CN106310870A - Device for gradually adsorbing and purifying ammonia gas and method for utilizing device to purify ammonia gas - Google Patents
Device for gradually adsorbing and purifying ammonia gas and method for utilizing device to purify ammonia gas Download PDFInfo
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- CN106310870A CN106310870A CN201611004702.2A CN201611004702A CN106310870A CN 106310870 A CN106310870 A CN 106310870A CN 201611004702 A CN201611004702 A CN 201611004702A CN 106310870 A CN106310870 A CN 106310870A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/12—Separation of ammonia from gases and vapours
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
- B01D2253/108—Zeolites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
- B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a device for gradually adsorbing and purifying ammonia gas and a method for utilizing the device to purify ammonia gas. The device comprises a No.1 adsorption column, a No.2 adsorption column, a No.3 adsorption column, a No.4 adsorption column, a No.5 adsorption column and a No.6 adsorption column. The low-purity ammonia gas (99.8%) is purified to high-purity and even higher purity (99.999%-99.995%) ammonia gas through multi-level absorption. After the raw ammonia gas is gradually adsorbed by the fillers in different serially connected adsorption columns, the related harmful impurity content in the raw ammonia gas is removed; the impurities contain harmful impurities including abundant grease, water, oxygen, nitrogen, carbon dioxide, sulfide, grains, and the like; the high-purity ammonia gas is lastly acquired after the impurities are removed; the nitrogen source supplied to the silicon nitride film in the solar industry can be realized; the clean technical ammonia gas can be supplied to the integrated circuit manufacturing, compound semiconductor, liquid crystal display and silicon wafer cleaning; the excellent technical basis is supplied to the purification of high-purity ammonia gas.
Description
Technical field
The present invention relates to low-purity ammonia purification technique, be specifically related to a kind of absorption step by step and purify device and the utilization of ammonia
This device purifies the method for ammonia.
Background technology
High-purity ammon is as the raw material of electron trade, and the quality of its product is most important, is directly connected to final products
Yield.High-purity ammon is all to have close relationship for the development of raw-material quality and cost and industry.
At present, high-purity ammon can apply to the row such as big sun energy, IC manufacturing, compound semiconductor, liquid crystal display
Industry, can be that the silicon nitride film in big sun energy industry provides nitrogen source, provide clean ammonia for cleaning silicon chip, it is also possible to for more
The purification of highly purified ammonia (99.9999%-99.99999%) provides extraordinary Process ba-sis.
At present, market mostly use ultrapure ammonia that extensive process produces as the source of goods, but, the method price is held high
Expensive, product-specific investments is big, and unit price is high.Accordingly, it would be desirable to develop the new method purifying ammonia, provide the product guaranteed both quality and quantity for client
Product, it is clear that be very important.
Summary of the invention
The invention aims to the shortcoming overcoming above-mentioned background technology, it is provided that a kind of absorption step by step purifies the dress of ammonia
Put and utilize the method that this device purifies ammonia.Raw material ammonia purifies after different adsorption column series connection absorption step by step, removes with this
The objectionable impurities such as oils and fats in raw material ammonia, moisture content, oxygen, nitrogen, carbon dioxide, sulfide, granule, have degree of depth absorption, absorption total
The advantages such as amount is big, it is ensured that product quality is continual and steady；Ammonia concentration after purification can reach 99.999% even more high-purity, can
Use and the production technology such as on-the-spot high-purity ammon processed meeting solar energy industry, use simultaneously a kind of adsorption column is carried out special again
Raw mode makes the filler in adsorption column regenerate completely.
