CN209484936U

CN209484936U - A kind of device of integrated High Purity Nitrogen and argon gas recycling

Info

Publication number: CN209484936U
Application number: CN201920132649.7U
Authority: CN
Inventors: 郝文炳
Original assignee: Shanghai Union Wind Energy Technology Co Ltd
Current assignee: Shanghai Union Wind Energy Technology Co Ltd
Priority date: 2019-01-25
Filing date: 2019-01-25
Publication date: 2019-10-11
Anticipated expiration: 2029-01-25

Abstract

The utility model discloses the devices that a kind of integrated High Purity Nitrogen and argon gas recycle, this method utilizes the connection function for assisting condenser/evaporator, argon gas recycling flow path and air nitrogen flow path have carried out Cooling capacity exchanging, the extra cooling capacity that expanding machine generates is transported to argon gas recycling flow path, the liquid argon amount of extraneous addition can be significantly reduced.Reduce the operation cost of equipment.Meanwhile the utility model has the convenience of liquid argon offer using recycling scene, provides cooling capacity with liquid argon, cryogenic rectification method is recycled to remove nitrogen, hydrogen, the rate of recovery of argon gas and the utilization rate of hydrogen are improved, the process and operation of cryogenic rectification is simplified, reduces operation energy consumption.In addition, the utility model generates cooling capacity by expanding machine also using integrated air nitrogen flow path, self-produced nitrogen in ice chest can reduce the limitation of regeneration gas, improve the recovery rate of recycling argon gas.

Description

A kind of device of integrated High Purity Nitrogen and argon gas recycling

Technical field

The utility model relates to the dresses of a kind of method of argon gas recycling more particularly to a kind of integrated High Purity Nitrogen and argon gas recycling It sets.

Background technique

Vertical pulling method (Czochralski method) is to produce the main method of monocrystalline silicon, the monocrystalline in the whole world 70%~80% Silicon is produced by vertical pulling method.Most common vertical pulling method production monocrystalline silicon technique is using i.e. as vacuum technology is again as flowing atmosphere work The decompression crystal pulling technique of skill；Decompression technique is to be passed through height into single crystal growing furnace burner hearth to continuous constant speed in silicon single crystal pulling process Purity argon, while vacuum pump is constantly from the outside pump Argon of burner hearth keeps in burner hearth vacustat in 20 supports or so, this The characteristics of kind of technique existing vacuum technology, and have the characteristics of flowing atmosphere technique.The vacuum pump of decompression crystal pulling technique generally uses Slide valve pump, slide valve pump are the oil-sealed rotary pumps that sealing is kept with oil.Argon gas is produced during carrying crystal-pulling due to high temperature Raw Si oxide and impurity volatile matter, and atmosphere is discharged by pumping for vacuum pump.

By the analysis to discharge argon gas, major impurity ingredient is oxygen, nitrogen, carbon monoxide, carbon dioxide, methane etc. Alkane, liquid lubricant mist；Recycling this part argon gas has very big realistic meaning.

The well-known technique of argon gas recovery purifying: thick oil removing is carried out to the argon gas recycled from single crystal growing furnace, then is cooled down through compression High-precision oil removing dedusting afterwards；Then the hydro carbons such as methane and carbon monoxide is made to react production water and dioxy with oxygen by high-temperature catalytic Change carbon, guarantees that oxygen is excessive (oxygen is not enough then added in impurity oxygen) in catalysis reaction；By after cooling under the action of catalyst So that excessive oxygen is generated water with the hydrogen reaction being added, and guarantee to react hydrogen excessive, after processing in argon gas impurity component be water, Carbon dioxide, hydrogen and nitrogen；Finally by argon gas room temperature absorbing unit absorption water and carbon dioxide, obtain containing only nitrogen and Hydrogen is the crude argon of impurity.Argon gas room temperature absorbing unit is made of two absorbers, equipped with absorption water and dioxy in absorber Change the adsorbent of carbon, an absorber carries out absorption work, and it includes pressure release that another absorber, which carries out, heats, blows cold regeneration Work.The gas of the reproduction operation uses nitrogen, and the regeneration nitrogen is from low-temperature fractionating tower production or outsourcing, argon gas in ice chest Room temperature absorbing unit is switched by program timer auto-controll operation.

