CN104406364A - Double-tower coupling type argon recovery and purifying equipment and argon recovery and purifying method - Google Patents
Double-tower coupling type argon recovery and purifying equipment and argon recovery and purifying method Download PDFInfo
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- CN104406364A CN104406364A CN201410618341.5A CN201410618341A CN104406364A CN 104406364 A CN104406364 A CN 104406364A CN 201410618341 A CN201410618341 A CN 201410618341A CN 104406364 A CN104406364 A CN 104406364A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/044—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a single pressure main column system only
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
- F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
- F25J3/04096—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of argon or argon enriched stream
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
- F25J3/0426—The cryogenic component does not participate in the fractionation
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
- F25J3/04951—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network
- F25J3/04963—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/58—Argon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/58—Argon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2260/00—Coupling of processes or apparatus to other units; Integrated schemes
- F25J2260/58—Integration in an installation using argon
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention relates to double-tower coupling type argon recovery and purifying equipment and an argon recovery and purifying method. The argon recovery and purifying equipment mainly comprises a cooling box, a main heat exchanger, a low-temperature rectifying tower and a liquid nitrogen pump, wherein at least the main heat exchanger and the low-temperature rectifying tower are arranged in the cooling box, the low-temperature rectifying tower is of a double-tower coupling structure which consists of an upper tower and a lower tower, the upper tower is an argon tower, the lower tower is a nitrogen tower, and a condenser is arranged at the top part of the argon tower. The method comprises the followings steps of sending crude argon into the cooling box to be cooled and liquefied by the main heat exchanger, throttling, then sending the crude argon into the argon tower of the low-temperature rectifying tower of the argon tower and nitrogen tower type double-tower coupling structure, enabling the argon, nitrogen and hydrogen in the argon tower to generate rectifying separation, obtaining pure liquid argon at the bottom part of the argon tower, boosting the pure liquid nitrogen by a liquid nitrogen pump, and reheating the pure liquid nitrogen by the main heat exchanger, so as to obtain a pure argon product. The equipment and the method have the characteristics that the recovery rate of the argon is high, the purity of the recovered argon is high, the content of impurity oxygen is low, the energy consumption of recovery purification is low, a nitrogen byproduct and an oxygen-rich air byproduct are obtained, and the like.
Description
Technical field
What the present invention relates to is that a kind of argon gas being mainly used in the double tower coupling of argon gas recovery purifying in monocrystalline silicon production reclaims purifier apparatus and argon gas reclaims purification process.
Background technology
Vertical pulling method (Czochralski method) is the main method of manufacture order crystal silicon, and the monocrystalline silicon in the whole world 70% ~ 80% is produced by vertical pulling method.The most frequently used vertical pulling method produce single crystal silicon technology adopts not only picture vacuum technology but also the decompression crystal pulling technique as flowing atmosphere technique; Decompression technique is in silicon single crystal pulling process, continuous constant speed ground passes into high purity argon in single crystal growing furnace burner hearth, vavuum pump is constantly from the outside pump Argon of burner hearth simultaneously, vacustat in burner hearth is kept to hold in the palm left and right 20, the feature of the existing vacuum technology of this technique, has again the feature of flowing atmosphere technique.The vavuum pump of decompression crystal pulling technique generally adopts slide valve pump, and slide valve pump is the oil-sealed rotary pump keeping sealing with oil.Argon gas carries the Si oxide and impurity volatile matter that produce due to high temperature in crystal-pulling process, and is discharged into air by pumping of vavuum pump.
By the analysis to discharge argon gas, major impurity composition is, the alkane such as oxygen, nitrogen, carbon monoxide, carbon dioxide, methane, liquid lubricant mist; Recycle this part argon gas and have very large realistic meaning.