The technical scheme is that a kind of absorption step by step purifies the device of ammonia, including an adsorption column, No. two absorption
Post, No. three adsorption columns, No. four adsorption columns, No. five adsorption columns, No. six adsorption columns；A described adsorption column respectively with No. two absorption
Post, No. three adsorption columns, No. four adsorption column connections；Described No. two adsorption columns connect with No. three adsorption columns, No. four adsorption columns respectively；Institute
State No. three adsorption columns to connect with No. four adsorption columns, No. five adsorption columns, No. six adsorption columns respectively；Described No. four adsorption columns are respectively with five
Number adsorption column, No. six adsorption columns connections；Described No. five adsorption columns and No. six adsorption column connections；A described adsorption column includes No. one
Adsorption column housing and be positioned at the porous ceramics adsorbent equipment of an adsorption column housing；Described No. two adsorption columns include No. two suctions
Attached column housing and be positioned at the porous ceramics adsorbent equipment of No. two adsorption column housings；Described No. three adsorption columns include No. three absorption
Post housing and be positioned at the first molecular sieve of No. three adsorption column housings；Described No. four adsorption columns include No. four adsorption column housings with
And it is positioned at the second molecular sieve of No. four adsorption column housings；Described No. five adsorption columns include No. five adsorption column housings and are positioned at five
Type three-molecular screen alternating in number adsorption column housing；Described No. six adsorption columns include No. six adsorption column housings and are positioned at No. six adsorption columns
The 4th molecular sieve in housing；A described adsorption column, No. two adsorption columns are connected to raw material ammonia inlet pipe respectively；Described No. five absorption
Post, No. six adsorption columns are connected to high-purity ammonia respectively and go out pipe；Each adsorption column is respectively equipped with sewage draining exit, regeneration ammonia entrance and heat
Nitrogen entrance；The aperture of described first molecular sieve is more than or equal to the aperture of described second molecular sieve；The aperture of described second molecular sieve
Aperture more than described type three-molecular screen alternating；The aperture of described type three-molecular screen alternating is more than or equal to the aperture of described 4th molecular sieve.
The device that absorption step by step disclosed by the invention purifies ammonia is three grades of absorption, is made up of six roots of sensation adsorption column, every suction
Attached column is designed with hot nitrogen entrance, sewage draining exit；In the present invention, all adsorption columns are designed with hot nitrogen entrance；Utilize hot nitrogen purging permissible
The impurity accelerating to adsorb adsorbent equipment is discharged from sewage draining exit, not only improves adsorption efficiency, increases refining effect, moreover it is possible to the suction being
Adsorption device recycles, and reduces equipment cost.Preferably, described hot nitrogen entrance and sewage draining exit are respectively at each adsorption column
Top and bottom, can increase purging effect.
In the present invention, described adsorption column is respectively equipped with regeneration ammonia entrance, and regeneration ammonia can be to adsorbent equipment, molecular sieve
Carry out regenerative adsorption process, resource utilization is greatly improved, and increases industrialization ammonia purification efficiency and refining effect, in order to
Increase regeneration effect, preferably regeneration ammonia entrance go out pipe with high-purity ammonia and connect, such that it is able to utilize purified ammonia to carry out
Absorption regeneration processes, and improves regeneration efficiency further, increases regeneration effect.
In the device of the purification ammonia of absorption step by step disclosed by the invention, an adsorption column and No. two adsorption columns are combined as first
Level absorption, No. three adsorption columns and No. four adsorption columns are combined as the second level and adsorb, and No. five adsorption columns and No. six adsorption columns are combined as the
Three grades of absorption.It is designed with valve between the adsorption column of two connections；Raw material ammonia inlet pipe and high-purity ammonia go out pipe and set the most respectively
There is valve；Can be beneficial to control air-flow, be also convenient for independent control.According to assembly of the invention, can be as the ammonia of two set parallel connections
Gas purifying plant, such as No. one adsorption column, No. three adsorption columns, No. five adsorption columns are a set of, No. two adsorption columns, No. four adsorption columns,
No. six adsorption columns are another set of；Can also be as a set of ammonia purifying plant, i.e. No. one adsorption column, No. two adsorption columns, No. three suctions
Attached column, No. four adsorption columns, No. five adsorption columns, No. six adsorption columns are composed in series a set of；Can also adsorption column, No. three absorption
Post, No. four adsorption columns, No. five adsorption columns are a set of ammonia purifying plant；The most both ammonia purification efficiency can have been improved, the most permissible
Absorption regeneration is purified with ammonia carry out, it is also possible to for the purification of particular/special requirement such as ultra-high purity ammonia simultaneously.
