CN101857201A - Device for producing high-purity oxygen and krypton-xenon concentrate and using method thereof - Google Patents
Device for producing high-purity oxygen and krypton-xenon concentrate and using method thereof Download PDFInfo
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Abstract
The invention relates to a device for producing high-purity oxygen and krypton-xenon concentrate from the liquid oxygen of a krypton and xenon-containing mixture and application thereof. The device comprises a first stage rectification tower and a second stage rectification tower, wherein a plurality of blocks of tower plates are arranged in the first stage rectification tower; a raw material inlet, namely a liquid oxygen inlet, is arranged on the side of the first stage rectification tower; a condensation evaporator is arranged at the top of the first stage rectification tower; a reboiler is arranged at the bottom of the first stage rectification tower; the middle part of the second stage rectification tower is connected with the upper part of the first stage rectification tower through a pipeline; a plurality of blocks of tower plates are arranged in the second stage rectification tower; a condensation evaporator is arranged at the top of the second stage rectification tower; and a reboiler is arranged at the bottom of the second stage rectification tower. High-purity gas oxygen (or liquid oxygen) is extracted from the plurality of blocks of tower plates or the tower on the lower part of the inlet in the second stage rectification tower; and the krypton and xenon-containing concentrate is obtained from the first stage rectification tower. Compared with the prior art, the device can reclaim the krypton and xenon-containing mixture and the high-purity oxygen at the same time, has a high pure oxygen recovery rate and wide application range and can operate alone without being connected with an air separation device.
Description
Technical field
The present invention relates to the method and apparatus of a kind of production high purity oxygen and krypton-xenon concentrate, especially relate to a kind of device and using method thereof of from the liquid oxygen product, extracting krypton-xenon concentrate and high purity oxygen simultaneously.
Background technology
It serves as general that technical process is produced high purity oxygen with cryogenic rectification method, stock liquid is mainly two kinds of the gentle oxygen of liquid oxygen, difference according to stock liquid, extract high purity oxygen technology in the liquid oxygen, mainly be to extract liquid oxygen (99.5～99.7%) from the master is cold, all the other are that nitrogen, argon, krypton, xenon and hydrocarbon polymer etc. enter in the high-purity oxygen column, carry out rectifying in the mode that refluxes, the high purity oxygen purity of producing is 99.995%, and the amount of producing of this method high purity oxygen is less.
Another kind of mode is to choose the raw material that the crude argon column phegma is made high-purity liquid oxygen, and about 5 blocks of column plates extract content 93.17%O from the argon column bottom
2, 6.8%Ar, 0.013%N
2Unstripped gas, send into the pure oxygen tower and carry out rectifying, through about 50 blocks of column plates, the about 20Nm of tower still output
3The purity of/h is 99.9995% high purity oxygen.This method raw material liquid oxygen is not to get from main cold-draw, but chooses the crude argon column phegma as raw material, and its extraction yield only has an appointment 1.43%.
Along with the continuous development of electronic industrial technology, the demand of high purity oxygen is increased day by day.At present generally adopting liquid oxygen is that raw material carries out producing of high purity oxygen, and extraction yield is lower.And in krypton xenon raw process flow process, through once, oxygen after secondarily purified, purity reaches 99.5%～99.99%, produces the splendid raw material of high purity oxygen, is characterized in that output is big, purity is high.And such unstripped gas generally take emptying or with other gas blended modes, regulate the condensation evaporation actuator temperature, fail to make full use of existing resource, realize recycling economy.
Summary of the invention
Purpose of the present invention is exactly a kind of rate of recovery height of high purity oxygen is provided in order to overcome the defective that above-mentioned prior art exists, produces the device and the using method thereof of krypton xenon mixture and high purity oxygen, widely used production high purity oxygen and krypton-xenon concentrate simultaneously.