In patent " method and apparatus of argon gas recovery purifying in monocrystalline silicon production " (application number: 201210078306.x), Cryogenic rectification part uses air cycle refrigeration, and energy consumption is high, and process is complicated, the excess hydrogen emptying of addition, and utilization rate is low.

Patent " a kind of the argon gas recovery purifying equipment and argon gas recovery purifying method of double tower coupling " (application number: 201410618341.5) it in, is compressed with air, double-column process, energy consumption is without advantage, and structure is complicated, increases equipment investment.

A kind of patent " device of single column cryogenic rectification recycling argon gas " (application number: in 201621146690.2), to keep The extraneous liquid argon amount that ice chest provides is larger, and is limited by regeneration gas, and recovery rate is relatively low.Patent, which only designs, carrys out deoxygenation, does not go Except the removal of excess carbon monoxide in raw material.

In patent " a kind of device and method for improving the argon gas rate of recovery " (application number: CN201810580354.6), use Be stream backed expansion, be suitable for argon gas band extrude tower situation, be not suitable for argon gas normal pressure and go out tower.

Therefore, those skilled in the art is dedicated to that development process is more succinct, and more convenient operation, energy consumption is lower, recovery rate Higher argon gas recovery method.

Utility model content

The purpose of this utility model is for moving component in the recycling of present argon gas is more, energy consumption is high, investment is big, recovery rate is low The features such as, using monocrystalline silicon producer have liquid argon supply condition, provide cryogenic rectification process be simple and convenient to operate, energy consumption Lower, the higher method of recovery rate is suitable for argon gas normal pressure and goes out tower

The purpose of this utility model is for moving component in the recycling of present argon gas is more, energy consumption is high, investment is big, recovery rate is low The features such as, the condition of liquid argon supply is had using monocrystalline silicon producer, provide a kind of cryogenic rectification process be simple and convenient to operate, Energy consumption is lower and the device of the higher integrated High Purity Nitrogen and argon gas recycling for going out tower suitable for argon gas low pressure normal pressure of recovery rate.

To achieve the above object, the utility model uses following technical scheme:

The utility model provides the device of a kind of integrated High Purity Nitrogen and argon gas recycling, comprising: rectifying ice chest is set to institute It states the main heat exchanger in ice chest, pure argon column, the argon column reboiler for being set to the pure argon column bottom, be set to the pure argon column top The argon column condenser/evaporator in portion, smart nitrogen tower, the nitrogen tower reboiler for being set to the smart nitrogen tower bottom, is set auxiliary condenser/evaporator It is placed in nitrogen tower condenser/evaporator, the gas-liquid separator, expanding machine of the smart nitrogen top of tower, and the argon being set to outside the ice chest Air compressor removes carbon monoxide remover, the first cooler, the second cooler, oxygen-eliminating device, air compressor machine, argon gas pre-cooling purification system, sky Purification system is pre-chilled in gas；Wherein:

The argon gas compressor successively by it is described except carbon monoxide remover, the first cooler, oxygen-eliminating device, the second cooler, Argon gas pre-cooling purification system, main heat exchanger are connect with the argon column reboiler by pipeline；The argon column reboiler passes through crude argon Throttle valve is connect with the pure argon column middle and upper part by pipeline；The pure argon column bottom is cold through pure liquid argon throttle valve and the argon column The evaporation side of solidifying evaporator is connected by pipeline；The argon column condenser/evaporator is connected pure outside the rectifying ice chest by pipeline Argon gas user pipe；The pure argon column top gas outlet is also connected by the gas side of pipeline and the argon column condenser/evaporator It connects；The pure argon column top gas outlet is also connect by pipeline with the gas side of the auxiliary condenser/evaporator, the auxiliary The evaporation side of condenser/evaporator is connect by pipeline with the pure argon column overhead-liquid entrance；