In the present invention, a described adsorption column top respectively with No. two adsorption columns bottom, bottom No. three adsorption columns, No. four suctions
Connect bottom attached column；Described No. two adsorption column tops respectively with bottom No. three adsorption columns, connect bottom No. four adsorption columns；Described three
Number adsorption column top respectively with bottom No. four adsorption columns, bottom No. five adsorption columns, connect bottom No. six adsorption columns；Described No. four suctions
Attached column top respectively with bottom No. five adsorption columns, connect bottom No. six adsorption columns；Described No. five adsorption column tops and No. six absorption
Column bottom connects；Described raw material ammonia inlet pipe is connected with bottom an adsorption column, No. two adsorption columns respectively, and described high-purity ammonia goes out
Pipe is connected with No. five adsorption columns, No. six adsorption column tops respectively.Gas is discharged by entrance bottom adsorption column, top, improves miscellaneous
Matter removal effect, raw material ammonia, after primary adsorption, secondary absorption, three grades of absorption series connection absorption, removes in raw material ammonia and contains
The a large amount of impurity having, this type of impurity comprises oxygen, nitrogen, oils and fats, sulfide, granule, powder and aqueous vapor and carbon dioxide, removes
After high-purity ammonia total impurities content less than 5ppm, commercial Application demand can be met.
In the present invention, described adsorption column lateral wall is provided with attemperator, is conducive to accelerating when hot nitrogen purging Regeneration Treatment
Adsorption column internal temperature promotes and insulation；Preferably, described heater is detachable heat-insulation device, in temperature-fall period,
It is rapid that dismounting attemperator is beneficial to adsorption column internal cooling.Preferably, adsorption column is provided with temperature sensor, can blow at hot nitrogen
Sweep, Regeneration Treatment time grasp the temperature in adsorption column.
In the present invention, connected by stainless steel pipes between adsorption column；Adsorption column housing can be that cylinder can also be
Other shapes, the flowing of preferably cylindrical beneficially gas is also avoided adsorbing dead angle, is arranged adsorbent equipment in housing.The present invention is one
In level absorption (i.e. No. an adsorption column, No. two adsorption columns), porous ceramics adsorbent equipment is set, secondary absorption (i.e. No. three adsorption columns,
No. four adsorption columns) and three grades of absorption (i.e. No. five adsorption columns, No. six adsorption columns) in be respectively provided with molecular sieve, can progressively filter
Impurity in raw material ammonia, the aperture of the especially first molecular sieve is more than or equal to the aperture of described second molecular sieve；Described second
The aperture of molecular sieve is more than the aperture of described type three-molecular screen alternating；The aperture of described type three-molecular screen alternating is more than or equal to described 4th molecule
The aperture of sieve, forms gradient remove impurity, beneficially refining effect.Preferably, the filtering accuracy of porous ceramics adsorbent equipment be 0.05～
0.1 micron, the model of the first molecular sieve and the second molecular sieve is all 13X, and the model of type three-molecular screen alternating and the 4th molecular sieve is all
4A；Raw material ammonia is entered by raw material ammonia inlet pipe, the most slightly a large amount of moisture content in absorption raw material ammonia, oils and fats, dust, particulate matter etc.
Impurity, then remove substantial amounts of moisture content in raw material ammonia, sulfur gas thing and carbon dioxide, the last degree of depth removes water a small amount of in raw material ammonia
Part, sulfur gas thing and carbon dioxide；Three grades of absorption the most all can remove the impurity such as oils and fats, oxygen nitrogen, through three adsorbent equipments
High-purity ammon after series connection absorption is up-to-standard, can go out pipe entrance client by high-purity ammonia and use district.
