CN101318635A - Process and apparatus for producing high-purity nitrogen gas - Google Patents
Process and apparatus for producing high-purity nitrogen gas Download PDFInfo
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- CN101318635A CN101318635A CNA200810123298XA CN200810123298A CN101318635A CN 101318635 A CN101318635 A CN 101318635A CN A200810123298X A CNA200810123298X A CN A200810123298XA CN 200810123298 A CN200810123298 A CN 200810123298A CN 101318635 A CN101318635 A CN 101318635A
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Abstract
The invention discloses a method for preparing high-purity nitrogen gas, and the method comprises the following steps: 1) at least one layer of gas separation membrane which allows the preferential permeation of oxygen and water vapor is used for separating the raw gas containing nitrogen gas and oxygen into a non-permeating gas with the nitrogen gas content over 95 per cent and a permeating gas with rich oxygen and water vapor; 2) the non-permeating gas is caused to contact an adsorbent from the lower part of the adsorbent and export the high-purity nitrogen gas with a nitrogen gas content of 99.99 percent from the top of the adsorbent, the adsorbent is an adsorbent which can selectively absorb oxygen and water vapor. The invention also discloses a device required for implementing the method. By adopting the method, the high-purity nitrogen gas can be produced at low cost; the method has the advantages of easy implementation, convenient and economical modification of the equipment.
Description
Technical field
The present invention relates to a kind ofly from the mixed gas based on nitrogen oxygen of air and so on, isolate the method for high-purity nitrogen, and a kind of preparation facilities that is used to implement this method.
Background technology
Nitrogen extensively is applied to fields such as the storage transportation of oil well protection, tertiary oil recovery, gas displacement, electronics manufacturing, Metal smelting or processing, various explosive substances and food fresh keeping as rare gas element.Airborne a nitrogen content is about 78%, isolates nitrogen from air, is the main method for preparing nitrogen in the world always.
The most frequently used nitrogen method of producing has Deep Cooling Method, transformation absorption (PSA) technology and gas membrane Seperation Technology at present.
Utilize cryogenic unit can be easy to obtain purity and be higher than 99.999% high pure nitrogen, but its energy consumption height, and plant investment is huge, has only when the nitrogen flow demand is big, utilizes deep cooling legal system nitrogen that economy is just arranged.
Present domestic application pressure swing adsorption can be produced the nitrogen more than 99.99%, along with industrial sectors such as electronics, metallurgy are more and more higher to the purity requirement of nitrogen, the performance that is limited to sorbent material, if expect the nitrogen that purity is higher, must increase the quantity of sorbent material, and then container dimensional is strengthened, and also increase greatly thereupon of air consumption, these factors have all limited pressure swing adsorption in the application of producing on the high pure nitrogen.
About gas membrane Seperation Technology, have document (Xu Renxian. present situation and future that gas separation membrane is used. membrane science and technology .2003) point out, utilize this method can prepare purity and reach 99.5% nitrogen, but if wish further to obtain the higher nitrogen of purity, the performance that is limited to present mould material, must increase membrane area, or improve air pressure, and then construction cost and process cost are increased.
In the prior art, also have PSA operation and gas membrane Seperation Technology are in series, in order to carrying out the isolating patent documentation of nitrogen oxygen (CN200580026452.6), but the special emphasis of this technology is that the nitrogen that it makes and the purity of oxygen are all not high to the collection that walks abreast of nitrogen and oxygen.In the step of membrane sepn, what this patent adopted is negative-pressure operation, and its unstripped gas is the parsing gas of transformation absorption, and pressure is lower.But this operates in when being used to remove minimum gas (such as the preparation high-purity nitrogen), will become very uneconomical.If want that preparing purity by the described method of this patent is higher than 99.99% nitrogen, must be cost to sacrifice equipment size and to increase cost of investment.
Summary of the invention
It is raw material that one of goal of the invention of the present invention is to provide a kind of mixed gas based on nitrogen oxygen with air and so on, therefrom isolates the method for high-purity nitrogen economically.
