CN1150964C - Equipment for producing nitrogen gas by using pressure swing adsorption process - Google Patents

Equipment for producing nitrogen gas by using pressure swing adsorption process

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Publication number
CN1150964C
CN1150964C CNB011048573A CN01104857A CN1150964C CN 1150964 C CN1150964 C CN 1150964C CN B011048573 A CNB011048573 A CN B011048573A CN 01104857 A CN01104857 A CN 01104857A CN 1150964 C CN1150964 C CN 1150964C
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China
Prior art keywords
nitrogen
adsorption tower
present
dew point
low
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Expired - Fee Related
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CNB011048573A
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Chinese (zh)
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CN1321536A (en
Inventor
顾飞龙
陈奕峰
张丽华
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Shanghai Research Institute of Chemical Industry SRICI
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Shanghai Research Institute of Chemical Industry SRICI
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Publication of CN1150964C publication Critical patent/CN1150964C/en
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Abstract

The present invention relates to a device for preparing low-dew point nitrogen by pressure swing adsorption, which mainly comprises an air compressor, a cooler, a high efficient oil expeller, a nitrogen-making adsorption tower, a nitrogen buffer tank, a nitrogen storage tank, an automatic control valve, a pipeline, etc. The present invention is characterized in that a drying adsorption tower is arranged between the nitrogen buffer tank and the nitrogen storage tank, and a spare drier is arranged behind the nitrogen storage tank. The device of the present invention can be used for preparing nitrogen whose dew point is below 60 DEG C below zero, the requirements of low dew points and continuous nitrogen supply in the production can be guaranteed, and the present invention has the advantages of compact device, low operation cost, low price of the device and practicality. The present invention can be used for situations of electronic technology, chemical industry, food packing and storage, etc.