Purpose of the present invention can be achieved through the following technical solutions:
The device of a kind of production high purity oxygen and krypton-xenon concentrate, it is characterized in that, this device comprises first step rectifying tower and second stage rectifying tower, in the described first step rectifying tower several piece column plate is set, on the pipeline of this first step rectifying Tata side material inlet is set, cat head is provided with condenser/evaporator, the tower still is provided with reboiler, the top of rectifying tower middle part, the described second stage and first step rectifying tower is through pipe connection, in this second stage rectifying tower the several piece column plate is set, cat head is provided with condenser/evaporator, the tower still is provided with reboiler, the tower side is provided with high-purity gas/liquid oxygen and takes out mouth, and the reboiler of described first step rectifying Tata still is connected with the condenser/evaporator of pipeline with first step rectifying tower and second stage rectifying tower cat head through throttling valve.
Described material inlet is located at apart from the height of at least one block of column plate of first step rectifying Tata still.
Stage number in the described first step rectifying tower is 8～20, and the stage number in the rectifying tower of the second stage is 40～100, preferred 68.
Described reboiler is the interchanger of electric heater or gas evaporation tower bottoms body.
Described high-purity gas/liquid oxygen is taken out and mouthful is located at apart from the height of 2～10 blocks of column plates of second stage rectifying Tata still, preferably apart from the height of 5 blocks of column plates of tower still.
Described high-purity gas/liquid oxygen is taken out mouth and is located at second stage rectifying Tata still.
The using method of a kind of production high purity oxygen and krypton-xenon concentrate device is characterized in that, this method may further comprise the steps:
(1) raw material is directed into through material inlet carries out rectification process in the first step rectifying tower, the temperature of control first step rectifying tower is-126～-164 ℃, pressure is 1.5～3bar, obtains krypton-xenon concentrate at the tower still, obtains removing the oxygen or the liquid oxygen of krypton, xenon and hydrocarbon polymer at cat head;
(2) oxygen that obtains of cat head or liquid oxygen enter second stage rectifying tower and continue rectifying, and the temperature of control second stage rectifying tower be-170～-175 ℃, and pressure is 2～5bar, takes out mouth at high-purity gas/liquid oxygen and obtains high-purity liquid oxygen or high-purity gas oxygen, and cat head obtains the oxygen argon mixture;
(3) nitrogen enters first step rectifying Tata still reboiler and is liquefied as liquid nitrogen, liquid nitrogen enters the overhead condensation vaporizer of first step rectifying tower and second stage rectifying tower through throttling valve throttling to low pressure, flash to gas nitrogen, the liquid nitrogen that is not evaporated is exported from first step rectifying tower as liquid nitrogen product.
Described raw material comprises the raw material liquid oxygen that contains krypton xenon mixture or contains krypton xenon mixture and be chilled to low wet oxygen near state of saturation in advance through interchanger, and described raw material liquid oxygen is for the industrial liquid oxygen that connects air separation plant or through concentrating and remove the liquid oxygen of high boiling point component such as methane.
Krypton xenon content is 3～20 times of krypton xenon content in the raw material in the described krypton-xenon concentrate, preferred 10 times.
Oxygen purity reaches 99.99v/v%-99.9997v/v% in described high-purity liquid oxygen or the high-purity gas oxygen.
Compared with prior art, the present invention has the following advantages:
Reclaim when (1) can realize krypton xenon mixture and high purity oxygen, wherein the rate of recovery height of high purity oxygen can reach more than 90%;
(2) high purity oxygen product gas is various informative, and the gas products of production can be a gas, also can produce liquid product and enter the liquid storage groove storage;
(3) two rectifying tower are set, can produce krypton-xenon concentrate and high purity oxygen product simultaneously.By rectifying step by step, poor krypton-xenon liquid that first step rectifier bottoms is produced or thick krypton-xenon liquid have removed high boiling component (Kr, Xe, C in the unstripped gas
1～C
3, CF
4, C
2F
6, SF
6Deng), only contain micro-Ar and N in the oxygen of tower top discharge
2, finally obtaining purity and be higher than 99.999% high purity oxygen product, wherein various foreign matter contents all are lower than the technical indicator of GB/T14599-2008 high purity oxygen;
(4) applied range, after the user was provided with liquid oxygen, liquid nitrogen cryogenics storage tank, apparatus of the present invention can break away from air separation plant, independent operating.