To achieve the above object of the invention, the present invention has taked following technical scheme:
A kind of preparation method of high-purity nitrogen comprises following steps successively:
(1), membrane type gas delivery: utilize one deck gas separation membrane at least, the unstripped gas that will comprise nitrogen and oxygen and air pressure and be 0.7～1.0Mpa be separated into permeability coefficient relative less non-see through gas and permeability coefficient relatively large see through gas, the described non-content of nitrogen in the gas that sees through is greater than 95%;
(2), pressure change adsorption type gas delivery: make the described non-gas that sees through contact with the sorbent material of adsorption of oxygen and water vapour optionally, derivation a nitrogen content is higher than 99.99% high-purity nitrogen.
Described unstripped gas is through the air after dedusting and the oil removing.
Described gas separation membrane is the polymeric membrane that can make the tubular fibre structure of oxygen, water vapour, carbonic acid gas penetrated preferably.Described sorbent material is a carbonaceous molecular sieve.
After finishing described step (2), make described sorbent material be lower than 2 * 10 at air pressure
3Resolve and derive parsing gas under the state of Pa, described parsing gas is imported in the described step (1) carry out circular treatment.
Another goal of the invention of the present invention is to provide a kind of preparation facilities that is used to implement the high-purity nitrogen of technique scheme.
To achieve the above object of the invention, the present invention has taked following technical scheme:
A kind of preparation facilities of high-purity nitrogen, this preparation facilities comprise membrane type gas separator and pressure change adsorption type gas separator.Described membrane type gas separator comprises: at least 1 grade of gas separation membrane that can make oxygen, water vapour, carbonic acid gas penetrated preferably; Be opened in the unstripped gas inlet and the non-pneumatic outlet that sees through of a side of described gas separation membrane; Be opened in described gas separation membrane opposite side see through pneumatic outlet.Described pressure change adsorption type gas separator comprises: enter the mouth with the described non-adsorbed gas for the treatment of that is connected through pneumatic outlet; The high-purity nitrogen outlet; The bottom treats that with described adsorbed gas inlet is connected, the top exports at least 1 pair of adsorption tower that is connected with described high-purity nitrogen, is filled with the sorbent material of energy preferentially adsorbed oxygen and water vapour in described adsorption tower.
Described preparation facilities also comprises surge tank, an end of this surge tank with describedly non-ly see through that pneumatic outlet is connected, the other end treats that adsorbed gas enters the mouth and is connected with described.
Described preparation facilities also comprises at least one vacuum pump, and the inlet end of this vacuum pump is connected with described adsorption tower, exhaust side is connected with described unstripped gas inlet.
Described preparation facilities also comprises:
First pipe connecting that the bottom of 2 adsorption towers in per 1 pair of described adsorption tower is interconnected;
Second pipe connecting that is in parallel and is provided with described first pipe connecting;
The 3rd pipe connecting that the top of 2 adsorption towers in per 1 pair of described adsorption tower is interconnected;
Be arranged on first switch-valve and second switch valve on described first pipe connecting with being in series;
Be arranged on the 3rd switch-valve and the 4th switch-valve on described second pipe connecting with being in series;
Be arranged on the 5th switch-valve and the 6th switch-valve on described the 3rd pipe connecting with being in series;
The 7th switch-valve, an end of the 7th switch-valve are connected to the described non-pneumatic outlet, the other end of seeing through and are connected on first pipe connecting between described first switch-valve and the described second switch valve;
The 8th switch-valve, an end of the 8th switch-valve are connected to the outlet of described high-purity nitrogen, the other end and are connected on the 3rd pipe connecting between described the 5th switch-valve and described the 6th switch-valve,
The inlet side that the inlet end of described vacuum pump is connected on second pipe connecting between described the 3rd switch-valve and described the 4th switch-valve, exhaust side is connected to described membrane module.
Described gas separation membrane is the polymeric membrane that can make the tubular fibre structure of oxygen, water vapour, carbonic acid gas penetrated preferably, and described sorbent material is a carbonaceous molecular sieve.
Preparation method and preparation facilities according to high-purity nitrogen of the invention process have following advantage:
1, before pressure change adsorption type gas delivery step, carry out the membrane type gas delivery of a positive pressure operation earlier, can be more economically a nitrogen content of about 75% in the air be concentrated to 95%～99.5%, greatly reduce the running load of follow-up pressure change adsorption type gas separator, the quantity of required sorbent material is obviously reduced, also reduced plant construction expense and floor space.