Description

The device of transformation absorption preparation nitrogen
The present invention relates to the device that a kind of pressure swing adsorption method prepares nitrogen, particularly a kind of device that adopts the low dew point nitrogen of pressure swing adsorption method preparation.
In prior art, the device that adopts pressure swing adsorption method to prepare nitrogen has multiple, as the rich nitrogen device of the coke molecular sieve of Ruian instrument three factories production, this device adopts the nitrogen producing procedure of pressurization absorption, vacuum desorption, before entering adsorption separation system, passes through air system of non heated regeneration dryer (filling activated alumina or silica gel) in advance, perhaps pass through refrigerant type dryer, be air-dried to earlier to a certain degree, make nitrogen through transformation absorption like this.But this method air-treatment amount is big, and because the compressed air water capacity is big, the tolerance that is consumed during drier regeneration is also big, and equipment investment is also big, and the nitrogen dew point that makes is about-43 ℃.
U.S. Patent Publication a kind of nitrogen-making device, patent No. US4439213.This device adopts the nitrogen producing procedure of pressurization absorption, normal pressure desorb, and the nitrogen dew point that makes is at about-43 ℃ approximately.
But in industrial production, often need to use more dry nitrogen, and existing nitrogen-making device still can not meet the needs of production.
The purpose of this invention is to provide a kind of device that adopts the low dew point nitrogen of pressure swing adsorption method preparation, the nitrogen that this device is produced can reach dew point below-60 ℃.
The present invention realizes like this.The device of transformation absorption preparation nitrogen of the present invention, mainly comprise air compressor, cooler, efficient degreasing device, two compositions such as system nitrogen adsorption tower, nitrogen buffer tank, dry adsorption tower, nitrogen basin, autocontrol valve and pipeline, described dry adsorption tower has 2~4, and 2 dry adsorption towers are preferably arranged.
The device of transformation absorption preparation nitrogen of the present invention is filled with 4A or 13X zeolite molecular sieve in the described dry adsorption tower.Drying mode is the heatless regeneration drying mode.
The device of transformation of the present invention absorption preparation nitrogen also is provided with standby drier, guarantees the continuity and the high reliability of low dew point nitrogen supply (NS) when preventing that dry adsorption tower from breaking down.Standby drier is filled with 4A or 13X zeolite molecular sieve equally.
The technical process of the low dew point nitrogen of device preparation of transformation absorption preparation nitrogen of the present invention is: raw air is compressed to 0.6~0.8MPa through air compressor, remove through the efficient degreasing device again and deoil, to enter in the system nitrogen adsorption tower of two filling carbon molecular sieves behind water and the dust, airborne oxygen, carbon dioxide and moisture are adsorbed agent and select absorption, absorbed component (being mainly nitrogen) does not then flow out from the adsorption tower port of export, enters nitrogen buffer tank.Afterwards, normal pressure is all pressed, is decompressed to adsorption tower, removes the impurity composition of absorption, finishes the regeneration of adsorbent.Raw air is sent in two adsorption tower alternate cycles operations continuously, continuous output nitrogen, and the nitrogen dew point that makes is-43 ℃, and promptly water content is about 100ppm, and purity is 98~99.9%, pressure 0.6MPa.Wish to get further low dew point nitrogen ,-43 ℃ the nitrogen that need will make is further dry.The nitrogen of dew point-43 ℃ is introduced dry adsorption tower again, filling 4A or 13X zeolite molecular sieve in the dry adsorption tower are used the heatless regeneration mode nitrogen are carried out depth drying, and dried nitrogen depoint depression is low to moderate below-60 ℃, be water content below 10ppm, nitrogen gas purity 98~99.9%.
Consider the harsh requirement of some production occasion and nitrogen quality without interruption to low dew point nitrogen (60 ℃), the present invention also connects in nitrogen basin back and is provided with standby drier, the demand of low dew point nitrogen in producing with absolute assurance.
Be used for the processing that dehydrates of important source material dimethyl cyclosiloxane (DMC) that organosilicon produces with the low dew point nitrogen (60 ℃) of system nitrogen device of the present invention preparation, the water content of DMC is dropped to about 80ppm by original 300ppm.And adopting steel cylinder nitrogen to dehydrate processing, the DMC water content has had decline by a relatively large margin by contrast at 120~140ppm.And use the low dew point nitrogen of system nitrogen device preparation of the present invention, the rubber that makes behind the dry DMC can keep higher molecular weight, and molecular weight is more stable, and the molecular weight fluctuation range is little, and the rubber that makes uses steel cylinder nitrogen more as clear as crystal.In addition, use low dew point nitrogen also to use steel cylinder nitrogen having bigger advantage aspect equipment investment benefit, the economy, the nitrogen cost can reduce significantly.
The present invention compared with prior art has the following advantages: one, the nitrogen dew point that makes of the device of transformation of the present invention absorption preparation nitrogen is low, and generally below-60 ℃, nitrogen gas purity is adjustable 98~99.9%; Two, the present invention dispose reasonable, complete, absolute guarantee to produce in to the low dew point of nitrogen with continuously for the requirement of nitrogen; Three, nitrogen-making device of the present invention is small and exquisite, and floor space is little, and running cost is low, and the cheap practicality of equipment price can be widely used in the occasion that electronics industry, chemical industry, medicine, packaging for foodstuff and storage etc. need low dew point nitrogen.
Further specify the present invention with specific embodiments of the invention and embodiment below, but embodiment not a limitation of the present invention.
Fig. 1 is the structural representation of apparatus of the present invention.
Fig. 2 is that the present invention's two tower carbon molecular sieve making nitrogen by pressure swing adsorption job orders and time distribution diagram are separated.
Fig. 3 is the present invention's two tower heatless regeneration operation program and sequential diagrams.
Number in the figure is expressed as:
The 1-air compressor, 2-cooler, 3-efficient degreasing device, 4a, 4b-nitrogen adsorption tower, 5-nitrogen buffer tank, the dry adsorption tower of 6a, 6b-, 7-nitrogen basin, the standby drier of 8-, 9, the 10-exhaust silencer, 11,12, the 13-pipeline;