The invention also discloses a kind of utilize above-mentioned step by step absorption purify ammonia device purify ammonia method, including with
Lower step:
(1) with an adsorption column and/or No. two adsorption columns as first class absorber；With No. three adsorption columns and/or No. four adsorption columns it is
Second class absorber；It is three grades of adsorbers with No. five adsorption columns and/or No. six adsorption columns；Respectively to an adsorption column, No. two absorption
Post, No. three adsorption columns, No. four adsorption columns, No. five adsorption columns, No. six adsorption columns carry out Regeneration Treatment；
The Regeneration Treatment of a described adsorption column is, in utilizing the heating of hot nitrogen to make an adsorption column, temperature reaches 250 DEG C, then
It is incubated 4 hours；Then, under in an adsorption column, gas pressure is 15psig, adjusting temperature in an adsorption column is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in a number adsorption column is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of an adsorption column；
The Regeneration Treatment of described No. two adsorption columns is, in utilizing the heating of hot nitrogen to make No. two adsorption columns, temperature reaches 250 DEG C, then
It is incubated 4 hours；Then, under in No. two adsorption columns, gas pressure is 15psig, adjusting temperature in No. two adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. two adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. two adsorption columns；
The Regeneration Treatment of described No. three adsorption columns is, in utilizing the heating of hot nitrogen to make No. three adsorption columns, temperature reaches 150 DEG C, then
It is incubated 2 hours；Then, under in No. three adsorption columns, gas pressure is 15psig, adjusting temperature in No. three adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. three adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. three adsorption columns；
The Regeneration Treatment of described No. four adsorption columns is, in utilizing the heating of hot nitrogen to make No. four adsorption columns, temperature reaches 150 DEG C, then
It is incubated 2 hours；Then, under in No. four adsorption columns, gas pressure is 15psig, adjusting temperature in No. four adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. four adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. four adsorption columns；
The Regeneration Treatment of described No. five adsorption columns is, in utilizing the heating of hot nitrogen to make No. five adsorption columns, temperature reaches 250 DEG C, then
It is incubated 2 hours；Then, under in No. five adsorption columns, gas pressure is 15psig, adjusting temperature in No. five adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. five adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. five adsorption columns；
The Regeneration Treatment of described No. six adsorption columns is, in utilizing the heating of hot nitrogen to make No. six adsorption columns, temperature reaches 250 DEG C, then
It is incubated 4 hours；Then, under in No. six adsorption columns, gas pressure is 15psig, adjusting temperature in No. six adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. six adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. six adsorption columns；
(2) first class absorber after raw material ammonia sequentially enters Regeneration Treatment, the second class absorber after Regeneration Treatment, Regeneration Treatment
After three grades of adsorbers, complete ammonia purify.
In the present invention, with an adsorption column and/or No. two adsorption columns as first class absorber；With No. three adsorption columns and/or four
Number adsorption column is second class absorber；It is three grades of adsorbers with No. five adsorption columns and/or No. six adsorption columns；Six adsorption columns can group
Become many set ammonia purification systems, if raw material ammonia fullness caused by stagnant QI foot sequentially pass through primary adsorption, secondary absorption, three grades adsorb, than
If an adsorption column, No. three adsorption columns, No. five adsorption columns are a set of, No. two adsorption columns, No. four adsorption columns, No. six adsorption columns are another
A set of；When an adsorption column, No. three adsorption columns, No. five adsorption columns carry out Regeneration Treatment, No. two adsorption columns, No. four adsorption columns,
The train of No. six adsorption column compositions can carry out ammonia purification, does not affect commercial production progress.
In the present invention, Regeneration Treatment can remove the impurity of adsorbent equipment, molecular sieve, it is ensured that it is pure that ammonia purifies environment,
But also enable to adsorbent equipment, regenerating molecular sieve, improve resource utilization, increase and purify the degree of depth, improve refining effect.
In the present invention, No. two adsorption columns and the most standby adsorption column of adsorption column, its regeneration is identical；No. three absorption
Post and No. four the most standby adsorption columns of adsorption column, its regeneration is identical；No. five adsorption columns and No. six the most standby suctions of adsorption column
Attached column, its regeneration is identical.