The air compressor machine successively passes through air precooling purification system, main heat exchanger, nitrogen tower reboiler and the gas-liquid separation Device is connected by pipeline, and the liquid outlet of the gas-liquid separator is by the bottom for assisting condenser/evaporator and the smart nitrogen tower Portion is connected by pipeline, and the liquid outlet of the gas-liquid separator is directly connect with the bottom of the smart nitrogen tower by pipeline；Institute State the gas vent of gas-liquid separator and the gas vent remittance merga pass pipeline of the auxiliary condenser/evaporator and the smart nitrogen The bottom of tower connects；The middle part of the main heat exchanger is connect with the bottom of the smart nitrogen tower by pipeline by the expanding machine； The gas vent of the essence nitrogen column overhead is connect with the high temperature side of the nitrogen tower condenser/evaporator by pipeline；The essence nitrogen tower Bottom is connect with the nitrogen tower condenser/evaporator by pipeline by throttle valve.

Further, Hydrogen Line is accessed on the pipeline between first cooler and the oxygen-eliminating device.

Further, the evaporation side of the argon column condenser/evaporator is connected by the main heat exchanger by pipeline described pure Argon gas user pipe.

Further, which is characterized in that the pure argon column top gas outlet is connected by the main heat exchanger by pipeline Connect the purifier in the argon gas pre-cooling purification system.

Further, purification system is pre-chilled by the heat exchanger, rectifying ice chest and the argon gas in the smart nitrogen top of tower In purifier pass through pipeline connect.

Further, the argon gas pre-cooling purification system and the air precooling purification system are by a precooler and two The purifier composition that platform is arranged in parallel.

It further, further include the throttle valve in each connecting pipe.

The utility model by adopting the above technical scheme, compared with prior art, has the following technical effect that

The method and device of integrated High Purity Nitrogen and argon gas recycling provided by the utility model, makes full use of auxiliary condensation evaporation The connection function of device, argon gas recycling flow path and air nitrogen flow path have carried out Cooling capacity exchanging, the extra cooling capacity that expanding machine is generated It is transported to argon gas recycling flow path, the liquid argon amount of extraneous addition can be significantly reduced, reduce the operation cost of equipment；It is existing using recycling Field has the convenience of liquid argon offer, provides cooling capacity with liquid argon, recycles cryogenic rectification method to remove nitrogen, hydrogen, improve argon gas The rate of recovery and hydrogen utilization rate, simplify the process and operation of cryogenic rectification, reduce operation energy consumption；Utilize integrated sky Gas nitrogen flow path generates cooling capacity by expanding machine, and self-produced nitrogen in ice chest can reduce the limitation of regeneration gas, improve recycling argon gas Recovery rate；In addition, the utility model also makes argon gas recycling stream using expander decompression in integrated air nitrogen flow path Road is suitable for argon gas low pressure and normal pressure goes out tower situation.

Detailed description of the invention

Fig. 1 is the flow diagram for the device that a kind of integrated High Purity Nitrogen of the utility model and argon gas recycle；

Wherein, each appended drawing reference are as follows:

1- argon gas compressor；2- removes carbon monoxide remover；The first cooler of 3-；4- oxygen-eliminating device；The second cooler of 5-；6- argon gas Purification system is pre-chilled；7- rectifying ice chest；7- rectifying ice chest；8- heat exchanger；9- argon column reboiler；10- pure argon column；11- argon column is cold Solidifying evaporator；12 auxiliary condenser/evaporators；13- gas-liquid separator；14- nitrogen tower reboiler；15- essence nitrogen tower；The condensation of 16- nitrogen tower is steamed Send out device；17- air compressor；18- air precooling purification system；19- expanding machine；20-V2 crude liquid argon throttle valve；The pure liquid of 21-V1 Argon throttle valve.

Specific embodiment

The utility model is described in more detail below by specific embodiment, for a better understanding of this reality With novel, but following embodiments are not intended to limit the scope of the utility model.

