquid of extracting out between middle rectifying part 13 and the following rectifying part 14, the adjustable throttle warp is the amount of the withdrawing fluid of rectifying part 14 down, and the result also can regulate the oxygen concentration in the liquid air that will enter second level rectifying column 7.
In the device based on the present invention, the inside rectifying of first order rectifying column partly is divided into three grades, and wherein ultra-pure liquid nitrogen is recovered between last rectifying part and middle rectifying part.The liquid air of removing the higher boiling component that between middle rectifying part and following rectifying part, reclaims by expansion valve decompression and the rectifying that supplies to second level rectifying column partly above, here it with by being positioned at the following reboiler vaporized gas counter current contacting of rectifying part, so low boiling component is by from wherein separating.Like this, below the rectifying part of second level rectifying column, reclaim ultra-pure liquid oxygen.Because above-mentioned structure can generate ultra-pure liquid nitrogen and ultra-pure liquid oxygen simultaneously by the simple mechanism that comprises two rectifying columns accordingly.
Brief Description Of Drawings:
Fig. 1 represents the nitrogen for ultra-high purity based on the present invention, an example of oxygen generator unit;
Fig. 2 represents the nitrogen for ultra-high purity based on the present invention, another example of oxygen generator unit;
Fig. 3 represents the nitrogen for ultra-high purity based on the present invention, the 3rd example of oxygen generator unit;
Fig. 4 represents the nitrogen for ultra-high purity based on the present invention, the 4th example of oxygen generator unit; And
Fig. 5 represents the nitrogen for ultra-high purity of prior art, an example of oxygengenerating plant.
The 1-compressor, 2-carbon monoxide/hydrogen converter, 3-refrigerator, 4a, 4b-carbon dioxide removal drier, 5-main heat exchanger, 6-first order rectifying column, 7-second level rectifying column, 8-nitrogen condenser, the 11-first upper space part, the last rectifying part of 12-, rectifying part in the middle of the 13-, rectifying part under the 14-, the 15-first lower space part, the 21-second upper space part, 22-rectifying part, the 23-second lower space part, 24-reboiler, 31-first expansion valve, 32-second expansion valve, 33-second expansion valve, 34-the 4th expansion valve, the 40-hot box, 50-expansion turbine, 60-flow control valve, the high purity nitrogen supply pipe of 100-, the 108-pipe, 109-nitrogen for ultra-high purity carrier pipe, 110-super high pure oxygen carrier pipe, 117-oxygen pipe, the 118-flue gas leading.
Claims (6)
1. a nitrogen for ultra-high purity, oxygen generator unit, it comprises:
By order from top to bottom have first upper space part, go up the rectifying part, middle rectifying part, the first order rectifying column of rectifying part and first lower space part down;
Second level rectifying column with second upper space part, rectifying part and second lower space part;
By indirectly cooling off the main heat exchanger of raw air with the refrigerant heat exchange, the air that this heat exchanger will so cool off deliver to described rectifying down partly below;
Be used for to described go up the rectifying part above provide high-purity liquid nitrogen to be used as withdrawing fluid the high-purity liquid nitrogen supply pipe;
Be used for cooling off the nitrogen condenser of the high pure nitrogen that is collected at first upper space part, this condenser with the high-purity liquid nitrogen of condensation like this deliver to rectifying partly above be used as a part of withdrawing fluid, and incoagulable gas is discharged system;
Be used for making first expansion valve of the oxygen-rich liquid air decompression that is collected at first lower space part, the oxygen that this valve will so generate is sent in the nitrogen condenser as refrigerant;
Be used for to make the oxygen that refrigerant discharges then at nitrogen condenser from condenser and send into the oxygen pipe that described main heat exchanger is made refrigerant;
Be used between last rectifying part and middle rectifying part, reclaiming the nitrogen for ultra-high purity carrier pipe that a part of withdrawing fluid is made ultra-pure liquid nitrogen;
Be used to make from second expansion valve of a part of withdrawing fluid decompression of sending between middle rectifying part and the following rectifying part, the rectifying that the solution-airmixture that this valve will so generate is delivered to second level rectifying column partly above;
What be arranged in second lower space part is used to heat the reboiler that the liquid that is collected at second lower space part makes its part evaporation;
Be used for to be collected at the flue gas leading that second upper space gas is partly discharged system; And
Be used for reclaiming the liquid that is collected at second lower space part and make the super high pure oxygen carrier pipe of ultra-pure liquid oxygen.
