CN1660468A - Separating method of mixed gas,nitrogen separator and its consumption system - Google Patents
Separating method of mixed gas,nitrogen separator and its consumption system Download PDFInfo
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- CN1660468A CN1660468A CN 200410059563 CN200410059563A CN1660468A CN 1660468 A CN1660468 A CN 1660468A CN 200410059563 CN200410059563 CN 200410059563 CN 200410059563 A CN200410059563 A CN 200410059563A CN 1660468 A CN1660468 A CN 1660468A
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Abstract
Provided is a method for separating a mixture gas with an economically advantageous and feasible PSA system, which stabilizes the purity of a nitrogen product gas, and a device for separating the nitrogen gas, and a system for consuming the nitrogen gas. A low-pressure regeneration process of an absorption tower is constituted of 99-20% of a process consisting of the discharge of a gas in the absorbing tower to the atmosphere and the washing of the inside of the absorption tower with the product gas, and 1-80% of a process comprising preparatory pressurizing in such a state that the absorption tower is closed and only a line for performing the washing of the inside of the absorption tower with the product gas is opened. The problem can be solved by the mixed gas separation method in which the oxygen concentration at the outlet of the absorption tower performing high pressure adsorption is detected and low-pressure regeneration is automatically changed according to a value set for the oxygen concentration.
Description
Technical field
The present invention relates to a kind of separation method and nitrogen separation device and nitrogen consume system of mixed gas.In more detail, relate to and a kind ofly depressing adding, to be that the unstripped gas of main component is supplied with in 2 of being filled with molecular-sieve carbon or the above adsorption tower with nitrogen, high pressure absorption and low pressure regeneration are alternately repeated in each adsorption tower, in the separation method of nitrogen as the isolated mixed gas of product gas, it is that the low pressure regeneration step of adsorption tower is according to making the gas that comprises in the adsorption tower account for 99～20% to the atmospheric steam exhaust and the step of cleaning in to adsorption tower with product gas, with comprise the sealing adsorption tower, only open and carry out the pipeline that in the adsorption tower of product gas, cleans and the step of pre-loading accounts for 1～80% and the mixed gas separation method that constitutes, the adsorption tower outlet oxygen concentration of high pressure absorption is carried out in detection, according to its oxygen concentration set(ting)value, low pressure regeneration is changed automatically, economic and the effective separation method of mixed gas, and nitrogen separation device and nitrogen system.
Background technology
In recent years, various fields such as sealed gas in metal treatment, semi-conductor manufacturing, chemical industry, the demand of nitrogen increases, as this nitrogen manufacture method, adopt pressure swing adsorption process (hereinafter to be referred as the PSA method) mostly, use carbon porous inseries such as molecular-sieve carbon, separation of nitrogen from forced air.So-called PSA method, be when unstripped gas is air, use common 2 or the above adsorption tower that is filled with molecular-sieve carbon, in an adsorption tower, supply with forced air and carry out oxygen absorption, take out as product gas with nitrogen, in other adsorption tower, carry out desorb simultaneously, the absorption of oxygen and desorb are alternately repeated between a plurality of adsorption towers, utilize rate of adsorption poor of oxygen and nitrogen, prepare the method for nitrogen continuously.
Particularly nearest, utilize the new application field of the nitrogen of PSA to enlarge, soldering welding electronic unit carried out in atmosphere originally on the printed circuit board (PCB), was studying under nitrogen atmosphere now and was carrying out.Carry out the soldering welding under nitrogen atmosphere, its advantage is to use unleaded soft solder also can prevent the oxidation of printed circuit board (PCB) or soft solder, but requires to utilize PSA stably to make, supply with nitrogen.
According to Fig. 2 explanation, use 2 adsorption towers, be the mixed gas of main component by PSA method separation of air etc. with nitrogen, obtain the existing method of nitrogen product.At first, importing air etc. from unstripped gas supply-pipe 1 is the unstripped gas of main component with nitrogen, utilizes compressor 2 to compress, and imports adsorption towers 4 or 5 by water cooler 3.Be filled with molecular-sieve carbon in each adsorption tower, during an adsorption tower absorption, the another one adsorption tower is just in desorb (regeneration).
That is, when utilizing adsorption tower 4 to adsorb, valve 7,11 and 12 is an open mode, and valve 8,9,10,13 and 14 is a closing condition.In addition, the nitrogen that the adsorption tower in the regeneration generates the adsorption tower in the absorption passes through aperture 15, cleans (flushing) adsorption tower.By described nitrogen wash, be widely adopted because can implement the PSA method more effectively, as described later, also the nitrogen of product storage tank 6 is supplied with adsorption tower (for example patent documentation 1,2) sometimes.
Patent documentation 1 spy opens flat 1-94915 communique
Pass through after fixed time, valve 8,10 and 13 one-tenth open modes, valve 7,9,12 and 14 one-tenth closing conditions, adsorption tower 5 adsorbs, adsorption tower 4 desorbs are carried out aforesaid operations repeatedly, make nitrogen as product gas.
The time that these valves are set according to timer, automatically switch one by one, the nitrogen storage of manufacturing is ensconced in the product storage tank 6, through flow rate-measuring device 17, takes out from product gas take-off pipe 19, then consumption.The 16th, measure the oxygen densitometer that product gas purity is used.Be adsorbed under the desorb utilization decompression of the gas (oxygen) on the molecular-sieve carbon or the normal atmosphere and carry out, valve 8 or 11 makes the desorption of gases that is adsorbed on the molecular-sieve carbon when the state of opening, and desorption gas is by vapor pipe 18 exhausts.