Argon gas reclaims the known technology of purifying: carry out thick oil removing to the argon gas reclaimed from single crystal growing furnace, then high accuracy oil removing dedusting after compressed cooling; Then made by high-temperature catalytic the hydro carbons such as methane and carbon monoxide produce water and carbon dioxide with oxygen reaction, in catalytic reaction, ensure oxygen excessive (impurity oxygen not then adds oxygen); By making excessive oxygen generate water with the hydrogen reaction added after cooling under catalyst action, and ensure that reaction hydrogen is excessive, after process, in argon gas, impurity component is water, carbon dioxide, hydrogen and nitrogen; Eventually pass argon gas normal temperature absorbing unit adsorbed water and carbon dioxide, obtain being only the crude argon of impurity containing nitrogen and hydrogen.Argon gas normal temperature absorbing unit is made up of two absorbers, and the adsorbent of adsorbed water and carbon dioxide is housed in absorber, and an absorber carries out absorption work, and another absorber carries out comprising pressure release, heats, the reproduction operation of blast-cold.The gas of described reproduction operation uses nitrogen, and this regeneration nitrogen is produced or outsourcing from low-temperature fractionating tower in ice chest, and argon gas normal temperature absorbing unit is switched by program timer auto-controll operation.
Summary of the invention
The object of the present invention is to provide a kind of argon gas rate of recovery high, recovery purity of argon is high, oxygen content is low, recovery purifying energy consumption is low, is particularly suitable for large-scale monocrystalline silicon production enterprise and carries out argon gas recovery purifier apparatus and the argon gas recovery purification process that a large amount of argon gas reclaims the double tower coupling of purifying recycling.
Object of the present invention has been come by following technical solution, a kind of argon gas of double tower coupling reclaims purifier apparatus, this equipment mainly comprises an ice chest, one main heat exchanger, low-temperature fractionating tower and liquid argon pump, in described ice chest, main heat exchanger and low-temperature fractionating tower are at least installed, described low-temperature fractionating tower is the double tower coupled structure be made up of Shang Ta and lower tower, wherein goes up that tower is argon column, lower tower is nitrogen tower, is middlely coupled by condenser/evaporator; The top of described argon column arranges condenser, and described argon column is a upper rectifying column that the crude argon rectifying entering this tower can be separated into liquid argon and rectifying waste gas; And described nitrogen tower is one air separation can be gone out nitrogen and make a part of nitrogen as byproduct, another part is used for the lower rectifying column of argon gas normal temperature absorbing unit regeneration.
Condenser/evaporator between argon column of the present invention and nitrogen tower is coupled to form by as the evaporimeter bottom argon column with as the condenser of nitrogen top of tower, thermal source is wherein the source nitrogen from nitrogen tower, low-temperature receiver is the liquid argon source from argon column, and source nitrogen is in intermediate condensation, and liquid argon evaporates in outside; The thermal source of the condenser that described argon column top is arranged is the upflowing vapor from argon column, and low-temperature receiver is the throttling oxygen-enriched liquid air from nitrogen tower bottom, and wherein upflowing vapor is in the intermediate condensation of condenser, and throttling oxygen-enriched liquid air evaporates in the outside of condenser; Described liquid argon pump is also installed in ice chest, and the liquid argon products export bottom described argon column connects described liquid argon pump and carries out supercharging, and by the main heat exchanger re-heat in ice chest to normal temperature access user argon gas pipe network.
At least be provided with in main heat exchanger of the present invention:
One crude argon cooling liquid passage, the import of this passage connects the crude argon inlet pipe entering ice chest, and outlet connection one choke valve accesses argon column again;
One pressure-air cooling passage, the import of this passage connects the compressed air inlet pipe entering ice chest, outlet access nitrogen tower;
One nitrogen re-heat passage, the import connection of this passage and the nitrogen outlet of nitrogen top of tower, the outlet of passage picks out ice chest by nitrogen tube;
An oxygen enrichment re-heat passage, the import of this passage is communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top respectively, and the outlet of passage picks out ice chest by oxygen enrichment tube connector; Or have two oxygen enrichment re-heat passages, the import of these two passages is communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top respectively, and the outlet of two passages picks out ice chest respectively by oxygen enrichment tube connector.