As schemed, one embodiment of the utility model:

Meanwhile Hydrogen Line is accessed on the pipeline between first cooler and the oxygen-eliminating device；The argon column condensation The evaporation side of evaporator connects the pure argon user pipe by pipeline by the main heat exchanger；Gas at the top of the pure argon column Body outlet connects the purifier that the argon gas is pre-chilled in purification system by pipeline by the main heat exchanger；The essence nitrogen Top of tower is connect with the purifier in argon gas pre-cooling purification system by pipeline by the heat exchanger, rectifying ice chest；Institute State the purifier that argon gas pre-cooling purification system and the air precooling purification system are arranged in parallel by a precooler and Liang Tai Composition；The utility model further includes the throttle valve in each connecting pipe.

Using a kind of method of the utility model embodiment, embodiment is as follows:

As shown in Fig. 1, argon gas (O is recycled₂<~0.4%, N₂<~1.5%, CO :~1500ppm, remaining is Ar) pressure Power is very low, first passes around argon gas compressor 1 and is forced into~0.5-0.75MPa (A) and after removing oil removing and dust, by GAr-101, Into except carbon monoxide remover 2.It except loading catalyst in carbon monoxide remover 2, is reacted by catalysis, is two catalyzing carbon monoxide Carbonoxide.CO exports content < 1ppm.The argon gas of removal CO enters cooler I3 by GAr-102 pipeline after coming out and is cooled to about 40 DEG C, oxygen-eliminating device 4 is entered after mixing in GAr-103 with the hydrogen of addition, in oxygen-eliminating device 4, oxygen reacts with hydrogen, It generates water and discharges heat, have difference depending on the rising of oxygen amount temperature, when O2 content is not higher than 0.4%, temperature can be < 100 ℃.Enter cooler II 5 by GA-104 high temperature argon and be cooled to 40 DEG C, argon gas is entered by GAr-105, purification system is pre-chilled Argon gas precooler in 6 is cooled to 5-8 DEG C and purifier removes water and carbon dioxide.Remaining argon gas mainly becomes are as follows: Ar, N2, H2 etc..

Dry crude argon (0.5-0.7MPa (A), 20 DEG C) enters rectifying ice chest 7 by pipeline GAr-106, initially enters Heat exchanger 8 is cooled to liquefaction point, by GAr-107, into the argon column reboiler 9 for being built in 10 bottom of pure argon column, argon column again It boils in device 9, most of gas (80%~95%) is liquefied, and the gas-liquid mixture fluid of argon column reboiler 9 is flowed from GAr-108 out Out, 10 middle and upper part of pure argon column is sent into through crude argon throttle valve V2 reducing pressure by regulating flow to 0.42MPa (A) participate in rectifying.Argon column reboiler 9 Operating pressure is~0.52~0.62MPaA, and the pressure of pure argon column 10 is 0.42MPa (A), temperature be argon gas at this pressure - 169.9 DEG C of boiling point.Since there are pressure difference, medium boiling temperature can make outside shape in argon column reboiler 9 according to pressure change At about 0.5~1.5 DEG C of the temperature difference, guarantee the heat exchange of argon column reboiler 9.

Into the fluid of pure argon column 10, gas part therein is with gas rising in tower, and liquid is under liquid in tower Drop, heat and mass transfer process occurs for gas-liquid in ascending and descending process, and the Ar content of liquid portion is higher and higher, obtains in tower bottom pure Liquid argon (depending on national standard or customer requirement, routinely can reach N2 < 4ppm).It is taken out by LARS-201 pipeline from rectifier bottoms Pure liquid argon is sent into the evaporation side of argon column condenser/evaporator 11 through pure liquid argon throttle valve V1 reducing pressure by regulating flow to 0.15MPa (A) out.It is extraneous Supplement liquid argon enters the evaporation side of condenser/evaporator 11 by pipeline LAr-305 together, supplements loss of refrigeration capacity for whole system.It is pure Liquid argon is evaporated to argon gas in 11 evaporation side of argon column condenser/evaporator, by heat exchanger re-heat to 17 DEG C of recycling cooling capacity, sends out rectifying Ice chest can pressurize according to user demand or directly supply gas.