, under practical situation, the usage quantity of nitrogen is not necessarily determined, intermittently uses sometimes, even intermittently do not use, usage quantity also has change in time mostly.In addition, for 1 nitrogen manufacturing installation, in most cases be used with many nitrogen consumer unit, usage quantity can change usually.For example disclose PSA device and the assembling in automatic soldering welding plant of using specific sorbing material in the patent documentation 3, but do not related to fully for solving usage quantity change problem.As the countermeasure that relaxes this change, usually take in nitrogen manufacturing installation with the ability about average usage quantity, large-scale nitrogen storage tank is set absorbs change, or replenish this device of the ability corresponding and the method for insufficient section when changing etc. with fixing usage quantity by other source of the gas such as liquid nitrogen.
Patent documentation 3 spies open flat 10-5522 communique
But, large-scale nitrogen storage tank is set, will correspondingly increase cost of equipment significantly, comprise area is set that in addition, according to the amplitude of fluctuation of nitrogen usage quantity, the nitrogen storage cell body of making is long-pending huge, can not realize as a rule in reality.In addition, the insufficient section during change depends on the method for other gas source, not only make the supply etc. of process complications, gas source and the installation cost that produces increases, and has slackened this device is supplied with cheap gas by unattended mode advantage.
In addition, when can the be corresponding maximum usage quantity of this set device, even the usage quantity of nitrogen reduces, the gas volume that is adsorbed on the molecular-sieve carbon is also almost constant, thereby the minimizing of the unstripped gas scale of construction of using is very little, and the minimizing of required drive is also very little.This can understand from following example easily, for example, the purity of product nitrogen gas is made as certain value, the feed rate of unstripped gas is 350, and the usage quantity of product nitrogen gas is 100, and the free air delivery of following adsorption tower to switch is 250 when turning round, even the usage quantity of product nitrogen gas reduces by half to 50, because free air delivery is constant, the unstripped gas feed rate is 300, only reduces more than 10% at most.In addition, when having reduced the usage quantity of nitrogen, the purity of nitrogen further improves, and preparation needs above superfluous purity not only almost nonsensical on using, and under different situations, brings bad influence sometimes.The energy aspect also is waste.
The method that addresses this is that, known is when controlling the PSA mode effectively, carries out gas separation method (patent documentation 4,5).Method described herein is just to carry out the method that next step operation is provided with like this when reaching a certain amount of according to resultant gas, but, these methods all are only to use conduct such as zeolite system: sorbing material, can implement when utilizing equilibrium adsorption in the gas phase to separate; When implementing the PSA method, using molecular-sieve carbon, when utilizing the difference of rate of adsorption to carry out gas delivery, adsorptive capacity, separating power change in time, and be inapplicable.
Patent documentation 4 spies open clear 54-16375 communique.
In addition, the known relevant method (patent documentation 6) of control that has with the PSA that uses molecular-sieve carbon.Document disclosed method is the oxygen concentration that detects from the product nitrogen gas that the product nitrogen gas storage tank comes out, determine the method for the suction desorb switching cycle (below be sometimes referred to as time semi-period) in the adsorption tower, but in the method, because in a single day nitrogen that adsorption tower is come out be stored in the product nitrogen gas storage tank, just can not corresponding sharply flow change the variation of the oxygen concentration of bringing.
Patent documentation 6 special fair 4-69085 communiques.
Detection is also arranged from the oxygen concentration in the nitrogen of adsorption tower, determine the method (patent documentation 7) of the switching time of adsorption tower.Although but utilize this method can make remaining oxygen concentration keep stable, owing to cause the increase of the unstripped gas scale of construction, energy aspect existing problems.And this method is owing to be to switch adsorption tower when reaching the oxygen concentration of setting, in the situation of sorbing material deterioration, perhaps to give play to ability 100% or when above, switching cycle can be shorter and shorter, the necessary unstripped gas scale of construction can cumulative adding.And under the situation of scarce capacities such as compressor of pressurization unstripped gas, switching cycle is in case shorten, and the pressure that reaches of adsorption tower then descends, thereby the separation efficiency of sorbing material worsens, and gas sometimes can not manufacture a product.
Patent documentation 7 spies open the 2000-42339 communique.
Summary of the invention
In addition, existing decrement method for controlling of operation (patent documentation 8) adopts with the gas that adsorbs on the sorbent material PSA method as product gas, can change the switching cycle of the switching valve of adsorption tower automatically according to the taking-up amount of product gas, reduces the electric consumption.Decrement method for controlling of operation disclosed herein is a kind of method of conserve energy, is considered to useful.
No. 2872678 communiques of patent documentation 8 special permissions
But, utilize this method owing to can not keep remaining oxygen constant concentration, so product nitrogen gas purity is too high easily.Thereby the object of the present invention is to provide a kind of purity of product nitrogen gas that can make stable, supplying products nitrogen stably simultaneously is by utilizing separation method and the nitrogen separation device and the nitrogen consume system of the mixed gas that the PSA mode carries out cost-effectively.