The argon gas utilizing above-mentioned double tower to be coupled reclaims purifier apparatus and carries out the method that argon gas reclaims purifying, and the method that described argon gas reclaims purifying comprises:
A) cooling of crude argon, first adopt known technology to produce only containing the crude argon of nitrogen hydrogen, crude argon 101 enters ice chest B1, then to enter main heat exchanger E1 cooling liquid be liquid argon 102; Liquid argon 102 enters argon column T1 and carries out rectifying separation after choke valve 103 throttling;
B) crude argon rectifying, crude argon carries out rectifying separation according to the characteristic that component boiling point is different in argon column T1, obtains liquid argon product 106 bottom argon column T1, discharges rectifying waste gas 112 at argon column T1 top; The condenser E3 condensation upflowing vapor 104 at argon column T1 top, the liquid 111 of condensation is as the phegma of argon column T1, and not solidifying gas is rectifying waste gas 112, and this rectifying waste gas 112 is extracted out from condenser E3 condensation side; Phegma 111 and the liquid that obtains through choke valve 103 throttling liquid argon 102 to decline liquid as rectifying, decline liquid carries out heat and mass with the upflowing vapor counter current contacting of evaporating from condenser/evaporator E2 bottom argon column T1, thus under flow to bottom argon column T1 and obtain liquid argon, upflowing vapor rises and to converge and gas that choke valve 103 throttling liquid argon 102 of hanging oneself obtains finally becomes upflowing vapor 104 at the bottom of tower; Bottom argon column T1, a part for liquid argon is discharged as product liquid argon 106, and another part is condensed evaporimeter E2 evaporation as upflowing vapor;
C) the producing of argon gas product, product liquid argon 106 is pressurized to the liquid argon 108 of user's argon gas ductwork pressure through liquid argon pump 107, and liquid argon 108 enters main heat exchanger E1 re-heat to be become the real argon gas 109 reclaiming purifying to normal temperature and enter user's argon gas pipe network; In product liquid argon 106, oxygen content general control is at below 2PPm, and the mole of product liquid argon 106 can reach more than 92% of argon mole in crude argon 101.
Method of the present invention also comprises:
D is through the compressed air 121 of impurity such as removing moisture content and carbon dioxide etc., enter ice chest B1, enter main heat exchanger E1 cooling again and become Cryogenic air 122, Cryogenic air 122 can be that gas also can contain a small amount of liquid entirely, Cryogenic air 122 enters low-temperature fractionating tower nitrogen tower T2, wherein gas fraction is as the upflowing vapor of nitrogen tower T2, and liquid part flows to the tower reactor at the bottom of tower; Upflowing vapor is with carrying out heat and mass from the phegma counter current contacting under overhead streams, obtain nitrogen 123 at nitrogen tower T2 top and enter condenser/evaporator E2 nitrogen 124, nitrogen 124 is condensed into liquid part as nitrogen tower liquid nitrogen reflux liquid 126 in condenser/evaporator E2, solidifying portion gas is that fixed gas 127 is extracted condenser/evaporator E2 out and discharged, and the discharge capacity of fixed gas 127 is generally less than 1% of compressed air 121; Liquid nitrogen reflux liquid 126 in nitrogen tower T2 to dirty, through flow to the heat and mass of upflowing vapor in the tower reactor at the bottom of nitrogen tower T2 tower with Cryogenic air 122 in flow to tower reactor liquid joint become oxygen-enriched liquid air 128 and extract out.
Nitrogen 123 of the present invention obtains byproduct nitrogen 125 through main heat exchanger E1 re-heat to normal temperature, and this nitrogen 125 part is as the regeneration nitrogen of argon gas normal temperature absorbing unit, and all the other can be used as plant protection gas and use;
Described oxygen-enriched liquid air 128 enters argon column condenser E3 after choke valve 129, as the upflowing vapor 104 of low-temperature receiver condensation from argon column T1 in condenser E3, self overwhelming majority is vaporizated into oxygen-rich steam 130, does not have evaporation section to discharge as oxygen-enriched liquid air 131 bottom condenser E3; The discharge effect of oxygen-enriched liquid air 131 is a small amount of CH preventing from containing in oxygen-enriched liquid air 128
4gathering at condenser E3 with heavy components such as nitrous oxides thus cause dangerous hidden danger, the discharge capacity of oxygen-enriched liquid air 131 is generally about 1% ~ 3% of oxygen-enriched liquid air 128 total amount; Converge after described oxygen-enriched liquid air 131 and oxygen-rich steam 130 go out condenser E3 and enter main heat exchanger E1 re-heat and become normal temperature oxygen-enriched air 133 to normal temperature; Or oxygen-enriched liquid air 131 and oxygen-rich steam 130 enter main heat exchanger E1 respectively, go out main heat exchanger E1 respectively; Oxygen-enriched air 133, as the regeneration gas of air normal temperature absorbing unit, also can be used for the place needing oxygen-enriched combusting.
