CN110526223A - A kind of high pure nitrogen purifying technique and device - Google Patents

A kind of high pure nitrogen purifying technique and device Download PDF

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Publication number
CN110526223A
CN110526223A CN201910967489.2A CN201910967489A CN110526223A CN 110526223 A CN110526223 A CN 110526223A CN 201910967489 A CN201910967489 A CN 201910967489A CN 110526223 A CN110526223 A CN 110526223A
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adsorption tower
purifying
adsorption
cooler
pure nitrogen
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CN201910967489.2A
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刘江淮
周金城
王胜利
沈冰
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Maanshan Iron and Steel Co Ltd
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Maanshan Iron and Steel Co Ltd
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Priority to CN201910967489.2A priority Critical patent/CN110526223A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/04Purification or separation of nitrogen
    • C01B21/0405Purification or separation processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/04Purification or separation of nitrogen
    • C01B21/0405Purification or separation processes
    • C01B21/0433Physical processing only
    • C01B21/045Physical processing only by adsorption in solids
    • C01B21/0455Physical processing only by adsorption in solids characterised by the adsorbent
    • C01B21/0466Zeolites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0043Impurity removed
    • C01B2210/0045Oxygen
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0043Impurity removed
    • C01B2210/0053Hydrogen
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0043Impurity removed
    • C01B2210/0068Organic compounds
    • C01B2210/007Hydrocarbons

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

A kind of high pure nitrogen purifying technique of the present invention and device, including increase a purifying column in prior art basis, it forms two purifying columns and is connected in parallel, the method for operation of the using and the reserved;Increase by one or two coolers, cooler are arranged in the air inlet pipeline of adsorption tower;It further include increasing by two adsorption towers, every two series connection of four adsorption towers form two groups of adsorption towers being connected in parallel, two groups of adsorption tower the using and the reserved;Present invention process includes: to cool down after raw nitrogen gas enters a purifying column purification through subcooler E1, enter First adsorption tower later, it is cooling to enter another cooler E2 after purification by First adsorption tower, enter second adsorption tower after cooling, it is further purified, it is examined high pure nitrogen product up to standard by membrane compressor compression, boosting, then carries out filling bottle through busbar connector;Present invention process and device can ensure that high-purity gas production safety, stabilization, long-term operation, significantly improve economic benefit.