The present inventor finds, in the separation method of the mixed gas that a kind of PSA of utilization mode is carried out, the low pressure regeneration step that makes adsorption tower is according to making the gas that comprises in the adsorption tower account for 97～20% to the step that atmospheric exhaust and product gas clean in to adsorption tower, with comprise the sealing adsorption tower, only open and carry out by product gas having applied for patent (patent documentation 9) before this to the pipeline that cleans in the adsorption tower and the step of pre-loading accounts for the separation method of 3～80% mixed gass that constitute.
Patent documentation 9 spies open 2002-159820
The separation method of this mixed gas provides a kind of cost-effective PSA mode, but, the present inventor has carried out repeatedly research at length for the separation method of the better mixed gas of exploitation, found that, be conceived to according to the taking-up amount of product gas and the oxygen concentration of adsorption tower changes, the set(ting)value by according to the outlet oxygen concentration of adsorption tower automatically changes the switching cycle of adsorption tower, can implement very good mixing gas separating method, until finishing the present invention.In the PSA mode,, be divided into the gas that comprises in the adsorption tower to the atmospheric steam exhaust and the step (steps A) of cleaning in to adsorption tower by product gas with the low pressure regeneration step of adsorption tower; With comprise the sealing adsorption tower, by the step (step B) of product gas to cleaning in the adsorption tower, by using the automatic mode that changes of switching cycle that makes adsorption tower according to the outlet oxygen concentration of adsorption tower, can reach better PSA mode thus, this is to be not easy the surprising effect expected from prior art.
Promptly, the 1st aspect of the present invention provides a kind of separation method of mixed gas, depress adding, to be that the unstripped gas of main component is supplied at least 2 adsorption towers that are filled with molecular-sieve carbon with nitrogen, carry out high pressure absorption, adsorption tower after absorption finishes carries out low pressure regeneration, in each adsorption tower, alternately repeat high pressure absorption and low pressure regeneration, in the separation method of nitrogen as the isolated mixed gas of product gas, it is characterized in that, it is that the low pressure regeneration step of adsorption tower is by making the gas that comprises in the adsorption tower account for 99～20% to the step that atmospheric steam exhaust and product gas clean in to adsorption tower, with comprise the sealing adsorption tower, only open and carry out by product gas to the pipeline that cleans in the adsorption tower and the step of pre-loading accounts for 1～80% mixed gas separation method that constitutes, the outlet oxygen concentration of the adsorption tower of high pressure absorption is carried out in detection, according to its oxygen concentration set(ting)value, low pressure regeneration is changed automatically.
The 2nd aspect of the present invention is a kind of nitrogen separation device that has used the separation method of this mixed gas.In addition, the 3rd aspect of the present invention is a kind of nitrogen consume system that has made up described nitrogen separation device and nitrogen consumer unit.
The present invention changes low pressure regeneration by the outlet oxygen concentration set(ting)value according to adsorption tower automatically, and a kind of method of cost-effective separating mixed gas can be provided.Utilize method of the present invention,, can implement cost-effective PSA mode because the unstripped gas scale of construction of consumption reduces.In addition, owing to can avoid product superfluous purity to occur, few to the influence of nitrogen consumer device, so have big industrial applicability.
The invention embodiment
In mixed gas separation method of the present invention, be filled with molecular-sieve carbon in the adsorption tower.Molecular-sieve carbon is the ultramicropore of a kind of existence 3～5 , with the charcoal of fine pore unanimity, coal, coke, Exocarpium cocois (Cocos nucifera L), resin, pitch etc. is raw material, carries out the gas sorbing material of the carbonaceous material such as wooden system, coal measures, resin system, pitch system of carbonization manufacturing through the pore adjustment at high temperature.
Use described molecular-sieve carbon, adopt the PSA method, can from nitrogen be the mixed gas of main component separation of nitrogen as product gas.In the separation method of mixed gas of the present invention, in at least 2 adsorption towers, fill molecular-sieve carbon, adding a supply of depressing in adsorption tower is the unstripped gas of principal constituent with nitrogen, carry out high pressure absorption, adsorption tower after absorption finishes carries out desorb in low pressure, alternately repeat high pressure absorption and low pressure regeneration at each adsorption tower, nitrogen is separated as product gas.
The unstripped gas that the present invention uses is a kind of with the gas of nitrogen as main component, common in the specific examples of described unstripped gas have an air, but so long as be main component with nitrogen, the gas that can utilize the PSA mode to implement is even it is also harmless to contain other gas such as carbonic acid gas.Wherein said principal constituent be meant 50 volume % or more than.
As previously mentioned, the taking-up amount one with product gas in the PSA mode of existing filling molecular-sieve carbon is decided to be the basis, even the taking-up amount of product gas reduces, the minimizing of required drive is also very little.When the taking-up amount of product gas reduces, under the required drive of the best, control the PSA mode cost-effectively, be called and turn down (turndown) control, the present invention relates to a kind of described improvement of turning down control.At first, taking-up amount and semi-period time relation when often taking out nitrogen with certain purity are described.
Fig. 3 is expression product nitrogen gas flow (Nm
3/ h) and an example of the relation of time semi-period (second).It is 60 seconds for example, with 100Nm with time semi-period
3When/h took out the nitrogen of product nitrogen gas purity 99.99% (oxygen concentration 100ppm), when the semi-period time lengthening was 120 seconds, the nitrogen that then obtains same purity was about 60Nm
3/ h.The oxygen concentration of adsorption tower outlet at this moment changes in time as shown in Figure 4.The part of feature the most of the present invention is, is conceived to the variation of the oxygen concentration in the outlet of this adsorption tower, switches adsorption tower when reaching the oxygen concentration of setting, and time semi-period is automatically changed, and can turn down more effectively like this.