Description of drawings
Fig. 1 is a structural representation of the present invention among the embodiment 1;
Fig. 2 is a structural representation of the present invention among the embodiment 2;
Fig. 3 is a structural representation of the present invention among the embodiment 3;
Fig. 4 is a structural representation of the present invention among the embodiment 4.
Among the figure, 1 is that first step rectifying tower, 2 is that second stage rectifying tower, 3 is that raw material, 4 is that low temperature nitrogen, 5 is that liquid nitrogen, 6 is that throttling valve, 7 is that liquid nitrogen, 8 is that oxygen, 9 is that nitrogen, 10 is that liquid nitrogen, 13 is that liquid nitrogen, 14 is that nitrogen, 15 is that high-purity liquid oxygen, 16 is that liquid oxygen, 17 is that oxygen argon mixture, 18 is that reboiler, 19 is that krypton-xenon concentrate, 20 is that condenser/evaporator, 21 is that reboiler, 22 is a condenser/evaporator.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1
The device of a kind of production high purity oxygen and krypton-xenon concentrate, its structure as shown in Figure 1, stock liquid oxygen product 3 is with 1000Nm
3/ h sends among the first step rectifying tower 1, and working pressure is provided with 10 blocks of column plates at 2bar in the tower, obtains 200Nm at the bottom of the tower
3/ h poor krypton-xenon liquid, the first washing of high boiling point components such as krypton, xenon, methane enters in the poor krypton-xenon liquid, the about 600ppm of krypton xenon wherein, the about 200ppm of methane, the about 20ppm of all the other foreign matter contents, contain high boiling point components such as krypton xenon in the oxygen 8 of top discharging hardly, bottom stream obtains poor krypton-xenon liquid, enters rectifying once more in the second stage rectifying tower 2.Poor krypton xenon tower bottom fluid adopts the nitrogen heating, temperature is reduced to the fluid nitrogen 4 of saturation point, through being separated into gas-liquid two-phase after reboiler 21 and the throttling valve 6, obtain liquid nitrogen 5, liquid nitrogen 7 and liquid nitrogen 13 enter respectively in the condenser/ evaporator 20 and 22 of two cats head as low-temperature receiver, and unnecessary liquid nitrogen is discharged by pipeline and entered storage tank, and liquid nitrogen vaporization is condensed into the oxygen of rising to carry out rectifying in the liquid oxygen reflux tower, liquid nitrogen is evaporated nitrogen 9 and the nitrogen 14 that obtains, and obtains krypton-xenon concentrate 19 at the tower still.
Oxygen streamline 8 enters the position, middle and upper part of second stage rectifying tower 2, apart from 6 column plate positions of condenser/evaporator, rectifying tower 2 bottom reboiler 18 in the second stage adopt electric heater, produce the required rising oxygen of rectifying, low-temperature receiver adopts through the liquid nitrogen 13 after the throttling valve 6, and the oxygen that cooling is risen produces the backflow liquid oxygen and sets up the rectifying operating mode.Second stage rectifying tower 2 working pressure 3bar, 68 blocks of column plates are set, high purity oxygen (liquid oxygen) is taken out mouth and is positioned at apart from 5 positions of tower still, obtain purity greater than high-purity liquid oxygen 15 of 99.999%, wherein the volume content of argon is less than 2ppm, total hydrocarbon content is less than 0.5ppm, and the liquid oxygen 16 that contains high boiling point impurity such as krypton xenon, methane is discharged in the bottom, and cat head obtains oxygen argon mixture 17.
Embodiment 2
The device of a kind of production high purity oxygen and krypton-xenon concentrate, its structure as shown in Figure 2, with the difference of embodiment 1 be to enter the oxygen streamline 8 of second stage rectifying tower 2 to be the liquid oxygen of first step rectifying tower 1 top condenser/evaporator condensation.