2, because sorbent material is particularly responsive to moisture,, could feed in the adsorption tower so the water content of unstripped gas is reduced in the acceptable scope of sorbent material.Gas separation membrane can together be removed moisture and oxygen when condensed nitrogen, thus the effect of playing the protection sorbent material, prolonging its work-ing life.
3, only need pressure change adsorption type gas separator of the prior art is transformed, set up the membrane module of one-level at least in its ingress as required, can obtain disclosed preparation facilities among the present invention, reequip with low cost.The also transformation of the outmoded pressure change adsorption type gas separator of decaying to some extent applicable to performance, or be used to promote its serviceability makes things convenient for to such an extent that make the higher nitrogen of purity.
Description of drawings
Accompanying drawing 1 is a device synoptic diagram of the present invention.
Wherein: 1, membrane type gas separator; 10, membrane module; 11, gas separation membrane; 12, unstripped gas inlet; 13, non-through pneumatic outlet, 14, through pneumatic outlet; 2, pressure change adsorption type gas separator; 20, adsorption tower; 21, treat the adsorbed gas inlet; 22, high-purity nitrogen outlet; 3, surge tank; 4, vacuum pump; 101, first pipe connecting; 102, second pipe connecting; 103, the 3rd pipe connecting; 201, first switch-valve; 202, second switch valve; 203, the 3rd switch-valve; 204, the 4th switch-valve; 205, the 5th switch-valve; 206, the 6th switch-valve; 207, the 7th switch-valve; 208, the 8th switch-valve.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described:
As shown in Figure 1, comprise membrane type gas separator 1 and pressure change adsorption type gas separator 2 according to high-purity nitrogen preparation facilities of the invention process.
Wherein, membrane type gas separator 1 is made up of 3 membrane modules 10 that adopt the one-level parallel way to be provided with, and is provided with the gas separation membrane 11 that oxygen and vapor permeation are crossed in this membrane module 10.Membrane module 10 is selected the PPA type gas film separation assembly of Bai Meiya (China) company limited for use, and the specified nitrogen flow of every membrane module 10 is 10Nm
3/ hr, under this flow, this membrane module 10 can be concentrated into nitrogen 99% concentration.
At the inlet side of membrane module 10 unstripped gas inlet 12 and the non-pneumatic outlet 13 that sees through are set, see through pneumatic outlet 14 in the side setting that sees through of membrane module 10.Air is carried out dedusting and oil removing, and pressure regulation is sent in the membrane module 10 from described unstripped gas inlet 12 to 1Mpa.The bigger gases of permeability coefficient such as oxygen, water vapour, carbon dioxide, to preferentially penetrate gas separation membrane 11, be disposed to the external world from seeing through pneumatic outlet 14, nitrogen is then relatively slowly concentrated at inlet side gradually because of seepage velocity, sends into the surge tank 3 from non-seeing through in the pneumatic outlet 13 at last.
The effect of surge tank 3 is the non-gas of temporarily accumulating after membrane module 10 concentrates that sees through, with its level pressure constant flow send in the pressure change adsorption type gas separator 2.
Pressure change adsorption type gas separator 2 is made up of 1 pair of adsorption tower 20, is filled with the sorbent material of energy preferentially adsorbed oxygen and water vapour in this adsorption tower 20.The CMS-200 type carbonaceous molecular sieve that sorbent material selects for use rich molecular sieve company limited of Changxing section to produce, the design denitrification production rate is 200Nm
3/ t, numerical evaluation goes out the quality of needed sorbent material thus.
Be provided with in the bottom of adsorption tower 20 by surge tank 3 with non-see through that pneumatic outlet 13 is connected indirectly treat adsorbed gas inlet 21, the top is provided with high-purity nitrogen outlet 22.Non-seeing through in gas is admitted to wherein 1 adsorption tower 20 from the bottom of adsorption tower 20 is moved upward gradually and fully contacts with sorbent material, and the non-oxygen and the water vapour that contain in the gas of seeing through is adsorbed the agent preferentially adsorbed.From the vertical high-purity nitrogens outlet of adsorption tower 20 22 gases of sending is purity up to 99.99% high-purity nitrogen.