In addition, molecular-sieve carbon process in time, the characteristic that has absorption property to change significantly, when the product nitrogen tolerance of taking-up changed in time semi-period significantly, nitrogen gas purity reduced for the moment sometimes.Thereby utilize flow detector to detect the momentary value of nitrogen flow, and detect the highest momentary value in time semi-period, determine time semi-period.In addition, detect new maximum in time semi-period, through to time semi-period that should momentary value the time, finish adsorption step or desorption procedure at once, change next step over to.By carrying out momentary value and the control of time semi-period, can not reduce nitrogen gas purity, continuous operation like this according to nitrogen flow.Under the situation of separation of nitrogen, use Fig. 1 to more specifically describe the present invention as unstripped gas use air.
Fig. 1 is in the existing P SA mode of Fig. 2 explanation in front, newly establishes oxygen densitometer 20 in the adsorption tower outlet, and flow detectors such as use traffic meter are turned down an example of product gas flow.Unstripped gases such as air utilize compressor 2 from 1 pressurization of unstripped gas supply-pipe, after utilizing water cooler 3 to be cooled to about normal temperature, enter adsorption tower 4 by valve 7, utilize the molecular-sieve carbon of filling, nitrogen that is separated into the oxygen, carbon dioxide etc. of easy absorption and is difficult to adsorb etc., isolating nitrogen is via valve 12, in case after being stored in the product storage tank 6, just can consume.
In the separation method of mixed gas of the present invention, the low pressure regeneration step of adsorption tower is by following formation: make the gas that comprises in the adsorption tower account for 99～20% to the step that atmospheric steam exhaust and product gas clean in to adsorption tower, with comprise the sealing adsorption tower, only open and carry out the step of the pipeline pre-loading that cleans in the adsorption tower being accounted for 1～80% by product gas.
Usually, in the regeneration step of PSA mode, emit in succession in order to make the gas of unstripped gas in atmospheric steam exhaust and cleaning adsorption tower in the adsorption tower, vapor pipe 18, vent valve 8 or 11 are just being opened so.The present invention shortens open hour of this vapor pipe 18, vent valve 8 or 11 in accounting for 99～20% scope of regeneration step (steps A), with remaining 1～80% as not emitting the gas that cleans in the adsorption tower, and the pre-loading step (step B) that adsorption tower is boosted.Just, in step B, only will carry out product gas places open state to the pipe (being equivalent to have among Fig. 1 the pipeline of aperture 15) that cleans in the adsorption tower.When setting control, implement the PSA method like this, can not reduce nitrogen gas purity thus and improve the yield of product gas.
Fig. 5 is under the situation of 2 adsorption towers, the operating process of each adsorption tower.Among Fig. 5, the operation of the 1st adsorption tower when being air with unstripped gas describes.When the 1st adsorption tower 4 is adsorbed state, utilize compressor 2 air pressurized by water cooler 3, be supplied to the 1st adsorption tower 4 by valve 7.At this adsorption of oxygen, nitrogen is by valve 12, as product stock in product storage tank 6.Valve 10,9,14,13 is in closing state, and valve 7,12 is in opened state.Valve 11 becomes closing state from opened state.In addition, flow into the 2nd adsorption tower 5, in the flushing adsorption tower from the product nitrogen gas in hole 15.
Then, open valve 14 and 9, the 1st and the 2nd adsorption tower is communicated with, carry out all pressures of two adsorption towers.Reclaim forced air by this step, in Fig. 5, remember into recovery.Afterwards, the 1st adsorption tower is regenerated.In the regeneration step of the 1st adsorption tower, in steps A, valve 7,9,14,12,11 is in closing state, and valve 10,13,8 is in opened state.Then, flow in the 1st adsorption tower 4, in the flushing adsorption tower from the product nitrogen gas in hole 15.In step B, shut-off valve 8.Open valve 14 and 9 then, be communicated with the 1st and the 2nd adsorption tower, two adsorption towers are all pressed.Repeat this operation later on termly, make nitrogen continuously.
Fig. 6 is the line chart of the interior pressure change of each adsorption tower in the above operation of expression, Fig. 7 is that expression makes the low pressure regeneration step of adsorption tower can't help to comprise the step that the gas in the adsorption tower cleans in to adsorption tower to atmospheric steam exhaust and product gas, with comprise the sealing adsorption tower, product gas is to the step of cleaning in the adsorption tower and the line chart of the pressure change in the adsorption tower of the existing mode that constitutes.As Fig. 6 and Fig. 7 explanation, when adsorption step was converted to regeneration step, the another one adsorption tower utilized pre-loading to improve the pressure of adsorption tower, thereby can shorten the recovery time of forced air at an adsorption tower.Particularly in large-scale plant, because the time decreased that the air compressor of the forced air that produces unstripped gas is turned round under no load condition, often discovery improves the effect of product gas yield.
In addition, improve adsorptive pressure by carrying out pre-loading, when product nitrogen gas purity improved, the pressure of nitrogen storage tank also raise, so the supply pressure of product gas also may improve.