In the present invention, in utilizing the heating of hot nitrogen ladder to make an adsorption column, temperature reaches 250 DEG C, and ladder heating-up temperature is
50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, can realize by being passed through the hot nitrogen of different temperatures；Hot nitrogen ladder is utilized to heat
In making No. two adsorption columns, temperature reaches 250 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, permissible
Realize by being passed through the hot nitrogen of different temperatures；In utilizing the heating of hot nitrogen ladder to make No. three adsorption columns, temperature reaches 150 DEG C, ladder
Heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, can realize by being passed through the hot nitrogen of different temperatures；The heating of hot nitrogen ladder is utilized to make
In obtaining No. four adsorption columns, temperature reaches 150 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, can be passed through not equality of temperature
The hot nitrogen of degree realizes；In utilizing the heating of hot nitrogen ladder to make No. five adsorption columns, temperature reaches 250 DEG C, and ladder heating-up temperature is 50
DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, can by be passed through different temperatures hot nitrogen realize；The heating of hot nitrogen ladder is utilized to make
In obtaining No. six adsorption columns, temperature reaches 250 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, Ke Yitong
Cross the hot nitrogen realization being passed through different temperatures.
In the present invention, all adsorption columns are passed through regeneration ammonia the most in seven times, the pressure of the regeneration ammonia being passed through for described seven times
It is followed successively by 5psig, 15psig, 30psig, 50psig, 75psig, 90psig, 90psig, is passed through regeneration ammonia the last time
In rear holding adsorption column, gas pressure is 50psig；Preferably, in adsorption column, temperature is to be passed through when 30 DEG C～50 DEG C again every time
Ammonifying gas；The absorption heat energy being conducive to adsorbent sheds in time, and the process of regeneration the most at different levels is more complete, effect is more preferable.
In the present invention, raw material ammonia is entered by raw material ammonia inlet pipe, first primary adsorption, removes a large amount of water in raw material ammonia
The impurity such as part, oils and fats, dust, particulate matter, more substantial amounts of moisture content, sulfur gas thing and titanium dioxide in secondary absorption removes raw material ammonia
Carbon, eventually passes three grades of adsorption deeplies and removes moisture content, sulfur gas thing and carbon dioxide a small amount of in raw material ammonia；Every grade of absorption is in difference
Degree all can remove the impurity such as oils and fats, oxygen nitrogen, and the high-purity ammon after three grades of adsorbent equipment series connection absorption is up-to-standard, can be by height
Pure ammonia goes out pipe entrance client and uses district.
The invention has the beneficial effects as follows:
(1) utilize method of the present invention it is only necessary to by the ammonia after vaporization by after adsorbent equipment, the adsorption column absorption of series connection is former
Expect the objectionable impurities such as the oils and fats in ammonia, moisture content, oxygen, nitrogen, carbon dioxide, sulfide, granule, the raw material ammonia of 99.8% the most at last
Gas is purified to high-purity ammonia of more than 99.999% purity；Meeting the prescription of solar energy client, easy to use, price is excellent honest and clean；
(2) device disclosed by the invention saves energy consumption, pollutes few, can be by ammonia relatively low for economic worth through inhaling through this device
Attached change into the ammonia that concentration is higher, improve the value of product, create preferable economic benefit；Without more Factory Building
With investment, and high efficiency, gas supply conduit can be continued, the source of the gas effect solving the industry is become apparent from, it is possible to be satisfied with the sun
Energy photovoltaic industry and other field, air ambient is not polluted by absorption method, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the structural representation that embodiment one adsorbs the device purifying ammonia step by step.
Wherein: 1 a, adsorption column；2, No. two adsorption columns；3, No. three adsorption columns；4, No. four adsorption columns；5, No. five absorption
Post；6, No. six adsorption columns；7, raw material ammonia inlet pipe；8, high-purity ammonia goes out pipe；9, sewage draining exit；10, regeneration ammonia entrance；11, heat
Nitrogen entrance；12, valve.