The purpose that adsorption tower 20 is set in pairs is for the ease of adsorption tower 20 is resolved.In order to finish analyzing step, in pressure change adsorption type gas separator 2, also be provided with following assembly:
First pipe connecting 101 that the bottom of 1 pair of adsorption tower 20 is interconnected;
Second pipe connecting 102 that is in parallel and is provided with first pipe connecting 101;
The 3rd pipe connecting 103 that the top of 1 pair of adsorption tower 20 is interconnected;
Be arranged on first switch-valve 201 and second switch valve 202 on first pipe connecting 101 with being in series;
Be arranged on the 3rd switch-valve 203 and the 4th switch-valve 204 on second pipe connecting 102 with being in series;
Be arranged on the 5th switch-valve 205 and the 6th switch-valve 206 on the 3rd pipe connecting 103 with being in series;
The 7th switch-valve 207;
The 8th switch-valve 208;
Be used for the vacuum pump 4 that to vacuumize in the adsorption tower 20.
Wherein, an end of the 7th switch-valve 207 is connected with treating adsorbed gas inlet 21, and the other end is communicated between first switch-valve 201 and the second switch valve 202.One end of the 8th switch-valve 208 is connected with high-purity nitrogen outlet 22, and the other end is communicated between the 5th switch-valve 205 and the 6th switch-valve 206.The inlet end of vacuum pump 4 is communicated between the 3rd switch-valve 203 and the 4th switch-valve 204, and exhaust side is communicated to unstripped gas inlet 12.
For the principle that explanation is resolved, carrying out absorption work at this tentative adsorption tower 20 that is positioned at the drawing left side, the adsorption tower 20 on right side is being resolved, and the working order of two towers must be switched now.
At first close the 7th switch-valve 207, the 8th switch-valve 208, the 3rd switch-valve 203, the 4th switch-valve 204, open first switch-valve 201, second switch valve 202, the 5th switch-valve 205, the 6th switch-valve 206, make the top and the bottom of 1 pair of adsorption tower 20 be communicated with respectively, 2 mutual balances of pressure that adsorption tower is interior, this is a pressure equalizing, and this process continues about 2 seconds.
Close first switch-valve 201 and the 5th switch-valve 205 then, and open the 3rd switch-valve 203, even the adsorption tower in left side 20 is connected with vacuum pump 4,4 pairs of these adsorption towers 20 of vacuum pump carry out vacuum pumping, and vacuum tightness is maintained at about 1.5 * 103Pa in the tower.Relative high-purity nitrogen of parsing oxygen content gas that is drawn out of and the non-gas that sees through are than higher, but still much smaller than airborne oxygen level, therefore these are resolved gas and send unstripped gas inlet 12 back to through vacuum pump 4, again participate in circulation, make as the required pressurized air of unstripped gas and significantly reduce, avoid the waste of raw material and energy, also reduced plant investment expense and process cost simultaneously.
Simultaneously, open the 7th switch-valve 207 and the 8th switch-valve 208, make the adsorption tower 20 on right side enter working order, treat that adsorbed gas is from being admitted in this adsorption tower 20 in surge tank 3.
When adsorption tower 20 work on right side finishes need resolve the time, equally at first close the 7th switch-valve 207, the 8th switch-valve 208, the 3rd switch-valve 203, the 4th switch-valve 204, open first switch-valve 201, second switch valve 202, the 5th switch-valve 205, the 6th switch-valve 206 then, all press.The bottom of order left side adsorption tower 20 is communicated with surge tank 3 then, and the bottom of right side adsorption tower 20 is connected with the inlet end of vacuum pump 4, both be said process repeatedly.
All switch-valves are magnetic valve, or are the pneumavalve by solenoid-driven, realize full automatic control by PLC.
Use aforesaid apparatus and method, can the comparatively economic concentration of producing be higher than 99.99% nitrogen.If require to obtain the nitrogen of greater concn, can increase the quantity of membrane module 10 as required, make the non-nitrogen gas concn of from membrane type gas separator 1, sending of gas that sees through greater than 99.5%, and then send into pressure change adsorption type gas separator 2, can make nitrogen gas concn and surpass 99.999% high-purity nitrogen.Same, under less demanding situation, also can reduce the quantity of membrane module 10 to nitrogen gas concn, reduce cost.