The gas at 10 top of pure argon column is mainly hydrogen and nitrogen, goes out after tower from GAr-301 pipeline and is divided into three parts, and one Divide and extracted out from GAr-302, through 8 re-heat of heat exchanger to~17 DEG C, is generally sent with after 1.5~3 DEG C of recycling cooling capacity lower than intake air temperature Out outside tower, as regeneration gas a part of argon gas pre-cooling purification system 6, the nitrogen come out with ice chest is purifier regeneration together With.The second part gas of tower top is condensed into liquid by the gas side that GAr-301 enters argon column condenser/evaporator 11, passes through LAr-306 flows back to pure argon column 10, provides liquid for rectifying.Part III gas enters auxiliary condenser/evaporator by GAr-304 12, it exchanges heat with part liquid air, after being condensed into liquid, after entering LAr-306 and second part liquid joint by LAr-305 It is sent into pure argon column 10.

Air is compressed to 0.6~1.0MPaA by air compressor machine 17, enters air precooling purification system 2 by GA-101, goes Water removal and carbon dioxide (wherein, CO2 < 1ppm).In GAr-102 be it is dry after air, the heat exchange into rectifying ice chest 7 Device 8 cools down, and from the middle part extraction section gas (temperature is -140 DEG C~-158 DEG C) of heat exchanger 8, is expanded into expanding machine 19 Nitrogen pressure tower (generally 0.3MPaA~0.5MPaA) is sent into nitrogen tower by GA-111.Another stock come out from 8 end of heat exchanger Air is cooled to condensing temperature.In GA-103, the micro band liquid of air, temperature is -165~-175 DEG C.Cryogenic air enters Nitrogen tower reboiler 14 by partial liquefaction, out after enter gas-liquid separator 13.In gas-liquid separator, liquid is from bottom LA-105 After outflow, it is divided into two strands, one LA-105 is sent directly into nitrogen tower 15, and the operating pressure of nitrogen tower is 0.33~0.43MPaA.It is another Stock LA-106 is sent into auxiliary condenser/evaporator 12, provides cooling capacity for it, the gas GAr-304 come out at the top of the pure argon column 10 that liquefies, Gas after being vaporized itself is mixed by GA-107 with from GA-108 of the gas Jing Guo V7 valve regulation of gas-liquid separator 13 out 15 bottom of nitrogen tower is sent into after conjunction, the rectifying for nitrogen tower 15 provides gas.

In the polylith column plate of nitrogen tower 15 (or filler) contacts uprising gas with dropping liq, heavy constituent (oxygen, argon Gas) it can gather in a liquid, it is finally to obtain high-purity nitrogen in tower top that light component (mainly nitrogen) can be gathered in gas (oxygen content is < 1ppm), the liquid of tower bottom become oxygen rich air because of the increase of liquid oxygen content (oxygen content is about 30%~40%).Nitrogen The pressure of tower is 0.3~0.4MPaA, and temperature is the boiling point of liquid under the pressure.After 15 tower top of nitrogen tower extraction nitrogen, it is divided into two Stock, one GN-301 are sent into the high temperature side of nitrogen tower condenser/evaporator 16, send nitrogen back to by LN-302 after liquid nitrogen by cooling down Tower participates in the rectifying of nitrogen tower 15 as the liquid of decline.Another gang of GN-302, after cooling capacity is recycled in 8 re-heat of main heat exchanger, Rectifying ice chest 7 is sent out, Argon Purifier 6 is sent into, is used as regeneration gas.

It is cold to be sent into nitrogen tower after throttle valve V6 adjusts pressure for the oxygen-enriched liquid air that the bottom of nitrogen tower 15 is extracted out by LA-201 Solidifying evaporator 16, provides cold source for it, itself is vaporizated into oxygen rich air and goes out nitrogen tower condenser/evaporator 16, enter master through GRO-202 After 8 re-heat of heat exchanger to 17 DEG C of room temperature, rectifying ice chest 7 is sent out.It is delivered to air precooling purification system 18, as dry gas, Participate in the regeneration of purifier.

Specific embodiment of the utility model is described in detail above, but it is merely an example, this is practical new Type is not restricted to particular embodiments described above.To those skilled in the art, any pair of the utility model carries out Equivalent modifications and substitution also all among the scope of the utility model.Therefore, in the spirit and model for not departing from the utility model Lower made equal transformation and modification are enclosed, should all be covered in the scope of the utility model.