Embodiment 3
The device of a kind of production high purity oxygen and krypton-xenon concentrate, its structure as shown in Figure 3, with the difference of embodiment 1 be that to enter the tower still reboiler of first step rectifying tower 1 be electric heater, the liquid nitrogen 13 that enters the condenser/evaporator 22 of the liquid nitrogen 7 of condenser/evaporator 20 of first step rectifying tower 1 and second stage rectifying tower 2 provides for outside liquid nitrogen 5, rather than the liquid nitrogen of the tower still reboiler condensation of embodiment 1 first step rectifying tower 1.
Embodiment 4
The device of a kind of production high purity oxygen and krypton-xenon concentrate, its structure as shown in Figure 4, with the difference of embodiment 3 be to enter the oxygen streamline 8 of second stage rectifying tower 2 to be the liquid oxygen of first step rectifying tower 1 top condenser/evaporator condensation.
The device of a kind of production high purity oxygen and krypton-xenon concentrate, this device comprises first step rectifying tower and second stage rectifying tower, first step rectifying tower in 8 blocks of column plates are set, on the pipeline of this first step rectifying Tata side material inlet is set, material inlet is located at apart from the height of a column plate of first step rectifying Tata still, cat head is provided with condenser/evaporator, the tower still is provided with the interchanger of gas evaporation tower bottoms body, the top of rectifying tower middle part, the second stage and first step rectifying tower is through pipe connection, 40 blocks of column plates are set in this second stage rectifying tower, cat head is provided with condenser/evaporator, the tower still is provided with the interchanger of gas evaporation tower bottoms body, the tower side is provided with high-purity gas/liquid oxygen and takes out mouth, high-purity gas/liquid oxygen is taken out mouth and is located at apart from the height of 2 blocks of column plates of second stage rectifying Tata still, and the reboiler of first step rectifying Tata still is connected with the condenser/evaporator of pipeline with first step rectifying tower and second stage rectifying tower cat head through throttling valve.
The using method of production high purity oxygen and krypton-xenon concentrate device may further comprise the steps:
(1) liquid oxygen that will concentrate and remove high boiling point components such as methane and contain krypton xenon mixture is directed into through opening for feed and carries out rectification process in the first step rectifying tower, the temperature of control first step rectifying tower is-126 ℃, pressure is 1.5bar, obtain krypton-xenon concentrate at the tower still, krypton xenon content is 10 times of krypton xenon content in the raw material in the krypton-xenon concentrate, obtains removing the oxygen of krypton, xenon and hydrocarbon polymer at cat head;
(2) oxygen that obtains of cat head enters second stage rectifying tower and continues rectifying, the temperature of control second stage rectifying tower is-170 ℃, and pressure is 2bar, takes out mouth at high-purity gas/liquid oxygen and obtains high-purity liquid oxygen, oxygen purity reaches 99.99v/v% in high-purity liquid oxygen or the high-purity gas oxygen, and cat head obtains the oxygen argon mixture.
(3) nitrogen enters first step rectifying Tata still reboiler and is liquefied as liquid nitrogen, liquid nitrogen enters the overhead condensation vaporizer of first step rectifying tower and second stage rectifying tower through throttling valve throttling to low pressure, flash to gas nitrogen, the liquid nitrogen that is not evaporated is exported from first step rectifying tower as liquid nitrogen product.
Embodiment 6
The device of a kind of production high purity oxygen and krypton-xenon concentrate, this device comprises first step rectifying tower and second stage rectifying tower, 20 blocks of column plates are set in the described first step rectifying tower, on the pipeline of this first step rectifying Tata side material inlet is set, material inlet is located at apart from the height of 5 blocks of column plates of first step rectifying Tata still.Cat head is provided with condenser/evaporator, the tower still is provided with reboiler, the top of rectifying tower middle part, the second stage and first step rectifying tower is through pipe connection, 100 blocks of column plates are set in this second stage rectifying tower, cat head is provided with condenser/evaporator, the tower still is provided with reboiler, and the tower still is provided with high-purity gas/liquid oxygen and takes out mouth, and the reboiler of first step rectifying Tata still is connected with the condenser/evaporator of pipeline with first step rectifying tower and second stage rectifying tower cat head through throttling valve.