2. a nitrogen for ultra-high purity, oxygen generator unit, it comprises:
By order from top to bottom have first upper space part, go up the rectifying part, middle rectifying part, the first order rectifying column of rectifying part and first lower space part down;
Second level rectifying column with second upper space part, rectifying part and second lower space part;
By indirectly cooling off the main heat exchanger of raw air with the refrigerant heat exchange, the air that this heat exchanger will so cool off deliver to described rectifying down partly below;
Be used for cooling off the nitrogen condenser of the high pure nitrogen that is collected at first upper space part, this condenser with the high-purity liquid nitrogen of condensation like this deliver to rectifying partly above be used as withdrawing fluid, and incoagulable gas is discharged system;
Be used for making first expansion valve of the oxygen-rich liquid air decompression that is collected at first lower space part, the oxygen that this valve will so generate is sent in the nitrogen condenser as refrigerant;
Be used for making at nitrogen condenser and do oxygen decompression that refrigerant discharged by this condenser then so that the expansion turbine that its temperature is descended, this machine is sent into main heat exchanger as refrigerant with the oxygen that temperature has reduced;
Be used between last rectifying part and middle rectifying part, reclaiming the nitrogen for ultra-high purity carrier pipe that a part of withdrawal liquid is made ultra-pure liquid nitrogen;
Be used to make from second expansion valve of a part of withdrawing fluid decompression of sending between middle rectifying part and the following rectifying part, the rectifying that the solution-airmixture that this valve will so generate is delivered to second level rectifying column partly above;
What be arranged in second lower space part is used to heat the reboiler that the liquid that is collected at second lower space part makes its part evaporation;
Be used for to be collected at the gas discharge pipe that second upper space gas is partly discharged system; And
Be used for reclaiming a part of liquid that is collected at second lower space part and make the super high pure oxygen carrier pipe of ultra-pure liquid oxygen.
3. according to a kind of nitrogen for ultra-high purity, the oxygen generator unit of claim 1 or 2, it also comprises the 3rd expansion valve, wherein ultra-pure liquid nitrogen is admitted to described the 3rd expansion valve through described nitrogen for ultra-high purity carrier pipe, so that make ultra-pure liquid nitrogen decompression, and so the ultra-pure nitrogen that generates is admitted to nitrogen condenser as a part of refrigerant, and then offers the system outside as a kind of product.
4. according to a kind of nitrogen for ultra-high purity, the oxygen generator unit of claim 1 or 2, wherein said reboiler is used to cool off the part material air of partly introducing from described first lower space as thermal source, and chilled raw air like this is turned back to the described first lower space part.
5. according to a kind of nitrogen for ultra-high purity, the oxygen generator unit of claim 1 or 2, wherein said reboiler is used for cooling off the part high pure nitrogen of partly introducing from described first upper space as thermal source, and chilled high-purity liquid nitrogen like this is delivered to described the top as a part of withdrawing fluid of rectifying part of going up.
6. according to a kind of nitrogen for ultra-high purity, the oxygen generator unit of claim 1 or 2, it also comprises flow control valve, wherein a part of withdrawing fluid directly enters described first lower space part between rectifying part and the described part of rectifying down by described flow control valve in the middle of described, regulates the amount of the withdrawing fluid of the described part of rectifying down of flowing through thus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96118992 CN1154464A (en) | 1995-11-02 | 1996-11-01 | Ultra high purity nitrogen and oxygen generator unit |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP286134/95 | 1995-11-02 | ||
| CN 96118992 CN1154464A (en) | 1995-11-02 | 1996-11-01 | Ultra high purity nitrogen and oxygen generator unit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1154464A true CN1154464A (en) | 1997-07-16 |
Family
ID=5125466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96118992 Pending CN1154464A (en) | 1995-11-02 | 1996-11-01 | Ultra high purity nitrogen and oxygen generator unit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1154464A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886871A (en) * | 2010-08-04 | 2010-11-17 | 四川空分设备(集团)有限责任公司 | Method and device for producing pressure oxygen by air separation |
| CN101922848A (en) * | 2009-06-16 | 2010-12-22 | 普莱克斯技术有限公司 | Be used to produce the method and apparatus of pressurized product |
| CN102322726A (en) * | 2011-06-13 | 2012-01-18 | 开封空分集团有限公司 | Air separating device and method for alternatively producing nitrogen gas and liquid nitrogen |
| CN102320581A (en) * | 2011-08-30 | 2012-01-18 | 开封黄河空分集团有限公司 | A kind of nitrogen reparation technology |
| CN107560320A (en) * | 2017-10-18 | 2018-01-09 | 上海宝钢气体有限公司 | A kind of method and device for producing high pure oxygen and High Purity Nitrogen |
-
1996
- 1996-11-01 CN CN 96118992 patent/CN1154464A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101922848A (en) * | 2009-06-16 | 2010-12-22 | 普莱克斯技术有限公司 | Be used to produce the method and apparatus of pressurized product |
| CN101922848B (en) * | 2009-06-16 | 2015-03-18 | 普莱克斯技术有限公司 | Method and apparatus for pressurized product production |
| CN101886871A (en) * | 2010-08-04 | 2010-11-17 | 四川空分设备(集团)有限责任公司 | Method and device for producing pressure oxygen by air separation |
| CN101886871B (en) * | 2010-08-04 | 2012-08-08 | 四川空分设备(集团)有限责任公司 | Method and device for producing pressure oxygen by air separation |
| CN102322726A (en) * | 2011-06-13 | 2012-01-18 | 开封空分集团有限公司 | Air separating device and method for alternatively producing nitrogen gas and liquid nitrogen |
| CN102320581A (en) * | 2011-08-30 | 2012-01-18 | 开封黄河空分集团有限公司 | A kind of nitrogen reparation technology |
| CN107560320A (en) * | 2017-10-18 | 2018-01-09 | 上海宝钢气体有限公司 | A kind of method and device for producing high pure oxygen and High Purity Nitrogen |
| CN107560320B (en) * | 2017-10-18 | 2022-11-22 | 上海宝钢气体有限公司 | Method and device for producing high-purity oxygen and high-purity nitrogen |
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