In the separation method of mixed gas of the present invention, the oxygen concentration in the exit of adsorption tower constantly detects with oxygen densitometer 20, according to the set(ting)value of oxygen concentration, low pressure regeneration is automatically changed.In fact, make it from oxygen densitometer 20 output direct signals, perhaps reach the signal of set(ting)value from the instrument output that obtains the oxygen densitometer signal, the sequencer that the signal input control valve of output is switched etc. carry out the switching of regeneration step and adsorption step.The oxygen concentration of carrying out in the exit of adsorption tower is measured, and considers that cost, answering time postpone the aspect that reduces, and preferably carry out at the position converged of the export pipeline of the medium a plurality of adsorption towers of pipeline that converge at valve 12 and 13.
In the separation method of mixed gas of the present invention, detect the oxygen concentration in the exit of adsorption tower, set(ting)value according to oxygen concentration automatically changes low pressure regeneration, but, when the change of rapid flow takes place, not only controlling according to the outlet oxygen concentration of adsorption tower, and combine by product gas flow and control, is effective.
The adsorption tower that desorb finishes utilizes nitrogen to wash before adsorbing.Cleaning can be as shown in Figure 2, use the nitrogen of adsorption tower outlet by the hole, but preferably as shown in Figure 8, use nitrogen to carry out, can suitably change the purge gas scale of construction from product storage tank 6 by purge gas flow detector 21 such as mass flow control device and T-valve 22.
The nitrogen gas amount of consumption utilizes flow detector 17 constantly to detect momentary value, measures.Be considered to this aspect, preferred use traffic meter is as detecting flow apparatus.In the separation method of mixed gas of the present invention, product nitrogen tolerance utilizes flow detectors such as under meter to measure, according to the amount of this product gas, change the flushing dose of product gas in the low pressure regeneration step automatically, from the energy-saving effect aspect is preferred more to carrying out in the adsorption tower.In the regeneration step, the flow that is applied to the product gas that cleans in the adsorption tower is very few, and cleaning degree is not enough, causes hypoplasia, otherwise, cross energy wastage at most, thus the sorbent material loading level that preferably sets per 1 adsorption tower be 10～100%/minute.
In order to make flushing dose (the purge gas scale of construction) the not grading automatical variation of product gas to carrying out in the adsorption tower, can use the detection purge gas scale of constructions such as above-mentioned mass flow control device, the flow of the product gas that detects according under meter moves mass flow control device etc., changes flushing dose.Change the purgative gas scale of construction, except that the method for using the mass flow control device, also can utilize following method, use valve and hole, many wash tubes are set, according to the valve of this wash tube of product gas amount switch.
Detection is predefined oxygen concentration on oxygen densitometer 20, is termination with the semi-period, at first makes valve 11 be in closing state.During this time, utilize hole 15 that adsorption tower 4 is connected with 5, carry out pre-loading through purge gas.Valve 7 and 12 forms closing condition then, and after carrying out even step, valve 10 and 13 is in open state in case form open at valve 9 and 14, and the adsorption tower 5 of desorb operation termination carries out adsorption operations.In addition, the adsorption tower 4 of absorption termination is decompressed to about normal atmosphere by opening valve 8, makes the desorption of gases such as oxygen that are adsorbed in molecular-sieve carbon, carries out the desorb operation.
When turning down, fixedly under the constant occasion of time semi-period and when making under the occasion of semi-period time fluctuation relatively required drive according to oxygen concentration, effect of the present invention is more obvious.Fig. 9 is expression product nitrogen gas gas flow (Nm
3/ h) and consume the figure of electric power (kWH) relation, for example make product flow from 64Nm
3/ hr is reduced to 30Nm
3During/hr, utilize method of the present invention to consume electric power as can be known and reduce 37% approximately.Figure 10 is the oxygen concentration in the expression product nitrogen gas gas and the figure of product nitrogen gas discharge relation in addition.Fixedly time semi-period constant, change flow, then oxygen concentration changes significantly, and is relative therewith, utilizes method of the present invention almost not change.
In the separation method of mixed gas of the present invention, when generating ability 100% running of this product gas, the switching cycle that makes this adsorption tower is 30 seconds～120 seconds a molecular-sieve carbon, preferred 100% switching cycle when turning round be 30 seconds or more than.When the generating ability of product gas turns round by 100%, the switching cycle of considering preferably to make adsorption tower from cost and energy aspect is 30 seconds～120 seconds a molecular-sieve carbon, for example is suitable for the adsorption tower switching cycle and is trade(brand)name 1.5GN-H, 1.5GN-S, the 2GN of Network ラ レ ケ ミ カ Le Co., Ltd. system of 60 seconds, 100 seconds, 120 seconds etc.
Figure 11 is the example that the situation of multiple compressors is set.For the air that makes unstripped gas is in pressurized state, use multiple compressors 2～2 and " when carrying out, when the nitrogen usage quantity of utilizing mass flowmeter to detect is lower than certain amount, stop for example 1 compressor in view of the above, carry out air pressurized with 2 compressors.When reducing, even the pressure regulator formula also needs the electric weight of 20～30% degree as the forced air usage quantity of unstripped gas.Set in advance multiple compressors, the minimizing according to using air capacity utilizes pressure regulator to make compressor become no load condition for this reason, or by reducing the operating number of compressor, can measure the minimizing of required drive.And as compressor, use galvanic current is transformed into alternating current, promptly the compressor of inversion control more can be brought into play energy-conservation effect, the preferred use.