The using method of production high purity oxygen and krypton-xenon concentrate device may further comprise the steps:
(1) liquid oxygen that will concentrate and remove high boiling point components such as methane and contain krypton xenon mixture is directed into through opening for feed and carries out rectification process in the first step rectifying tower, the temperature of control first step rectifying tower is-164 ℃, pressure is 3bar, obtain krypton-xenon concentrate at the tower still, krypton xenon content is 3 times of krypton xenon content in the raw material in the krypton-xenon concentrate, obtains removing the liquid oxygen of krypton, xenon and hydrocarbon polymer at cat head;
(2) liquid oxygen that obtains of cat head enters second stage rectifying tower and continues rectifying, the temperature of control second stage rectifying tower is-175 ℃, and pressure is 5bar, takes out mouth at high-purity gas/liquid oxygen of tower still and obtains high-purity gas oxygen, oxygen purity reaches 99.9997v/v% in high-purity gas oxygen, and cat head obtains the oxygen argon mixture;
(3) nitrogen enters first step rectifying Tata still reboiler and is liquefied as liquid nitrogen, liquid nitrogen enters the overhead condensation vaporizer of first step rectifying tower and second stage rectifying tower through throttling valve throttling to low pressure, flash to gas nitrogen, the liquid nitrogen that is not evaporated is exported from first step rectifying tower as liquid nitrogen product.
Claims (10)
1. device of producing high purity oxygen and krypton-xenon concentrate, it is characterized in that, this device comprises first step rectifying tower and second stage rectifying tower, in the described first step rectifying tower several piece column plate is set, on the pipeline of this first step rectifying Tata side material inlet is set, cat head is provided with condenser/evaporator, the tower still is provided with reboiler, the top of rectifying tower middle part, the described second stage and first step rectifying tower is through pipe connection, in this second stage rectifying tower the several piece column plate is set, cat head is provided with condenser/evaporator, the tower still is provided with reboiler, the tower side is provided with high-purity gas/liquid oxygen and takes out mouth, and the reboiler of described first step rectifying Tata still is connected with the condenser/evaporator of pipeline with first step rectifying tower and second stage rectifying tower cat head through throttling valve.
2. the device of a kind of production high purity oxygen according to claim 1 and krypton-xenon concentrate is characterized in that, described material inlet is located at apart from the height of at least one block of column plate of first step rectifying Tata still.
3. the device of a kind of production high purity oxygen according to claim 1 and krypton-xenon concentrate is characterized in that, the stage number in the described first step rectifying tower is 8～20, and the stage number in the rectifying tower of the second stage is 40～100, preferred 68.
4. the device of a kind of production high purity oxygen according to claim 1 and krypton-xenon concentrate is characterized in that, described reboiler is the interchanger of electric heater or gas evaporation tower bottoms body.
5. the device of a kind of production high purity oxygen according to claim 1 and krypton-xenon concentrate is characterized in that, described high-purity gas/liquid oxygen is taken out and mouthful is located at apart from the height of 2～10 blocks of column plates of second stage rectifying Tata still, preferably apart from the height of 5 blocks of column plates of tower still.
6. the device of a kind of production high purity oxygen according to claim 1 and krypton-xenon concentrate is characterized in that, described high-purity gas/liquid oxygen is taken out mouth and is located at second stage rectifying Tata still.