The fresh liquid argon 105 of supplementary rectifying institute chilling requirement directly can be passed into bottom argon column T1 of the present invention, then discharge argon column T1 with the liquid argon product reclaimed and become liquid argon product 106, fresh liquid argon 105 also can add in liquid argon 108 after liquid argon pump 107, or described fresh liquid argon 105 directly enters after main heat exchanger E1 carries out re-heat to enter separately argon gas pipe network separately.
The present invention first uses known technology to produce the crude argon only containing hydrogen nitrogen, then the present invention is used to carry out being separated of argon gas and nitrogen hydrogen, the crude argon using known technology to produce enters main heat exchanger cooling liquid in ice chest, enter low-temperature fractionating tower, make argon gas and nitrogen hydrogen produce rectifying to be separated, obtain pure liquid argon, liquid argon obtains straight argon product after the re-heat of liquid argon pump supercharging main heat exchanger; The argon gas rate of recovery of argon gas retracting device of the present invention can reach 92% even higher, and fresh liquid argon can supplement cryogenic rectification cold while supplementing argon gas waste, so just do not need additionally to arrange refrigeration plant as decompressor etc., thus simple flow and minimizing investment.
It is high that the present invention has the argon gas rate of recovery, and reclaim purity of argon high, oxygen content is low, reclaims purifying energy consumption low, is particularly suitable for large-scale monocrystalline silicon production enterprise and carries out the features such as a large amount of argon gas recovery purifying recycling.
Accompanying drawing explanation
Fig. 1 is the structure explanation schematic flow sheet that argon gas of the present invention reclaims purification devices.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be described in detail: shown in Fig. 1, and the argon gas of a kind of double tower coupling of the present invention reclaims purifier apparatus, and this equipment mainly comprises an ice chest B1, a main heat exchanger E1, low-temperature fractionating tower and liquid argon pump 107.
Ice chest purposes is for Cryo Equipment pipeline provides a cold insulated cabinet, and equipment pipe is arranged in the full pearlife of middle rear filling, thus minimizing medium apparatus pipeline transmits cold in environment.The placement of liquid argon pump can be placed in ice chest and also can be placed on outside ice chest, and being placed on ice chest then needs outward to adopt vacuum tube heat insulation.
In described ice chest B1, main heat exchanger E1 and low-temperature fractionating tower are at least installed, described low-temperature fractionating tower is the double tower coupled structure be made up of Shang Ta and lower tower, wherein go up that tower is argon column T1, lower tower is nitrogen tower T2, centre is coupled by condenser/evaporator E2, it can save energy consumption, saves space; The top of described argon column T1 arranges condenser E3, and described argon column T1 is a upper rectifying column that the crude argon rectifying entering this tower can be separated into liquid argon and rectifying waste gas; And air separation one can be gone out nitrogen and make a part of nitrogen as byproduct by described nitrogen tower T2, another part is used for the lower rectifying column of argon gas normal temperature absorbing unit regeneration.
Condenser/evaporator E2 between described argon column T1 and nitrogen tower T2 is coupled to form by as the evaporimeter bottom argon column T1 with as the condenser at nitrogen tower T2 top, thermal source is wherein the source nitrogen from nitrogen tower T2, low-temperature receiver is the liquid argon source from argon column T1, source nitrogen is in intermediate condensation, and liquid argon evaporates in outside; The thermal source of the condenser that described argon column top is arranged is the upflowing vapor from argon column, and low-temperature receiver is the throttling oxygen-enriched liquid air from nitrogen tower bottom, and wherein upflowing vapor is in the intermediate condensation of condenser, and throttling oxygen-enriched liquid air evaporates in the outside of condenser; Described liquid argon pump 107 is also installed in ice chest B1, and the liquid argon products export bottom described argon column T1 connects described liquid argon pump 107 and carries out supercharging, and by the main heat exchanger re-heat in ice chest B1 to normal temperature access user argon gas pipe network.