As mentioned above, we are illustrated according to aim of the present invention fully, but the present invention is not limited to the foregoing description and implementation method.The practitioner of correlative technology field can carry out different variations and enforcement in the scope of technological thought permission of the present invention.
Claims (10)
1, a kind of preparation method of high-purity nitrogen is characterized in that, comprises following steps successively:
(1), membrane type gas delivery: utilize one deck gas separation membrane at least, the unstripped gas that will comprise nitrogen and oxygen and air pressure and be 0.7～1.0Mpa be separated into permeability coefficient relative less non-see through gas and permeability coefficient relatively large see through gas, the described non-content of nitrogen in the gas that sees through is greater than 95%;
(2), pressure change adsorption type gas delivery: make the described non-gas that sees through contact with the sorbent material of adsorption of oxygen and water vapour optionally, derivation a nitrogen content is higher than 99.99% high-purity nitrogen.
2, the preparation method of high-purity nitrogen according to claim 1 is characterized in that: described unstripped gas is through the air after dedusting and the oil removing.
3, the preparation method of high-purity nitrogen according to claim 1 is characterized in that: described gas separation membrane is the polymeric membrane that can make the tubular fibre structure of oxygen, water vapour, carbonic acid gas penetrated preferably.
4, the preparation method of high-purity nitrogen according to claim 1 is characterized in that: described sorbent material is a carbonaceous molecular sieve.
5, the preparation method of high-purity nitrogen according to claim 1 is characterized in that: after finishing described step (2), make described sorbent material be lower than 2 * 10 at air pressure
3Resolve and derive parsing gas under the state of Pa, described parsing gas is imported in the described step (1) carry out circular treatment.
6, a kind of preparation facilities of high-purity nitrogen is characterized in that: this preparation facilities comprises membrane type gas separator (1) and pressure change adsorption type gas separator (2),
Described membrane type gas separator (1) comprises: at least 1 grade of gas separation membrane (11) that can make oxygen, water vapour, carbonic acid gas penetrated preferably; Be opened in the unstripped gas inlet (12) and the non-pneumatic outlet (13) that sees through of a side of described gas separation membrane (11); Be opened in described gas separation membrane (11) opposite side see through pneumatic outlet (14),
Described pressure change adsorption type gas separator (2) comprises: with described non-see through that pneumatic outlet (13) is connected treat adsorbed gas inlet (21); High-purity nitrogen outlet (22); The bottom treats that with described adsorbed gas inlet (21) is connected, the top exports at least 1 pair of adsorption tower (20) that (22) are connected with described high-purity nitrogen, is filled with the sorbent material of energy preferentially adsorbed oxygen and water vapour in described adsorption tower (20).
7, the preparation facilities of high-purity nitrogen according to claim 6, it is characterized in that: described preparation facilities also comprises surge tank (3), an end of this surge tank (3) with describedly non-ly see through that pneumatic outlet (13) is connected, the other end with described treat adsorbed gas enter the mouth (21) be connected.
8, the preparation facilities of high-purity nitrogen according to claim 6, it is characterized in that: described preparation facilities also comprises at least one vacuum pump (4), and the inlet end of this vacuum pump (4) is connected with described adsorption tower (20), exhaust side is connected with described raw material gas port (12).
9, the preparation facilities of high-purity nitrogen according to claim 8 is characterized in that: described preparation facilities also comprises:
First pipe connecting (101) that the bottom of 2 adsorption towers (20) in per 1 pair of described adsorption tower (20) is interconnected;
Second pipe connecting (102) that is in parallel and is provided with described first pipe connecting (101);
The 3rd pipe connecting (103) that the top of 2 adsorption towers (20) in per 1 pair of described adsorption tower (20) is interconnected;
Be arranged on first switch-valve (201) and second switch valve (202) on described first pipe connecting (101) with being in series;
Be arranged on the 3rd switch-valve (203) and the 4th switch-valve (204) on described second pipe connecting (102) with being in series;
Be arranged on the 5th switch-valve (205) and the 6th switch-valve (206) on described the 3rd pipe connecting (103) with being in series;
The 7th switch-valve (207), an end of the 7th switch-valve (207) are connected to the described non-pneumatic outlet (13), the other end of seeing through and are connected on first pipe connecting (101) between described first switch-valve (201) and the described second switch valve (202);
The 8th switch-valve (208), an end of the 8th switch-valve (208) are connected to described high-purity nitrogen outlet (22), the other end and are connected on the 3rd pipe connecting (103) between described the 5th switch-valve (205) and described the 6th switch-valve (206),
The inlet end of described vacuum pump (4) is connected to the inlet side that second pipe connecting (102) is gone up, exhaust side is connected to described membrane module (10) between described the 3rd switch-valve (203) and described the 4th switch-valve (204).