Description

A kind of high pure nitrogen purifying technique and device
Technical field
The invention belongs to Cryogenic air separation and liquefaction field more particularly to high-pure gas purifying techniques and device.
Background technique
High-purity nitrogen purifying plant is using pure nitrogen gas as unstripped gas, after purified equipment deep purifying, absorption, through examining The high pure nitrogen product for meeting national standard GB/T8979-2008 is produced, later by membrane compressor compression, boosting, then is passed through Busbar connector carries out filling bottle.In statement below, high-purity nitrogen is referred to as " high pure nitrogen ".
Purifier apparatus is the key equipment for removing impurity component in raw material pure nitrogen gas in high pure nitrogen purifying plant.Existing skill Art purifier apparatus be by purifying column, adsorption tower group at;The working principle of purifier apparatus is to be removed first by cleanser in purifying column Oxygen, methane, hydrogen, hydrocarbon in purity nitrogen, then water, carbon dioxide, acetylene in purity nitrogen are adsorbed by molecular sieve in adsorption tower, most It tests afterwards to nitrogen after purification, the high pure nitrogen that purity reaches national standard is carried out subsequent filling process.
Cleanser in purifier apparatus purifying column can not be recycled by regeneration, can only be regularly replaced;Purifying is set 13X adsorbent of molecular sieve in standby adsorption tower heats regeneration because its physical characteristic can pass through and is recycled.Therefore, it purifies The scientific optimization design of apparatus and process process is particularly important.
Currently, the schematic diagram of the universal process flow of high pure nitrogen purifying plant is shown in attached drawing 1, including purifying column, two Platform adsorption tower (use, a regeneration), is realized to pure nitrogen gas deep purifying, adsorption function.Purifier apparatus process flow is set A purifying column is counted, because of the physical characteristic of cleanser in purifying column, can not be recycled by regeneration method, it is necessary to periodically more It changes, causes the high pure nitrogen purifying plant cycle of operation shorter;Meanwhile when purifying column breaks down, purifying plant must be shut down Maintenance;The stoppage in transit of device caused by above-mentioned two kinds of factors necessarily affects high pure nitrogen production economy.
In addition, raw material pure nitrogen gas absorbs heat during purifying column removes oxygen, methane, hydrogen, hydrocarbon, temperature Degree increases;Later, enter adsorption tower by the unstripped gas that purifying column purifies, the 13X adsorbent of molecular sieve in adsorption tower is adsorbing In unstripped gas while water, carbon dioxide, acetylene, adsorbent of molecular sieve also absorbs heat, leads to adsorbent of molecular sieve temperature It increasing, adsorption capacity reduces, adsorption effect declines, and the adsorption tower duty cycle shortens, and adsorption tower must switch over operation, this When, 13X adsorbent of molecular sieve must use self-produced high pure nitrogen to carry out hot reactivation as regeneration gas source, cause entire high-purity Nitrogen purification device operating cost increases.
Summary of the invention
A kind of high pure nitrogen purifying technology scheme one of the present invention (see Fig. 2) are as follows: increase by one in prior art basis Two purifying columns are arranged in parallel, form the method for operation of the using and the reserved by platform purifying column;It is further added by a cooler E1, it is cooling Device E1 is arranged between the purifying column and adsorption tower;Present invention process method include: raw nitrogen gas enter two it is in parallel net After changing tower purification, after subcooler E1 is cooling, the adsorption tower being connected in parallel into two, after purification by adsorption tower, through examining It tests qualification and obtains high pure nitrogen product;Two purifying columns and two adsorption towers are the using and the reserved, maintain high pure nitrogen purification system System non-stop run.
It is special that the physics that cleanser can not be recycled by regeneration method in one purifying column is designed for purifier apparatus Property, the purifying column of a same model is added for purifier apparatus, two purifying columns are designed as being connected in parallel, and form 1 with 1 standby fortune High pure nitrogen purifying plant long-term operation is effectively ensured in line mode.
For the high phenomenon of adsorption tower operating temperature of purifier apparatus design, in the adsorption tower admission line after purifying column 1 gas cooler is added, gas cooler is exchanged heat using pure nitrogen gas in cooling water and adsorption tower air inlet pipeline, reduces adsorption tower Operating temperature.Because adsorbent of molecular sieve adsorption temp is lower, physical absorption efficiency is higher, and adsorbent of molecular sieve adsorption temp reduces 10 DEG C, adsorption capacity, which improves, is not less than 13%, so reducing adsorbent of molecular sieve adsorption temp, can effectively improve molecular sieve suction Attached dose of adsorption effect.When the 13X adsorbent of molecular sieve operating temperature in adsorption tower is high, to guarantee adsorption effect, adsorption tower work Make cycle time, adsorption tower must switch over operation at this time, make adsorbent of molecular sieve heating regeneration to restore efficacy of adsorption. Thus purifying plant operating cost is caused to increase.