At least be provided with in main heat exchanger E1 of the present invention:
One crude argon cooling liquid passage 1, the import of this passage connects crude argon 101 inlet pipe entering ice chest B1, and outlet connection one choke valve 103 accesses argon column T1 again;
One pressure-air cooling passage 2, the import of this passage connects compressed air 121 inlet pipe entering ice chest B1, outlet access nitrogen tower T2;
One nitrogen re-heat passage 3, the import connection of this passage and the nitrogen outlet at nitrogen tower T2 top, the outlet of passage picks out ice chest B1 by nitrogen tube;
An oxygen enrichment re-heat passage 4, the import of this passage is communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column T1 top respectively, and the outlet of passage picks out ice chest B1 by oxygen enrichment tube connector; Or have two oxygen enrichment re-heat passages, the import of these two passages is communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top respectively, and the outlet of two passages picks out ice chest respectively by oxygen enrichment tube connector.
The argon gas utilizing described double tower to be coupled reclaims purifier apparatus and carries out the method that argon gas reclaims purifying, and the method that described argon gas reclaims purifying comprises:
A) cooling of crude argon, first adopt known technology to produce only containing the crude argon of nitrogen hydrogen, crude argon 101 enters ice chest B1, then to enter main heat exchanger E1 cooling liquid be liquid argon 102; Liquid argon 102 enters argon column T1 and carries out rectifying separation after choke valve 103 throttling;
B) crude argon rectifying, crude argon carries out rectifying separation according to the characteristic that component boiling point is different in argon column T1, obtains liquid argon product 106 bottom argon column T1, discharges rectifying waste gas 112 at argon column T1 top; The condenser E3 condensation upflowing vapor 104 at argon column T1 top, the liquid 111 of condensation is as the phegma of argon column T1, and not solidifying gas is rectifying waste gas 112, and this rectifying waste gas 112 is extracted out from condenser E3 condensation side; Phegma 111 and the liquid that obtains through choke valve 103 throttling liquid argon 102 to decline liquid as rectifying, decline liquid carries out heat and mass with the upflowing vapor counter current contacting of evaporating from condenser/evaporator E2 bottom argon column T1, thus under flow to bottom argon column T1 and obtain liquid argon, upflowing vapor rises and to converge and gas that choke valve 103 throttling liquid argon 102 of hanging oneself obtains finally becomes upflowing vapor 104 at the bottom of tower; Bottom argon column T1, a part for liquid argon is discharged as product liquid argon 106, and another part is condensed evaporimeter E2 evaporation as upflowing vapor;
C) the producing of argon gas product, product liquid argon 106 is pressurized to the liquid argon 108 of user's argon gas ductwork pressure through liquid argon pump 107, and liquid argon 108 enters main heat exchanger E1 re-heat to be become the real argon gas 109 reclaiming purifying to normal temperature and enter user's argon gas pipe network; In product liquid argon 106, oxygen content general control is at below 2PPm, and the mole of product liquid argon 106 can reach more than 92% of argon mole in crude argon 101.
Shown in Fig. 1, the main component of rectifying waste gas 112 is nitrogen, hydrogen and argon gas, the rate of recovery of argon in how many direct reflection crude argons 101 of this portion gas amount.
Method of the present invention also comprises:
Through the compressed air 121 of impurity such as removing moisture content and carbon dioxide etc., enter ice chest B1, enter main heat exchanger E1 cooling again and become Cryogenic air 122, Cryogenic air 122 can be that gas also can contain a small amount of liquid entirely, Cryogenic air 122 enters low-temperature fractionating tower nitrogen tower T2, wherein gas fraction is as the upflowing vapor of nitrogen tower T2, and liquid part flows to the tower reactor at the bottom of tower; Upflowing vapor is with carrying out heat and mass from the phegma counter current contacting under overhead streams, obtain nitrogen 123 at nitrogen tower T2 top and enter condenser/evaporator E2 nitrogen 124, nitrogen 124 is condensed into liquid part as nitrogen tower liquid nitrogen reflux liquid 126 in condenser/evaporator E2, solidifying portion gas is that fixed gas 127 is extracted condenser/evaporator E2 out and discharged, and the discharge capacity of fixed gas 127 is generally less than 1% of compressed air 121; Liquid nitrogen reflux liquid 126 in nitrogen tower T2 to dirty, through flow to the heat and mass of upflowing vapor in the tower reactor at the bottom of nitrogen tower T2 tower with Cryogenic air 122 in flow to tower reactor liquid joint become oxygen-enriched liquid air 128 and extract out.