The separation method of mixed gas of the present invention is preferred for the nitrogen separation device, and this nitrogen separation device and nitrogen gas consumer unit cooperate, and is preferably used as the nitrogen gas consume system and uses.The nitrogen gas consume system can be 1 of a nitrogen gas tripping device, and 1 or many of nitrogen gas consumer unit also can be many of nitrogen gas tripping devices, and many of nitrogen gas consumption device are all preferably used.With these example moudle types be shown among Figure 12 and Figure 13.Described nitrogen gas consume system is preferably as soldering welding plant use automatically.
Figure 14 is as the nitrogen gas consumer unit, and the example of many automatic soldering welding plant situations is set.Automatically the soldering welding plant itself is known, but as the present invention, and when a plurality of automatic soldering welding plant was set, even the operating number of soldering welding plant changes automatically, the change of its product nitrogen gas gas purity was also very little.Utilize embodiment to more specifically describe the present invention below.
Embodiment 1
The Exocarpium cocois (Cocos nucifera L) that use is filled with Network ラ レ ケ ミ カ Le Co., Ltd. system is the system PSA of Network ラ レ ケ ミ カ Le Co., Ltd. unit R K-22i (the sorbent material volume 0.248m of molecular-sieve carbon 1.5GN-H
3/ tower) and made up the PSA tripping device of コ ベ Le コ system inversion compressor VS410AD-H, set nitrogen gas purity 99.99% (oxygen concentration 100ppm).The mensuration of the outlet oxygen concentration of adsorption tower is used the oxygen densitometer of Off ジ Network ラ Co., Ltd. system as shown in Figure 1 at the position that export pipeline converges.In addition the flushing dose in the regeneration step be 30% of quantity of sorbent/minute.
100% running ability the during nitrogen gas purity 99.99% of this device is 30Nm
3/ hr, the switching cycle of the molecular-sieve carbon of use is approximately 60 seconds.This device that turns round, under adsorptive pressure 0.8MPa with 30Nm
3/ hr obtains the nitrogen gas of purity 99.99%.Wherein regeneration step is, the gas that comprises in the adsorption tower is 60 seconds (98%) to atmospheric exhaust and product gas to the steps A of the cleaning in the adsorption tower, and the step B that comprises pre-loading is 1 second (2% is weak), and consumption electric power is 26kWH.
Remove nitrogen gas is set at 15Nm
3Outside/hr the running, other and embodiment 1 identical the operation stably obtain the nitrogen of purity 99.99%.At this moment time semi-period is approximately 150 seconds.Wherein regeneration step is, the gas that comprises in the adsorption tower is 60 seconds (40%) to atmospheric exhaust and product gas to the steps A of the cleaning in the adsorption tower, and the step B that comprises pre-loading is 90 seconds (60%), and consumptions electric power is 17kWH, significantly reduction.
Embodiment 3
Remove the amount utilize flow measurement fixed output quota product gas, for a change flushing dose and prepare 2 flushing doses be 15% of sorbing material amount/minute wash tube, become 15Nm at nitrogen gas one
3Below/the hr, control and outside turning round with regard to the mode that becomes 1 wash tube, other and embodiment 2 carry out same operation, and time semi-period is approximately 160 seconds.Wherein regeneration step is, the gas that comprises in the adsorption tower is 60 seconds (38%) to atmospheric exhaust and product gas to the steps A of the cleaning in the adsorption tower, and the step B that comprises pre-loading is 100 seconds (62%), and consumptions electric power is 16kWH, further minimizing.
Embodiment 4
Remove nitrogen gas is set at 10Nm
3Outside/hr the running, other and embodiment 1 carry out same operation, stably obtain the nitrogen of purity 99.99%.At this moment time semi-period is approximately 300 seconds.Wherein regeneration step is, the gas that comprises in the adsorption tower is 60 seconds (20%) to atmospheric exhaust and product gas to the steps A of the cleaning in the adsorption tower, and the step B that comprises pre-loading is 240 seconds (80%), and consumption electric power is 15kWH.
Remove nitrogen gas is set at 25Nm
3Outside/hr the running, other and embodiment 1 carry out same operation, and time semi-period is approximately 75 seconds.Wherein regeneration step is, the gas that comprises in the adsorption tower is 70 seconds (93%) to atmospheric exhaust and product gas to the steps A of the cleaning in the adsorption tower, and the step B that comprises pre-loading is 5 seconds (7% is weak), and consumption electric power is 23kWH.
Comparative example 1
Remove nitrogen gas is set at 0Nm
3Outside/hr the running, other and embodiment 1 carry out same operation, and time semi-period is approximately 600 seconds.Wherein regeneration step is, the gas that comprises in the adsorption tower is 60 seconds (10%) to atmospheric exhaust and product gas to the steps A of the cleaning in the adsorption tower, the step B that comprises pre-loading is 540 seconds (90%), consumption electric power is reduced to 13kWH, but, under this condition when 0 increases the product gas amount, the purity of product gas is unstable for a long time.