The further technical solution two of the present invention is (see Fig. 3): increase by two adsorption towers, four adsorption towers every two are connected, Form two groups of adsorption towers being connected in parallel, be further added by a cooler E2, cooler E2 setting two concatenated adsorption towers it Between;Raw nitrogen gas cools down after entering a purifying column purification through subcooler E1, enters First adsorption tower later, by first Platform adsorption tower enters another cooler E2 cooling after purification, enters second adsorption tower after cooling and is further purified, through examining Qualification obtains high pure nitrogen product up to standard.In order to further enhance adsorption effect, accelerate adsorbent of molecular sieve cooling time, Adsorption efficiency is promoted, a cooler E2 is increased, absorption process is divided into secondary completion, optimizes adsorption effect, is adsorbed more thorough.
Scheme one or two in view of the above technology, the further technical solution of the present invention are to add according to process requirements One or two gas cooler E1 or E1 and E2 be shell-and-tube heat exchanger, gas cooler export raw material pure nitrogen gas temperature design For no more than 30 DEG C.It is exchanged heat by the raw nitrogen gas in the cooling water and pipeline in shell, reaches cooling raw material pure nitrogen gas Purpose, it is ensured that gas cooler export nitrogen temperature at 30 DEG C or less.
In order to more cost-effectively realize purification effect, two optimal technical solution of technical solution of the present invention are as follows: configuration four The adsorption tower of same model, adsorption tower volume are the 50% of the adsorption tower volume of former universal design.
A kind of high pure nitrogen purifying plant (see Fig. 2) of the present invention, described device include a purifying column, two adsorption towers, Raw nitrogen gas air inlet pipe accesses purifying column, and purifying column is connect by pipeline with two adsorption towers in parallel, and two adsorption towers one are used One is standby, and what purified nitrogen output channel was connect with membrane compressor, which be followed by busbar connector, carries out filling bottle;It is characterized in that: In Increase a purifying column on the basis of above-mentioned apparatus, two purifying columns are arranged in parallel, the method for operation of the using and the reserved is formed;Increase again A cooler E1, cooler E1 is added to be arranged between the purifying column and adsorption tower.
A kind of further technical solution (see Fig. 3) of high pure nitrogen purifying plant of the present invention is: add two adsorption towers, four Every two series connection of platform adsorption tower form two groups of adsorption towers being connected in parallel, and are further added by a cooler E2, and cooler E2 setting exists Between two concatenated adsorption towers;The technical program optimal case are as follows: the adsorption tower of four same models of configuration, adsorption tower volume It is the 50% of the adsorption tower volume of former universal design.
A kind of high pure nitrogen purifying plant of the present invention, wherein the gas cooler E1 added is arranged in one group of adsorption tower In middle First adsorption tower air inlet pipeline, second absorption is arranged in one group of adsorption tower in another gas cooler E2 added In tower air inlet pipeline.
1 purifying column of universal technical flow design of high-purity nitrogen purifying plant purifier apparatus, because net in purifying column Agent physical characteristic can not be recycled, it is necessary to regularly replace by regeneration method.
Meanwhile 2 adsorption towers of the universal technical flow design of high-purity nitrogen purifying plant purifier apparatus, because of adsorption tower Purity nitrogen adsorbate and 13X adsorbent of molecular sieve operating temperature it is high, the adsorption tower duty cycle is short, and adsorption tower must switch over fortune Row is regenerated with heating, and purifying plant operating cost is high.So measure is just from change high-purity nitrogen purifying plant purifier apparatus Process flow is set about.
Adsorbent of molecular sieve adsorption temp is lower, and physical absorption efficiency is higher, and adsorbent of molecular sieve adsorption temp reduces by 10 DEG C, adsorption capacity, which improves, is not less than 13%, reduces adsorbent of molecular sieve adsorption temp, can effectively improve adsorbent of molecular sieve suction Attached effect.
It is special that the physics that cleanser can not be recycled by regeneration method in 1 purifying column is designed for purifier apparatus Property, the purifying column of 1 same model is added for purifier apparatus.2 purifying columns are designed as parallel form setting, and purifying column forms 1 With the 1 standby method of operation, high-purity nitrogen purifying plant long-term operation is effectively ensured.
For the high phenomenon of adsorption tower operating temperature of purifier apparatus design, the gas of 2 same models is added for purifier apparatus Body cooler, gas cooler are exchanged heat using purity nitrogen in cooling water and absorber air inlet pipeline, reduce adsorption tower operating temperature.
Meanwhile under the conditions of 13X molecular sieve design loadings do not change in keeping adsorption tower, 13X molecular sieve is filled respectively In the absorber for entering 4 same models.Every 2 absorbers are arranged with cascade, are configured to 1 group of adsorption tower, form 2 groups of suctions Attached tower, 1 group of adsorption tower operation, 1 group of adsorption tower regeneration are spare.