Described nitrogen 123 obtains byproduct nitrogen 125 through main heat exchanger E1 re-heat to normal temperature, and this nitrogen 125 part is as the regeneration nitrogen of argon gas normal temperature absorbing unit, and all the other can be used as plant protection gas and use;
Described oxygen-enriched liquid air 128 enters argon column condenser E3 after choke valve 129, as the upflowing vapor 104 of low-temperature receiver condensation from argon column T1 in condenser E3, self overwhelming majority is vaporizated into oxygen-rich steam 130, does not have evaporation section to discharge as oxygen-enriched liquid air 131 bottom condenser E3; The discharge effect of oxygen-enriched liquid air 131 is a small amount of CH preventing from containing in oxygen-enriched liquid air 128
4gathering at condenser E3 with heavy components such as nitrous oxides thus cause dangerous hidden danger, the discharge capacity of oxygen-enriched liquid air 131 is generally about 1% ~ 3% of oxygen-enriched liquid air 128 total amount; Converge after described oxygen-enriched liquid air 131 and oxygen-rich steam 130 go out condenser E3 and enter main heat exchanger E1 re-heat and become normal temperature oxygen-enriched air 133 to normal temperature; Or oxygen-enriched liquid air 131 and oxygen-rich steam 130 enter main heat exchanger E1 respectively, go out main heat exchanger E1 respectively; Oxygen-enriched air 133, as the regeneration gas of air normal temperature absorbing unit, also can be used for the place needing oxygen-enriched combusting.
The fresh liquid argon 105 of supplementary rectifying institute chilling requirement directly can be passed into bottom argon column T1 of the present invention, then discharge argon column T1 with the liquid argon product reclaimed and become liquid argon product 106, fresh liquid argon 105 also can add in liquid argon 108 after liquid argon pump 107, or described fresh liquid argon 105 directly enters after main heat exchanger E1 carries out re-heat to enter separately argon gas pipe network separately.
Cryogenic rectification of the present invention adopts double tower coupled structure, upper tower is argon column, and lower tower is nitrogen tower, and centre is coupled together by condenser/evaporator, rectifying institute chilling requirement provides by supplementing fresh liquid argon, while recovery purifying argon gas, produce nitrogen byproduct and oxygen-enriched air byproduct.
embodiment:
Reclaim in purifying project at the argon gas designed for certain monocrystalline silicon production enterprise, the amount of crude argon 101 is 960Nm
3/ H, argon molar content ~ 97% in crude argon 101, nitrogen and hydrogen molar content ~ 3%, argon mole is ~ 931.2 Nm
3/ H.Product liquid argon 106 output 927 Nm
3/ H, oxygen content 1.5PPm, nitrogen content 3PPm.Fresh liquid argon 127 directly passes into bottom argon column, and fresh liquid argon 127 magnitude of recruitment is 60Nm
3/ H, the argon gas amount reclaimed from crude argon is 867 Nm
3/ H.The rate of recovery of argon gas is 93.1%, and the supplementary rate of fresh liquid argon is 6.25% of crude argon.The amount of compressed air 121 is 1250 Nm
3/ H, the output of nitrogen 123 is 230 Nm
3/ H.
Utilize argon gas organic efficiency of the present invention to reach more than 92%, purity of argon is 1.5PPm oxygen and 3PPm nitrogen, and it is simple that rectifying cold adopts fresh liquid argon to supplement without the need to the low system of extra refrigeration plant energy consumption, and can produce nitrogen byproduct and secondary oxygen air byproduct.