Claims

1. the device of a kind of integrated High Purity Nitrogen and argon gas recycling characterized by comprising rectifying ice chest is set to the ice chest Interior main heat exchanger, pure argon column, the argon column reboiler for being set to the pure argon column bottom, the argon being set at the top of the pure argon column Tower condenser/evaporator, smart nitrogen tower, the nitrogen tower reboiler for being set to the smart nitrogen tower bottom, is set to institute at auxiliary condenser/evaporator Nitrogen tower condenser/evaporator, the gas-liquid separator, expanding machine of smart nitrogen top of tower are stated, and the argon gas compression being set to outside the ice chest Machine removes carbon monoxide remover, the first cooler, the second cooler, oxygen-eliminating device, air compressor machine, argon gas pre-cooling purification system, air precooling Purification system；Wherein:

The argon gas compressor successively removes carbon monoxide remover, the first cooler, oxygen-eliminating device, the second cooler, argon gas by described Pre-cooling purification system, main heat exchanger are connect with the argon column reboiler by pipeline；The argon column reboiler throttles by crude argon Valve is connect with the pure argon column middle and upper part by pipeline；It is steamed through pure liquid argon throttle valve and the argon column condensation pure argon column bottom The evaporation side for sending out device is connected by pipeline；The argon column condenser/evaporator connects the pure argon outside the rectifying ice chest by pipeline User pipe；The pure argon column top gas outlet is also connect by pipeline with the gas side of the argon column condenser/evaporator；Institute It states the outlet of pure argon column top gas also to connect by pipeline with the gas side of the auxiliary condenser/evaporator, the auxiliary condensation is steamed The evaporation side of hair device is connect by pipeline with the pure argon column overhead-liquid entrance；

It is logical that the air compressor machine successively passes through air precooling purification system, main heat exchanger, nitrogen tower reboiler and the gas-liquid separator The liquid outlet of piping connection, the gas-liquid separator is logical by the bottom of the auxiliary condenser/evaporator and the smart nitrogen tower Piping connection, the liquid outlet of the gas-liquid separator are directly connect with the bottom of the smart nitrogen tower by pipeline；The gas The gas vent remittance merga pass pipeline and the smart nitrogen tower of the gas vent of liquid/gas separator and the auxiliary condenser/evaporator Bottom connection；The middle part of the main heat exchanger is connect with the bottom of the smart nitrogen tower by pipeline by the expanding machine；It is described The gas vent of smart nitrogen column overhead is connect with the high temperature side of the nitrogen tower condenser/evaporator by pipeline；The bottom of the essence nitrogen tower It is connect with the nitrogen tower condenser/evaporator by pipeline by throttle valve.

2. the device of integrated High Purity Nitrogen according to claim 1 and argon gas recycling, which is characterized in that first cooler Hydrogen Line is accessed on pipeline between the oxygen-eliminating device.

3. the device of integrated High Purity Nitrogen according to claim 1 and argon gas recycling, which is characterized in that the argon column condensation is steamed The evaporation side of hair device connects the pure argon user pipe by pipeline by the main heat exchanger.

4. the device of integrated High Purity Nitrogen according to claim 1 and argon gas recycling, which is characterized in that at the top of the pure argon column Gas vent is connect with argon gas pre-cooling purification system by pipeline by the main heat exchanger.

5. the device of integrated High Purity Nitrogen according to claim 1 and argon gas recycling, which is characterized in that the essence nitrogen top of tower Gas vent is connect with the air precooling purification system by pipeline by the main heat exchanger.

6. the device of integrated High Purity Nitrogen according to claim 1 and argon gas recycling, which is characterized in that the argon gas pre-cooling is pure Change system and the air precooling purification system are made of the purifier that a precooler and Liang Tai are arranged in parallel.

7. the device of integrated High Purity Nitrogen according to claim 1 and argon gas recycling, which is characterized in that further include being set to each company Throttle valve on adapter tube road.