1 gas cooler added is arranged in 1 group of adsorption tower in First absorber air inlet pipeline, net to reduce Purity nitrogen temperature in First absorber air inlet pipeline in change tower export pipeline, adsorption tower.
Another 1 gas cooler added is arranged in 1 group of adsorption tower in second absorber air inlet pipeline, to reduce First absorber export pipeline in adsorption tower, purity nitrogen temperature in second absorber air inlet pipeline.With this, adsorption tower work is improved Make the period, reduce purifying plant operating cost.
The schematic diagram of high-purity nitrogen purifying plant purifier apparatus process flow of the invention is specifically shown in attached drawing 2.
Detailed description of the invention
The universal process flow diagram of Fig. 1 high pure nitrogen purifying plant.
One process flow diagram of Fig. 2 technical solution of the present invention.
Two process flow diagram of Fig. 3 technical solution of the present invention.
Accompanying drawings symbol description:
1, purifying column A1;11, purifying column A2;2, adsorption tower B1;3, adsorption tower B2;12, gas cooler E1;13, gas Cooler E2;4, membrane compressor C;21, adsorption tower B11;22, adsorption tower B21;31, adsorption tower B12;32, adsorption tower B22.
Specific embodiment
The implementation of 3 pairs of technical solution of the present invention is described in further details with reference to the accompanying drawing:
Present invention implementation includes to 2 same models added in high-purity nitrogen purifying plant purifier apparatus process flow The absorber type selecting and corresponding pipeline, valve configuration of gas cooler and 4 same models.
The high-purity nitrogen purifying plant purifier apparatus process flow to have been put into operation for 2018 with Ma Gang gas branch company For, see attached drawing 2.
Gas pipeline and exits and entrances valve, the disengaging implication of configuration are imported and exported for the purification tower configuration for the same model added The model of body pipeline and exits and entrances valve, material specification are identical as former universal pipeline, the valve of purification tower configuration.
The 2 same model gas coolers added are shell-and-tube heat exchanger, and shell side is raw material pure nitrogen gas, tube side is cooling Water.
It is to fully meet adsorption tower operation work temperature no more than 30 DEG C that gas cooler, which exports raw material pure nitrogen gas temperature design, Degree requires.Gas cooler material is all selected as stainless steel with gas pipeline, the exits and entrances valve being equipped with for gas cooler Material, to reach high pure nitrogen production requirement.
The volume of 4 same model absorbers is selected as the 50% of the adsorption tower volume of former universal design, can be complete Meet 13X molecular sieve design loadings volume requirement.
Absorption tower technology of the absorber device structure, material, design specification of 4 same models with former universal design It is required that identical.
The high-purity nitrogen purifying plant purifier apparatus concrete operation method that horse steel gas companies have put into operation for 2018 It is as follows:
Liquid nitrogen storage tank operating pressure is adjusted to 0.5MPa, opens the total intake valve of high pure nitrogen purifier apparatus.
Intake valve, outlet valve in the purifying column A1 that standard-sized sheet uses, it is complete close intake valve in the purifying column A2 in stand-by state, Outlet valve, the electric heater of the electric heater of the purifying column A1 that puts into operation, stoppage in transit purifying column A2, make purifying column A1 it is in operating status, Purifying column A2 is in stoppage in transit state.
Standard-sized sheet gas cooler E1, the inlet valve of gas cooler E2, back-water valve (BWV), put into operation gas cooler E1, E2, makes gas The outlet body cooler E1, gas cooler E2 raw material pure nitrogen gas temperature is respectively less than 30 DEG C.
Standard-sized sheet adsorption tower B11, the intake valve of adsorption tower B12, outlet valve, the full air inlet for closing adsorption tower B21, adsorption tower B22 Valve, outlet valve, make adsorption tower B11, adsorption tower B12 be in operating status, and adsorption tower B21, adsorption tower B22 are in stoppage in transit shape State.When the in-line analyzer show value of high-purity nitrogen purifier apparatus reaches high-purity nitrogen national normal value, diaphragm is opened Formula compressor intake valve, displacement, starting membrane compressor, carries out high-purity nitrogen and fills a bottle operation.
The process flow of this high-purity nitrogen purifying plant purifier apparatus, guarantee high-purity nitrogen purifying plant safety, Stablize, long-term operation, improve high-purity nitrogen production economy benefit, make full use of the existing appointed condition of purifying plant, only 1 purifying column, 2 gas coolers, corresponding pipeline and valve need to be increased, equipment ordering expense increases few.
The method of the present invention is clear, simple and fast, cheap practical, can fundamentally solve high-purity nitrogen purification dress well It sets long-term operation, reduce high-purity nitrogen production cost problem.
The adsorption tower operating temperature of horse steel high-purity nitrogen purifying plant purifier apparatus of the invention is not more than 30 DEG C, purifying Equipment designs rated power 7.7KW.H, service life 5 years, leads to better than domestic with what external high-purity nitrogen purifying plant used With type process flow and Tong Chang, with the purifier apparatus 10.5KW.H of yield design rated power, 2 years service life.