Claims (7)
1. the argon gas of a double tower coupling reclaims purifier apparatus, this equipment mainly comprises an ice chest, one main heat exchanger, low-temperature fractionating tower and liquid argon pump, it is characterized in that, in described ice chest, main heat exchanger and low-temperature fractionating tower are at least installed, described low-temperature fractionating tower is the double tower coupled structure be made up of Shang Ta and lower tower, wherein go up that tower is argon column, lower tower is nitrogen tower, to be middlely coupled by condenser/evaporator; The top of described argon column arranges condenser, and described argon column is a upper rectifying column that the crude argon rectifying entering this tower can be separated into liquid argon and rectifying waste gas; And described nitrogen tower is one air separation can be gone out nitrogen and make a part of nitrogen as byproduct, another part is used for the lower rectifying column of argon gas normal temperature absorbing unit regeneration.
2. the argon gas of double tower coupling according to claim 1 reclaims purifier apparatus, it is characterized in that the condenser/evaporator between described argon column and nitrogen tower is coupled to form by as the evaporimeter bottom argon column with as the condenser of nitrogen top of tower, thermal source is wherein the source nitrogen from nitrogen tower, low-temperature receiver is the liquid argon source from argon column, source nitrogen is in intermediate condensation, and liquid argon evaporates in outside; The thermal source of the condenser that described argon column top is arranged is the upflowing vapor from argon column, and low-temperature receiver is the throttling oxygen-enriched liquid air from nitrogen tower bottom, and wherein upflowing vapor is in the intermediate condensation of condenser, and throttling oxygen-enriched liquid air evaporates in the outside of condenser; Described liquid argon pump is also installed in ice chest, and the liquid argon products export bottom described argon column connects described liquid argon pump and carries out supercharging, and by the main heat exchanger re-heat in ice chest to normal temperature access user argon gas pipe network.
3. the argon gas of double tower coupling according to claim 1 and 2 reclaims purifier apparatus, it is characterized in that at least being provided with in main heat exchanger:
One crude argon cooling liquid passage, the import of this passage connects the crude argon inlet pipe entering ice chest, and outlet connection one choke valve accesses argon column again;
One pressure-air cooling passage, the import of this passage connects the compressed air inlet pipe entering ice chest, outlet access nitrogen tower;
One nitrogen re-heat passage, the import connection of this passage and the nitrogen outlet of nitrogen top of tower, the outlet of passage picks out ice chest by nitrogen tube;
An oxygen enrichment re-heat passage, the import of this passage is communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top respectively, and the outlet of passage picks out ice chest by oxygen enrichment tube connector; Or have two oxygen enrichment re-heat passages, the import of these two passages is communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top respectively, and the outlet of two passages picks out ice chest respectively by oxygen enrichment tube connector.
4. utilize the argon gas of double tower coupling described in claim 1 or 2 or 3 to reclaim purifier apparatus and carry out an argon gas recovery purification process, it is characterized in that described argon gas reclaims purification process and comprises:
A) cooling of crude argon, first adopt known technology to produce only containing the crude argon of nitrogen hydrogen, crude argon (101) enters ice chest (B1), then to enter main heat exchanger (E1) cooling liquid be liquid argon (102); Liquid argon (102) enters argon column (T1) and carries out rectifying separation after choke valve (103) throttling;
B) crude argon rectifying, crude argon carries out rectifying separation according to the characteristic that component boiling point is different in argon column (T1), obtains liquid argon product (106), discharge rectifying waste gas (112) at argon column (T1) top in argon column (T1) bottom; Condenser (E3) condensation upflowing vapor (104) at argon column (T1) top, the liquid (111) of condensation is as the phegma of argon column (T1), and not solidifying gas is rectifying waste gas (112), and this rectifying waste gas (112) is extracted out from condenser (E3) condensation side; Phegma (111) and the liquid that obtains through choke valve (103) throttling liquid argon (102) to decline liquid as rectifying, decline liquid carries out heat and mass with the upflowing vapor counter current contacting of evaporating from argon column (T1) bottom condenser/evaporator (E2), thus under flow to argon column (T1) bottom and obtain liquid argon, upflowing vapor rises and to converge and gas that choke valve of hanging oneself (103) throttling liquid argon (102) obtains finally becomes upflowing vapor (104) at the bottom of tower; A part for argon column (T1) bottom liquid argon is discharged as product liquid argon (106), and another part is condensed evaporimeter (E2) evaporation as upflowing vapor;
C) the producing of argon gas product, product liquid argon (106) is pressurized to the liquid argon (108) of user's argon gas ductwork pressure through liquid argon pump (107), and the argon gas (109) that liquid argon (108) enters main heat exchanger (E1) re-heat becomes real recovery purifying to normal temperature enters user's argon gas pipe network; In product liquid argon (106), oxygen content general control is at below 2PPm, and the mole of product liquid argon (106) can reach more than 92% of argon mole in crude argon (101).