Comparative example 2
The Exocarpium cocois (Cocos nucifera L) that use is filled with Network ラ レ ケ ミ カ Le Co., Ltd. system is the system PSA of the Network ラ レ ケ ミ カ Le Co., Ltd. unit R K-22 of molecular-sieve carbon 1.5GN-H, there is コ ベ Le コ to make the PSA tripping device of compressor SG370AD-H with combination, taking-up amount according to product gas, when the switching cycle of change adsorption tower turns round automatically, under adsorptive pressure 0.8MPa, with 30Nm
3/ hr obtains the nitrogen of purity 99.99%.Nitrogen is being set at 10Nm
3When/hr turned round, the purity of nitrogen was that quality is too high more than 99.99%, considers cost, and this is ideal results not necessarily.The nitrogen gas amount is 30Nm
3/ hr and 10Nm
3Consumption electric power during/hr is respectively 26kWH, 22kWH.
Comparative example 3
Use identical device with embodiment 1, only nitrogen gas is set at 15Nm with steps A (not carrying out pre-loading)
3/ hr and turning round implements regeneration step thus.Time semi-period is approximately 150 seconds, and consumption electric power is 17kWH.But product gas purity is that quality is too high more than 99.99%, considers not necessarily ideal results of cost.
Embodiment 6
Except that use has the Exocarpium cocois (Cocos nucifera L) that is filled with Network ラ レ ケ ミ カ Le Co., Ltd. system is adsorption tower (the sorbent material volume 0.358m of molecular-sieve carbon 1.5GN-S
3/ tower) Network ラ レ ケ ミ カ Le Co., Ltd. system PSA unit and combination have outside the PSA tripping device of コ ベ Le コ system contravariant compressor VS410AD-H, and other and embodiment 1 carry out identical operations.100% running ability the during nitrogen gas purity 99.99% of this device is 30Nm
3/ hr, the switching cycle of the molecular-sieve carbon of use is approximately 100 seconds.This device that turns round is under adsorptive pressure 0.8MPa, with 30Nm
3/ hr obtains the nitrogen of purity 99.99%.Wherein regeneration step is, the gas in the adsorption tower is 100 seconds (99%) to atmospheric exhaust and product gas to the steps A that the cleaning in the adsorption tower constitutes, and the step B that pre-loading constitutes is 1 second (1%), and consumption electric power is 25kWH.
Embodiment 7
Except that use has the Exocarpium cocois (Cocos nucifera L) that is filled with Network ラ レ ケ ミ カ Le Co., Ltd. system is adsorption tower (the sorbent material volume 0.446m of molecular-sieve carbon 2GN
3/ tower) Network ラ レ ケ ミ カ Le Co., Ltd. makes the PSA unit and has made up outside the PSA tripping device of コ ベ Le コ system contravariant compressor VS410AD-H, and other and embodiment 1 carry out identical operations.100% running ability the during nitrogen gas purity 99.99% of this device is 30Nm
3/ hr, the switching cycle of the molecular-sieve carbon of use is approximately 120 seconds.This device that turns round is under adsorptive pressure 0.8MPa, with 30Nm
3/ hr obtains the nitrogen of purity 99.99%.Wherein regeneration step is, the gas in the adsorption tower is 118 seconds (98%) to atmospheric exhaust and product gas to the steps A that the cleaning in the adsorption tower constitutes, and the step B that pre-loading constitutes is 2 seconds (2%), and consumption electric power is 26kWH.
Embodiment 8
To the nitrogen separation device of embodiment 1, connect 2 per 1 consumption 15Nm
3The nitrogen consumer unit of the nitrogen gas of/hr turns round, and in addition carries out identical operations with embodiment 1, when no matter the running number of nitrogen gas consumption device is 1 or 2 the time, can supply with the stable nitrogen gas of purity.
Embodiment 9
2 in the nitrogen separation device of embodiment 1 and per 1 consumption 15Nm
34 of the nitrogen consumer unit of the nitrogen gas of/hr connect, and turn round, and in addition carry out identical operations with embodiment 1, even under the situation of the running number of nitrogen gas consumer unit change, also can supply with the stable nitrogen gas of purity.
To the nitrogen separation device of embodiment 1, connect 2 per 1 consumption 15Nm
3The automatic soldering welding plant of the nitrogen gas of/hr, turn round, in addition, other and embodiment 7 carry out identical operations, no matter automatically the running number of soldering welding plant is under 1 the situation still under 2 the situation, can supply with the stable nitrogen gas of purity.Soldering quality of welded in addition is stable, is not pinpointing the problems aspect the quality of product.
The possibility of utilizing on the industry
Utilize the present invention, can according to the oxygen concentration setting value of adsorption tower outlet, automatically change low pressure again Give birth to, the cost-effectively method of separating mixed gas is provided. Method of the present invention is because the raw material gas of consumption Amount reduces, and can implement cost-effectively the PSA mode, is preferably applied to heat treatment, the semiconductor of metal Make etc., particularly automatic solder welder.
Description of drawings
Fig. 1 is an example of PSA device flow process of the present invention.
Fig. 2 is the flow process of existing P SA device.
Fig. 3 is the figure of expression time semi-period and product nitrogen gas gas flow relation.
Fig. 4 is the figure that expression adsorption tower outlet oxygen concentration changes.
The operating process of the adsorption tower when Fig. 5 is 2 adsorption towers of expression.
Fig. 6 is the line chart of expression by the pressure change of adsorption tower of the present invention.
Fig. 7 is the line chart of expression by the pressure change of the adsorption tower of existing P SA mode.
Fig. 8 is the flow process of the other scheme of expression cleaning.
Fig. 9 is expression product nitrogen gas gas flow and consumes the figure of the relation of electric power.