Claims (7)

1. a kind of high pure nitrogen purifying technique, the technique includes: that raw nitrogen gas enters purifying column purification, enters absorption later Tower, two adsorption towers are connected in parallel, the using and the reserved, after purification by adsorption tower, through examining qualification to obtain high pure nitrogen product;Its It is characterized in: increases a purifying column on the basis of above-mentioned process, two purifying columns are arranged in parallel, the using and the reserved are formed The method of operation;It is further added by a cooler E1, cooler E1 is arranged between the purifying column and adsorption tower;Present invention process side Method includes: after raw nitrogen gas enters two purifying column purifications in parallel, after subcooler E1 is cooling, to be connected in parallel into two Adsorption tower, after purification by adsorption tower, through examine qualification obtain high pure nitrogen product;Two purifying columns and two adsorption towers are equal For the using and the reserved, the non-stop run of high pure nitrogen purification system is maintained.
2. a kind of high pure nitrogen purifying technique according to claim 1, it is characterized in that: increase by two adsorption towers, four suctions Attached every two series connection of tower form two groups of adsorption towers being connected in parallel, and are further added by a cooler E2, and cooler E2 is arranged at two Between concatenated adsorption tower;Raw nitrogen gas cools down after entering a purifying column purification through subcooler E1, enters First later Adsorption tower, it is cooling to enter another cooler E2 after purification by First adsorption tower, enter after cooling second adsorption tower into The purifying of one step, it is qualified through examining, obtain high pure nitrogen product up to standard.
3. a kind of high pure nitrogen purifying technique according to claim 1 or 2, it is characterized in that: one or two added Gas cooler E1 or E1 and E2 is shell-and-tube heat exchanger, and it is no more than 30 that gas cooler, which exports raw material pure nitrogen gas temperature design, ℃。
4. a kind of high pure nitrogen purifying technique according to claim 2, it is characterized in that: four same model adsorption towers Volume be selected as former universal design adsorption tower volume 50%.
5. a kind of high pure nitrogen purifying plant, described device includes a purifying column, two adsorption towers, and raw nitrogen gas air inlet pipe connects Enter purifying column, purifying column is connect by pipeline with two adsorption towers in parallel, two adsorption tower the using and the reserved, purified nitrogen What gas output channel was connect with membrane compressor, which be followed by busbar connector, carries out filling bottle;It is characterized in that: increasing on the basis of above-mentioned apparatus Add a purifying column, two purifying columns are arranged in parallel, the method for operation of the using and the reserved is formed;It is further added by a cooler E1, Cooler E1 is arranged between the purifying column and adsorption tower.
6. a kind of high pure nitrogen purifying plant according to claim 5, it is characterized in that: two adsorption towers are added, four suctions Attached every two series connection of tower form two groups of adsorption towers being connected in parallel, and are further added by a cooler E2, and cooler E2 is arranged at two Between concatenated adsorption tower.
7. device according to claim 6, it is characterized in that: the gas cooler E1 added is arranged in one group of adsorption tower In middle First adsorption tower air inlet pipeline, second absorption is arranged in one group of adsorption tower in another gas cooler E2 added In tower air inlet pipeline.
CN201910967489.2A 2019-10-12 2019-10-12 A kind of high pure nitrogen purifying technique and device Pending CN110526223A (en)

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Cited By (1)

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CN114702015A (en) * 2021-10-29 2022-07-05 上海伟创标准气体分析技术有限公司 Purification device and purification method for high-purity nitrogen

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