5. argon gas according to claim 4 reclaims purification process, it is characterized in that described method also comprises:
Through the compressed air (121) of impurity such as removing moisture content and carbon dioxide etc., enter ice chest (B1), enter main heat exchanger (E1) cooling again and become Cryogenic air (122), Cryogenic air (122) can be that gas also can contain a small amount of liquid entirely, Cryogenic air (122) enters low-temperature fractionating tower nitrogen tower (T2), wherein gas fraction is as the upflowing vapor of nitrogen tower (T2), and liquid part flows to the tower reactor at the bottom of tower; Upflowing vapor is with carrying out heat and mass from the phegma counter current contacting under overhead streams, obtain nitrogen (123) at nitrogen tower (T2) top and enter condenser/evaporator (E2) nitrogen (124), nitrogen (124) is condensed into liquid part as nitrogen tower liquid nitrogen reflux liquid (126) in condenser/evaporator (E2), not solidifying portion gas is that fixed gas (127) extracts condenser/evaporator (E2) discharge out, and the discharge capacity of fixed gas (127) is generally less than 1% of compressed air (121); Liquid nitrogen reflux liquid (126) in nitrogen tower (T2) to dirty, through flow to the heat and mass of upflowing vapor in the tower reactor at the bottom of nitrogen tower (T2) tower with Cryogenic air (122) in flow to tower reactor liquid joint become oxygen-enriched liquid air (128) and extract out.
6. argon gas according to claim 5 reclaims purification process, it is characterized in that described nitrogen (123) obtains byproduct nitrogen (125) through main heat exchanger (E1) re-heat to normal temperature, this nitrogen (125) part is as the regeneration nitrogen of argon gas normal temperature absorbing unit, and all the other can be used as plant protection gas and use;
Described oxygen-enriched liquid air (128) enters argon column condenser (E3) after choke valve (129), as the upflowing vapor (104) of low-temperature receiver condensation from argon column (T1) in condenser (E3), self overwhelming majority is vaporizated into oxygen-rich steam (130), do not have evaporation section to discharge as oxygen-enriched liquid air (131) from condenser (E3) bottom, the discharge capacity of oxygen-enriched liquid air (131) is generally 1% ~ 3% of oxygen-enriched liquid air (128) total amount; Converge after described oxygen-enriched liquid air (131) and oxygen-rich steam (130) go out condenser (E3) and enter main heat exchanger (E1) re-heat and become normal temperature oxygen-enriched air (133) to normal temperature; Or oxygen-enriched liquid air (131) and oxygen-rich steam (130) enter main heat exchanger (E1) respectively, go out main heat exchanger (E1) respectively; Oxygen-enriched air (133) as the regeneration gas of air normal temperature absorbing unit, or for needing the place of oxygen-enriched combusting.
7. the argon gas according to claim 4 or 6 reclaims purification process, it is characterized in that described argon column (T1) bottom directly can pass into the fresh liquid argon (105) of supplementary rectifying institute chilling requirement, then discharge argon column (T1) with the liquid argon product reclaimed and become liquid argon product (106), fresh liquid argon (105) also can add in liquid argon (108) after liquid argon pump (107), or described fresh liquid argon (105) directly enters after main heat exchanger (E1) carries out re-heat to enter separately argon gas pipe network separately.
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| CN115060041B (en) * | 2022-06-28 | 2024-04-05 | 四川空分集团工程有限公司 | System and method for producing nitrogen by liquid-air supercooling, backflow and expansion double towers |
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