V 1, V 2, V 3, V 4, V 5, V 6, V 7, V 8, V 9, V 10, V 11, V 12-operated pneumatic valve;
B 1, B 2-ball valve;
Z 1, Z 2, Z 3, Z 4-check-valves;
P 1, P 2, P 3, P 4, P 5, P 6-bypass ball valve.
As shown in Figure 1, the device of transformation of the present invention absorption preparation nitrogen successively by assembly such as air compressor 1, cooler 2, efficient degreasing device 3, two system nitrogen adsorption tower 4a and 4b, nitrogen buffer tank 5, two dry adsorption tower 6a and 6b, nitrogen basin 7, standby drier 8 and be connected the pipeline of each assembly and control device in the valve of gas flow form.
With reference to Fig. 1, Fig. 2 and Fig. 3, system nitrogen process is: air is compressed to 0.6~0.8MPa through air compressor 1, through cooler 2 coolings, behind 3 oil removings of efficient degreasing device, water, dust, enters the system nitrogen adsorption tower 4a and the 4b of two filling carbon molecular sieves.
Adopt two tower carbon molecular sieve making nitrogen by pressure swing adsorption operation one-period to divide six step programs, cycle period is 120 seconds, the operation of two tower alternate cycles, output nitrogen continuously.Be example mainly below, six step programs are illustrated successively with system nitrogen adsorption tower 4a.
The first step, 0~10 second.System nitrogen adsorption tower 4a absorption.Operated pneumatic valve V 1Open operated pneumatic valve V 3And V 5Close, compressed air enters 4a system nitrogen adsorption tower by the bottom, and airborne oxygen, water, carbon dioxide etc. are adsorbed by carbon molecular sieve, nitrogen enrichment in gas phase, and by operated pneumatic valve V 7Obtain product nitrogen gas.Make nitrogen adsorption tower 4b operated pneumatic valve V simultaneously 6Open V 2And V 8Close, carry out steps of exhausting.
Second step, 10~58 seconds.System nitrogen adsorption tower 4a absorption.Operated pneumatic valve V 1And V 7Continue to open, compressed air enters from the bottom, and product nitrogen gas is by operated pneumatic valve V 7Obtain, simultaneously, a certain proportion of product nitrogen gas is by ball valve B 1Entering another system nitrogen adsorption tower 4b washes.At this moment, system nitrogen adsorption tower 4b carries out rinsing step.
The 3rd step, 58~60 seconds.System nitrogen adsorption tower 4a all presses.Close operated pneumatic valve V 1And V 7, open operated pneumatic valve V 3And V 4, the conducting simultaneously of system nitrogen adsorption tower 4a and 4b upper and lower side, upper and lower end carries out pressure equalizing, and the nitrogen of enrichment is recovered and is used for system nitrogen adsorption tower 4b is boosted in the system nitrogen adsorption tower 4a gas phase.At this moment, the system nitrogen adsorption tower 4b step of boosting.
The 4th step, 60~70 seconds.System nitrogen adsorption tower 4a exhaust.Close operated pneumatic valve V 3And V 4, open operated pneumatic valve V 5, carry out exhaust process, make the oxygen, water, carbon dioxide etc. of carbon molecular sieve layer absorption obtain desorb, by operated pneumatic valve V 5Discharge by exhaust silencer 9.At this moment, system nitrogen adsorption tower 4b carries out adsorption step.
The 5th step, 70~118 seconds, system nitrogen adsorption tower 4a flushing.A part of nitrogen that system nitrogen adsorption tower 4b produces is by ball valve B 1Enter the upper end of system nitrogen adsorption tower 4a, from top to bottom the carbon molecular sieve layer is washed, so that the carbon molecular sieve layer obtains sufficient desorption and regeneration.Simultaneously, system nitrogen adsorption tower 4b carries out adsorption step.
The 6th step, 118~120 seconds.System nitrogen adsorption tower 4a boosts.Close operated pneumatic valve V 5, open operated pneumatic valve V 3And V 4, at this moment, automatic adsorption tower 4a being boosted by the nitrogen of making enrichment in the nitrogen adsorption tower 4b gas phase, a cycle period is finished.At this moment, system nitrogen adsorption tower 4b all presses step.
By-43 ℃ approximately of the nitrogen dew points that makes in the carbon molecular sieve system nitrogen adsorption tower, nitrogen gas purity 98~99.9% through behind the nitrogen buffer tank 5, enters the depth drying that two dry adsorption towers carry out nitrogen.The typical recycling cycle of the heatless regeneration drying nitrogen that the present invention adopts is 20 minutes, two dry adsorption tower blocked operations, the low dew point nitrogen of output continuously.Fill 4A or 13X zeolite molecular sieve in dry adsorption tower 6a and the 6b.Being example with dry adsorption tower 6a below illustrates successively to four step programs of cycle period.
The first step, 0~9 minute.Dry adsorption tower 6a absorption.Operated pneumatic valve V 9Open, dew point-43 ℃ nitrogen approximately enters dry adsorption tower 6a by nitrogen buffer tank 5, and moisture is selected absorption by zeolite molecular sieve, and low dew point nitrogen (60 ℃) is exported through check-valves Z3.At this moment, operated pneumatic valve V 12Open, dry adsorption tower 6b carries out evacuation step.
Second step, 9~10 minutes.Dry adsorption tower 6a absorption.Operated pneumatic valve V 9Continue to open, low dew point nitrogen (60 ℃) is through check-valves Z 3Continue output, simultaneously, the part of low dew point nitrogen is through ball valve B 2, check-valves Z 2 Dry adsorption tower 6b is boosted.At this moment, the dry adsorption tower 6b step of boosting.
The 3rd step, 10~19 minutes.Dry adsorption tower 6a emptying.Operated pneumatic valve V 9Close, open operated pneumatic valve V 11, residual gas carries out the molecular sieve layer desorption and regeneration through exhaust silencer 10 emptyings in the dry adsorption tower.At this moment, dry adsorption tower 6b carries out adsorption step.
The 4th step, 19~20 minutes.Dry adsorption tower 6a pressurising.Close operated pneumatic valve V 11, this moment is through ball valve B 2, check-valves Z 1The low dew point nitrogen of a part of being come by dry adsorption tower 6b boosts to dry adsorption tower 6a, finishes a cyclic process.At this moment, operated pneumatic valve V 10Open check-valves Z 4Open, dry adsorption tower 6b carries out adsorption step.
After two tower heatless regeneration dryings, the nitrogen dew point that obtains is regulated in the ball valve nitrogen basin 7 standby below-60 ℃.
Generally speaking, ball valve P 2, P 3, P 4Open ball valve P 1, P 5, P 6Close, low dew point nitrogen (60 ℃) is drawn by nitrogen basin 7, directly uses for producing from pipeline 13 outputs.Only when the dry adsorption tower of heatless regeneration broke down, dew point was drawn goal P for about-43 ℃ nitrogen from nitrogen buffer tank 5 1Open ball valve P 2, P 3Close, nitrogen enters nitrogen basin 7 through pipeline 12, ball valve P 4Close ball valve P 5Open, the nitrogen that goes out nitrogen basin 7 is through behind standby drier 8 depth dryings, the ball valve P of low dew point nitrogen (60 ℃) through opening that makes 6Use for producing.Filling 4A or 13X zeolite molecular sieve in the standby drier 8.