Figure 10 is the figure of the relation of the oxygen concentration in expression product nitrogen gas flow and the product nitrogen gas gas.
Figure 11 is the example that the flow process of multiple compressors is set.
Figure 12 is 1 nitrogen gas tripping device, the module map of the nitrogen gas consume system of many nitrogen gas consumer unit formations.
Figure 13 is many nitrogen gas tripping devices, the module map of the nitrogen gas consume system of many nitrogen gas consumption device formations.
Figure 14 is provided with the example of many automatic soldering welding plants as the flow process of nitrogen gas consumption device.
Nomenclature
1 unstripped gas supply-pipe
2 compressors
2 ' compressor
2 ' compressor
3 water coolers
4 adsorption towers
5 adsorption towers
6 product storage tanks
7～14 valves
15 holes
15 ' hole
16 oxygen densitometers
17 flow rate-measuring devices
18 vapor pipes
19 product gas take-off pipes
20 oxygen densitometers
21 purge gas flow detectors
22 T-valve
23～24 valves
Claims (10)
1. the separation method of a mixed gas, it is characterized in that, depress adding, to be that the unstripped gas of main component is supplied to 1 at least 2 adsorption towers that are filled with molecular-sieve carbon with nitrogen, carry out high pressure absorption, adsorption tower after absorption finishes carries out low pressure regeneration, in each adsorption tower, alternately repeat high pressure absorption and low pressure regeneration, in the separation method of nitrogen as the isolating mixed gas of product gas, it is that the low pressure regeneration step of adsorption tower is according to making the gas that comprises in the adsorption tower account for 99～20% to the atmospheric steam exhaust and the step of cleaning in to adsorption tower by product gas, with comprise the sealing adsorption tower, only open and carry out the step of the pre-loading of the pipeline that cleans in the adsorption tower being accounted for 1～80% mixed gas separation method that constitutes by product gas, the outlet oxygen concentration of the adsorption tower of high pressure absorption is carried out in detection, according to the set(ting)value of its oxygen concentration, low pressure regeneration is changed automatically.
2. as the separation method of the mixed gas of claim 1 record, wherein carry out at the position converged of the export pipeline that is determined at a plurality of adsorption towers of this outlet oxygen concentration.
3. as the separation method of claim 1 or 2 mixed gass of putting down in writing, wherein the amount of this product gas utilizes under meter to measure, and according to the amount of this product gas, changes automatically in the low pressure regeneration step by the flushing dose in the adsorption tower of product gas.
4. as the separation method of the mixed gas of any one record of claim 1～3, wherein used and made when the generating ability of this product gas is 100% running, the switching cycle of this adsorption tower is 30 seconds～120 seconds a molecular-sieve carbon, and the switching cycle in 100% when running be 30 seconds or more than.
5. as the separation method of the mixed gas of any one record of claim 1～4, wherein, the compressor of this unstripped gas of pressurizeing is a kind of compressor of inversion control, according to the taking-up amount of product gas the working rate of this compressor is automatically changed.
6. use the nitrogen separation device of separation method of the mixed gas of claim 1～5 record.
7. with described nitrogen separation device of claim 6 and the combined nitrogen consume system of nitrogen consumer unit.
8. as the nitrogen consume system of claim 7 record, wherein, this nitrogen separation device is 1, and this nitrogen consumer unit is 1 or many.
9. as the nitrogen consume system of claim 7 record, wherein, this nitrogen separation device is many, and this nitrogen consumer unit is many.
10. as the nitrogen consume system of any one record of claim 7～9, wherein, this nitrogen consumer unit is automatic soldering welding plant.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP53670/2004 | 2004-02-27 | ||
| JP2004053670 | 2004-02-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1660468A true CN1660468A (en) | 2005-08-31 |
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ID=35010199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410059563 Pending CN1660468A (en) | 2004-02-27 | 2004-05-31 | Separating method of mixed gas,nitrogen separator and its consumption system |
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| Country | Link |
|---|---|
| CN (1) | CN1660468A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351156A (en) * | 2011-07-28 | 2012-02-15 | 湖南科技大学 | Sulfuric acid plant production device without discharge of tail gas and process method therefor |
| CN104057208A (en) * | 2013-03-21 | 2014-09-24 | 吴宁 | Multifunctional welding machine |
| CN105073225A (en) * | 2013-02-15 | 2015-11-18 | 皇家飞利浦有限公司 | Oxygen separator and method of generating oxygen |
-
2004
- 2004-05-31 CN CN 200410059563 patent/CN1660468A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351156A (en) * | 2011-07-28 | 2012-02-15 | 湖南科技大学 | Sulfuric acid plant production device without discharge of tail gas and process method therefor |
| CN102351156B (en) * | 2011-07-28 | 2013-03-27 | 湖南科技大学 | Sulfuric acid plant production device without discharge of tail gas and process method therefor |
| CN105073225A (en) * | 2013-02-15 | 2015-11-18 | 皇家飞利浦有限公司 | Oxygen separator and method of generating oxygen |
| CN105073225B (en) * | 2013-02-15 | 2017-12-26 | 皇家飞利浦有限公司 | Oxygen separator and the method for producing oxygen |
| US9873078B2 (en) | 2013-02-15 | 2018-01-23 | Koninklijke Philips N.V | Oxygen separator and method of generating oxygen |
| CN104057208A (en) * | 2013-03-21 | 2014-09-24 | 吴宁 | Multifunctional welding machine |
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