10, the preparation method of high-purity nitrogen according to claim 6 is characterized in that: described gas separation membrane is the polymeric membrane that can make the tubular fibre structure of oxygen, water vapour, carbonic acid gas penetrated preferably, and described sorbent material is a carbonaceous molecular sieve.
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| CNA200810123298XA CN101318635A (en) | 2008-06-16 | 2008-06-16 | Process and apparatus for producing high-purity nitrogen gas |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344393A (en) * | 2011-06-25 | 2012-02-08 | 杨贻方 | Equipment for producing fertilizers by wind energy |
| CN105399063A (en) * | 2015-12-08 | 2016-03-16 | 山东恒业石油新技术应用有限公司 | Combined high pressure nitrogen purification equipment |
| CN106185844A (en) * | 2016-07-06 | 2016-12-07 | 合肥良骏汽车材料有限公司 | A kind of nitrogen gas generator produced for roof of the vehicle |
| CN106698366A (en) * | 2017-03-15 | 2017-05-24 | 合肥良骏汽车材料有限公司 | Nitrogen generating device used for production of vehicle ceiling |
| CN109941614A (en) * | 2019-05-07 | 2019-06-28 | 广东顺德柏杉电器科技有限公司 | A kind of anaerobic preservation device |
| CN110156016A (en) * | 2019-06-14 | 2019-08-23 | 林千果 | The combined recovery device and method of carbon dioxide in flue gas, nitrogen and oxygen |
| CN110294464A (en) * | 2018-03-23 | 2019-10-01 | 中国石油化工股份有限公司 | High-purity nitrogen generation system and method for nitrogen flooding |
| CN111377417A (en) * | 2020-04-09 | 2020-07-07 | 苏州纳特云端净化设备有限公司 | Nitrogen production intelligent start-stop instant gas supply process |
| CN112498712A (en) * | 2020-12-11 | 2021-03-16 | 中国航空工业集团公司金城南京机电液压工程研究中心 | Combined hollow fiber membrane and molecular sieve machine-mounted oil tank inerting device |
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2008
- 2008-06-16 CN CNA200810123298XA patent/CN101318635A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344393A (en) * | 2011-06-25 | 2012-02-08 | 杨贻方 | Equipment for producing fertilizers by wind energy |
| CN105399063A (en) * | 2015-12-08 | 2016-03-16 | 山东恒业石油新技术应用有限公司 | Combined high pressure nitrogen purification equipment |
| CN106185844A (en) * | 2016-07-06 | 2016-12-07 | 合肥良骏汽车材料有限公司 | A kind of nitrogen gas generator produced for roof of the vehicle |
| CN106698366A (en) * | 2017-03-15 | 2017-05-24 | 合肥良骏汽车材料有限公司 | Nitrogen generating device used for production of vehicle ceiling |
| CN110294464A (en) * | 2018-03-23 | 2019-10-01 | 中国石油化工股份有限公司 | High-purity nitrogen generation system and method for nitrogen flooding |
| CN109941614A (en) * | 2019-05-07 | 2019-06-28 | 广东顺德柏杉电器科技有限公司 | A kind of anaerobic preservation device |
| CN110156016A (en) * | 2019-06-14 | 2019-08-23 | 林千果 | The combined recovery device and method of carbon dioxide in flue gas, nitrogen and oxygen |
| CN111377417A (en) * | 2020-04-09 | 2020-07-07 | 苏州纳特云端净化设备有限公司 | Nitrogen production intelligent start-stop instant gas supply process |
| CN112498712A (en) * | 2020-12-11 | 2021-03-16 | 中国航空工业集团公司金城南京机电液压工程研究中心 | Combined hollow fiber membrane and molecular sieve machine-mounted oil tank inerting device |
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