Detailed description of the invention
Embodiment one
See accompanying drawing 1, step by step absorption purify the device of ammonia include an adsorption column 2, No. three adsorption columns 3 of 1, No. two adsorption columns,
No. four adsorption columns 5, No. six adsorption columns 6 of 4, No. five adsorption columns；A described adsorption column top respectively with No. two adsorption columns bottom, three
Connect bottom number adsorption column, bottom No. four adsorption columns；Described No. two adsorption column tops respectively with No. three adsorption columns bottom, No. four suctions
Connect bottom attached column；Described No. three adsorption column tops respectively with No. four adsorption columns bottom, bottom No. five adsorption columns, No. six adsorption columns
Bottom connection；Described No. four adsorption column tops respectively with bottom No. five adsorption columns, connect bottom No. six adsorption columns；Described No. five suctions
Attached column top connects bottom No. six adsorption columns；Described raw material ammonia inlet pipe 7 respectively with an adsorption column, No. two adsorption columns bottom
Connecting, described high-purity ammonia goes out pipe 8 and is connected with No. five adsorption columns, No. six adsorption column tops respectively；Described adsorption column is respectively equipped with
Sewage draining exit 9, regeneration ammonia entrance 10 and hot nitrogen entrance 11；Regeneration ammonia entrance goes out pipe with high-purity ammonia and connects, can be direct
Ammonia after purifying is used for adsorption column Regeneration Treatment；It is designed with valve 12 between the adsorption column of two connections；Raw material ammonia enters
Pipe and high-purity ammonia go out pipe and are also respectively equipped with valve；Can be beneficial to control air-flow, be also convenient for independent control；Hot nitrogen purging people
Mouth, sewage draining exit, regeneration ammonia entrance lay respectively at the top of each adsorber, bottom, bottom；For sake of simplicity, it is identical in accompanying drawing
Parts mark at one, and some traditional valve do not indicate.
In the device of the above-mentioned purification ammonia of absorption step by step, a described adsorption column includes an adsorption column housing and is positioned at
Porous ceramics adsorbent equipment in a number adsorption column housing；Described No. two adsorption columns include No. two adsorption column housings and are positioned at two
Porous ceramics adsorbent equipment in number adsorption column housing；Described No. three adsorption columns include No. three adsorption column housings and are positioned at No. three
The first molecular sieve in adsorption column housing；Described No. four adsorption columns include No. four adsorption column housings and are positioned at No. four adsorption column shells
The second internal molecular sieve；Described No. five adsorption columns include No. five adsorption column housings and are positioned at the of No. five adsorption column housings
Type three-molecular screen alternating；Described No. six adsorption columns include No. six adsorption column housings and are positioned at the 4th molecule of No. six adsorption column housings
Sieve；Porous ceramics adsorbent equipment is aluminium sesquioxide adsorbent equipment, and filtering accuracy is 0.05 micron, first, second molecular sieve
Model is 13X, and the model of the three, the 4th molecular sieves is 4A.Porous ceramics adsorbent equipment, molecular sieve this as existing product, its
It is arranged in adsorption column by conventional means.
With an adsorption column and/or No. two adsorption columns as first class absorber；With No. three adsorption columns and/or No. four adsorption columns it is
Second class absorber；It is three grades of adsorbers with No. five adsorption columns and/or No. six adsorption columns；Raw material ammonia through primary adsorption, two grades
After absorption, three grades of absorption series connection absorption, removing a large amount of impurity contained in raw material ammonia, this type of impurity comprises oxygen, nitrogen, oil
Fat, sulfide, granule, powder and aqueous vapor and carbon dioxide.Primary adsorption wherein loads aluminium sesquioxide adsorbent as many
Hole ceramic adsorbent device, the most slightly adsorbs the impurity such as a large amount of moisture content in raw material ammonia, oils and fats, dust, particulate matter；In secondary absorption
Filling molecular sieve (13X), as adsorbent equipment, mainly removes substantial amounts of moisture content, sulfur gas thing and carbon dioxide in raw material ammonia；Three grades
Absorption loads molecular sieve (4A) and removes moisture content, sulfur gas thing and titanium dioxide a small amount of in raw material ammonia as adsorbent equipment, major depth
Carbon.Three groups of absorption the most all can remove the impurity such as oils and fats, oxygen nitrogen.High-purity ammon quality after three adsorbent equipment absorption
Qualified, client can be entered by shutoff valve through pipeline and use district.