Claims (4)

1, a kind of device of transformation absorption preparation nitrogen, mainly comprise: be connected with air compressor [1], cooler [2], efficient degreasing device [3], system nitrogen adsorption tower [4a, 4b], nitrogen buffer tank [5], nitrogen basin [7] in turn by pipeline, autocontrol valve is installed on the pipeline, it is characterized in that: be provided with dry adsorption tower between nitrogen buffer tank [5] and nitrogen basin [7], described dry adsorption tower has 2~4.
2, the device of transformation absorption preparation nitrogen as claimed in claim 1 is characterized in that described dry adsorption tower has 2.
3, the device of transformation absorption preparation nitrogen as claimed in claim 1 or 2 is characterized in that being filled with in the described dry adsorption tower 4A or 13X zeolite molecular sieve.
4, the device of transformation as claimed in claim 1 or 2 absorption preparation nitrogen is characterized in that: also connect in nitrogen basin [7] back and be provided with standby drier [8].
CNB011048573A 2000-07-07 2001-02-20 Equipment for producing nitrogen gas by using pressure swing adsorption process Expired - Fee Related CN1150964C (en)

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CNB011048573A CN1150964C (en) 2000-07-07 2001-02-20 Equipment for producing nitrogen gas by using pressure swing adsorption process

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Application Number Priority Date Filing Date Title
CN00218326 2000-07-07
CN00218326.9 2000-07-07
CNB011048573A CN1150964C (en) 2000-07-07 2001-02-20 Equipment for producing nitrogen gas by using pressure swing adsorption process

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CN1150964C true CN1150964C (en) 2004-05-26

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102039083B (en) * 2010-08-23 2012-11-14 杭州普菲科空分设备有限公司 Isotonic purifying and drying system without resurgent gas loss and technological process thereof
CN102380286B (en) * 2011-11-28 2014-05-07 广西大学 Method for separating and purifying marsh gas and carbon dioxide through variable frequency and variable pressure adsorption
CN105080288A (en) * 2015-08-25 2015-11-25 江苏嘉宇流体装备有限公司 Adsorption column for low-dew-point pressure swing adsorption nitrogen making machine
CN105402604A (en) * 2015-12-29 2016-03-16 甘肃银光聚银化工有限公司 Nitrogen and compressed air co-production gas supply method
CN106276823B (en) * 2016-10-14 2018-10-23 北京石油化工工程有限公司 Low dew point swing adsorption nitrogen producing apparatus and technological process
CN108518920A (en) * 2018-05-04 2018-09-11 无锡市申隆气体设备有限公司 A kind of low dew point PSA nitrogen gas generating systems
CN111217340A (en) * 2020-01-15 2020-06-02 云南电网有限责任公司电力科学研究院 On-spot preparation facilities of high-purity carrier gas

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