7. using method of producing high purity oxygen and krypton-xenon concentrate device is characterized in that this method may further comprise the steps:
(1) raw material is directed into through material inlet carries out rectification process in the first step rectifying tower, the temperature of control first step rectifying tower is-126～-164 ℃, pressure is 1.5～3bar, obtains krypton-xenon concentrate at the tower still, obtains removing the oxygen or the liquid oxygen of krypton, xenon and hydrocarbon polymer at cat head;
(2) oxygen that obtains of cat head or liquid oxygen enter second stage rectifying tower and continue rectifying, and the temperature of control second stage rectifying tower be-170～-175 ℃, and pressure is 2～5bar, takes out mouth at high-purity gas/liquid oxygen and obtains high-purity liquid oxygen or high-purity gas oxygen, and cat head obtains the oxygen argon mixture;
(3) nitrogen enters first step rectifying Tata still reboiler and is liquefied as liquid nitrogen, liquid nitrogen enters the overhead condensation vaporizer of first step rectifying tower and second stage rectifying tower through throttling valve throttling to low pressure, flash to gas nitrogen, the liquid nitrogen that is not evaporated is exported from first step rectifying tower as liquid nitrogen product.
8. the using method of a kind of production high purity oxygen according to claim 7 and krypton-xenon concentrate device, it is characterized in that, described raw material comprises the raw material liquid oxygen that contains krypton xenon mixture or contains krypton xenon mixture and be chilled to low wet oxygen near state of saturation in advance through interchanger, and described raw material liquid oxygen is for the industrial liquid oxygen that connects air separation plant or through concentrating and remove the liquid oxygen of high boiling point component such as methane.
9. the using method of production high purity oxygen according to claim 7 and krypton-xenon concentrate device is characterized in that, krypton xenon content is 3～20 times of krypton xenon content in the raw material in the described krypton-xenon concentrate, preferred 10 times.
10. the using method of a kind of production high purity oxygen according to claim 7 and krypton-xenon concentrate device is characterized in that, oxygen purity reaches 99.99v/v%-99.9997v/v% in described high-purity liquid oxygen or the high-purity gas oxygen.
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Cited By (7)
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| CN103215066A (en) * | 2012-12-12 | 2013-07-24 | 滁州市润达溶剂有限公司 | Distillation separation device and method for liquid hydrocarbon mixture |
| CN105107218A (en) * | 2015-07-24 | 2015-12-02 | 包头轻工职业技术学院 | Continuous distillation device |
| CN106679333A (en) * | 2016-12-30 | 2017-05-17 | 清远市联升空气液化有限公司 | High-purity oxygen preparation device and method for preparing high-purity oxygen through same |
| CN107684828A (en) * | 2017-10-20 | 2018-02-13 | 江苏华益科技有限公司 | A kind of rectifier unit of high pure oxygen 16 |
| CN108362074A (en) * | 2018-03-26 | 2018-08-03 | 四川空分设备(集团)有限责任公司 | A kind of method and apparatus for extracting krypton and xenon from Extra large air separation plant |
| CN112432429A (en) * | 2020-11-02 | 2021-03-02 | 杭州制氧机集团股份有限公司 | Device and method for extracting krypton and xenon in liquid oxygen through low-temperature rectification |
| CN115854653A (en) * | 2023-02-27 | 2023-03-28 | 河南心连心深冷能源股份有限公司 | Device and process for producing poor krypton-xenon and ultra-pure oxygen by adopting same heat pump |
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| CN108362074A (en) * | 2018-03-26 | 2018-08-03 | 四川空分设备(集团)有限责任公司 | A kind of method and apparatus for extracting krypton and xenon from Extra large air separation plant |
| CN108362074B (en) * | 2018-03-26 | 2023-11-24 | 四川空分设备(集团)有限责任公司 | Method and device for extracting krypton and xenon from oversized air separation equipment |
| CN112432429A (en) * | 2020-11-02 | 2021-03-02 | 杭州制氧机集团股份有限公司 | Device and method for extracting krypton and xenon in liquid oxygen through low-temperature rectification |
| CN112432429B (en) * | 2020-11-02 | 2024-02-20 | 杭氧集团股份有限公司 | Device and method for extracting krypton and xenon in liquid oxygen through low-temperature rectification |
| CN115854653A (en) * | 2023-02-27 | 2023-03-28 | 河南心连心深冷能源股份有限公司 | Device and process for producing poor krypton-xenon and ultra-pure oxygen by adopting same heat pump |
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Application publication date: 20101013 |