Embodiment two
A kind of absorption step by step purifies the device of ammonia, and basically identical with embodiment one, difference is porous ceramics adsorbent equipment
For aluminium sesquioxide adsorbent equipment, filtering accuracy is 0.1 micron；All adsorption column lateral walls are provided with attemperator, all absorption
Post is provided with temperature sensor.
Embodiment three
A kind of device utilizing embodiment two carries out the method that absorption method purifies high-purity ammonia, comprises the following steps:
(1) hot nitrogen lead to superheated nitrogen entrance a number adsorption column is carried out displacement purging, heating-up temperature use staged rise, 50
DEG C, 100 DEG C, 150 DEG C, 200 DEG C, the mode of 250 DEG C heats, until the top and bottom temperature of adsorption column reaches 250 DEG C
And maintain 4 hours；Keeping nitrogen pressure 15psig in adsorption column, natural cooling reaches 35 DEG C；Remove adsorption column external heat preserving device
To lower the temperature quickly to reach temperature required；Being passed through regeneration ammonia in adsorption column in seven times, the speed being passed through is successively
5psig, 15psig, 30psig, 50psig, 75psig, 90psig, 90psig, when being passed through regeneration ammonia every time, temperature in adsorption column
Degree is 30 DEG C；The pressure 50psig in adsorption column is kept, until temperature is 30 in adsorption column after being passed through regeneration ammonia for the last time
℃；Finally discharge regeneration ammonia, to complete an adsorption column regeneration；
(2) hot nitrogen lead to superheated nitrogen entrance No. two adsorption columns are carried out displacement purging, heating-up temperature use staged rise, 50
DEG C, 100 DEG C, 150 DEG C, 200 DEG C, the mode of 250 DEG C heats, until the top and bottom temperature of adsorption column reaches 250 DEG C
And maintain 4 hours；Keeping nitrogen pressure 15psig in adsorption column, natural cooling reaches 45 DEG C；Remove adsorption column external heat preserving device
To lower the temperature quickly to reach temperature required；Being passed through regeneration ammonia in adsorption column in seven times, the speed being passed through is successively
5psig, 15psig, 30psig, 50psig, 75psig, 90psig, 90psig, when being passed through regeneration ammonia every time, temperature in adsorption column
Degree is 30 DEG C；The pressure 50psig in adsorption column is kept, until temperature is 30 in adsorption column after being passed through regeneration ammonia for the last time
℃；Finally discharge regeneration ammonia, to complete No. two adsorption column regeneration；
(3) hot nitrogen lead to superheated nitrogen entrance No. three adsorption columns are carried out displacement purging, heating-up temperature use staged rise, 50
DEG C, 100 DEG C, the mode of 150 DEG C heats, until the top and bottom temperature of adsorption column reaches 150 DEG C and maintains 2 hours；
Keeping nitrogen pressure 15psig in adsorption column, natural cooling reaches 45 DEG C；Remove adsorption column external heat preserving device to lower the temperature quickly
To reach temperature required；In adsorption column, be passed through regeneration ammonia in seven times, the speed being passed through be successively 5psig, 15psig,
30psig, 50psig, 75psig, 90psig, 90psig, when being passed through regeneration ammonia, in adsorption column, temperature is 50 DEG C every time；Finally
The pressure 50psig in adsorption column is kept, until temperature is 50 DEG C in adsorption column after being once passed through regeneration ammonia；Finally discharge again
Ammonifying gas, to complete an adsorption column regeneration；
(4) hot nitrogen lead to superheated nitrogen entrance No. four adsorption columns are carried out displacement purging, heating-up temperature use staged rise, 50
DEG C, 100 DEG C, the mode of 150 DEG C heats, until the top and bottom temperature of adsorption column reaches 150 DEG C and maintains 2 hours；
Keeping nitrogen pressure 15psig in adsorption column, natural cooling reaches 35 DEG C；Remove adsorption column external heat preserving device to lower the temperature quickly
To reach temperature required；In adsorption column, be passed through regeneration ammonia in seven times, the speed being passed through be successively 5psig, 15psig,
30psig, 50psig, 75psig, 90psig, 90psig, when being passed through regeneration ammonia, in adsorption column, temperature is 50 DEG C every time；Finally
The pressure 50psig in adsorption column is kept, until temperature is 50 DEG C in adsorption column after being once passed through regeneration ammonia；Finally discharge again
Ammonifying gas, to complete No. four adsorption column regeneration；
(5) hot nitrogen lead to superheated nitrogen entrance No. five adsorption columns are carried out displacement purging, heating-up temperature use staged rise, 50
DEG C, 100 DEG C, 150 DEG C, 200 DEG C, the mode of 250 DEG C heats, until the top and bottom temperature of adsorption column reaches 250 DEG C
And maintain 4 hours；Keeping nitrogen pressure 15psig in adsorption column, natural cooling reaches 35 DEG C；Remove adsorption column external heat preserving device
To lower the temperature quickly to reach temperature required；Being passed through regeneration ammonia in adsorption column in seven times, the speed being passed through is successively
5psig, 15psig, 30psig, 50psig, 75psig, 90psig, 90psig, when being passed through regeneration ammonia every time, temperature in adsorption column
Degree is 40 DEG C；The pressure 50psig in adsorption column is kept, until temperature is 40 in adsorption column after being passed through regeneration ammonia for the last time
℃；Finally discharge regeneration ammonia, to complete No. five adsorption column regeneration；
(6) hot nitrogen lead to superheated nitrogen entrance No. six adsorption columns are carried out displacement purging, heating-up temperature use staged rise, 50
DEG C, 100 DEG C, 150 DEG C, 200 DEG C, the mode of 250 DEG C heats, until the top and bottom temperature of adsorption column reaches 250 DEG C
And maintain 4 hours；Keeping nitrogen pressure 15psig in adsorption column, natural cooling reaches 40 DEG C；Remove adsorption column external heat preserving device
To lower the temperature quickly to reach temperature required；Being passed through regeneration ammonia in adsorption column in seven times, the speed being passed through is successively
5psig, 15psig, 30psig, 50psig, 75psig, 90psig, 90psig, when being passed through regeneration ammonia every time, temperature in adsorption column
Degree is 40 DEG C；The pressure 50psig in adsorption column is kept, until temperature is 40 in adsorption column after being passed through regeneration ammonia for the last time
℃；Finally discharge regeneration ammonia, to complete No. six adsorption column regeneration.
With an adsorption column as first class absorber, with No. three adsorption columns as second class absorber, it it is three grades with No. five adsorption columns
Adsorber, is controlled by valve switch, can carry out when carrying out ammonia and purifying No. two adsorption columns, No. four adsorption columns, six
The Regeneration Treatment of number adsorption column；Raw material ammonia is passed through an adsorption column through raw material ammonia inlet pipe, enters back into No. two adsorption columns and enters
Row primary adsorption, removes in raw material ammonia the impurity such as substantial amounts of moisture content, oils and fats, dust, particulate matter；Subsequently into No. three absorption
Post, enters back into No. four adsorption columns and carries out secondary absorption, to remove the gaseous impurities such as residue moisture content, sulfide, carbon dioxide；Finally
Enter No. five adsorption columns, enter back into No. six adsorption columns and carry out the absorption of three grades of degree of depth, remove moisture content a small amount of in ammonia, sulfide and
Carbon dioxide.Ammonia after thtee-stage shiplock adsorbs can reach 99.999% and above purity；Adsorbed by this valve method
The high purity ammonia gas impurity content purified is as shown in table 1.
Major impurity component and content in table 1 high-purity ammon
Embodiment four
Adsorption column Regeneration Treatment is with embodiment three, ammonia purification step difference, with an adsorption column and No. two adsorption columns
For first class absorber, with No. three adsorption columns and No. four adsorption columns as second class absorber, with No. five adsorption columns and No. six adsorption columns it is
Three grades of adsorbers, carry out a series connection to No. six adsorption columns by valve switch；Can effectively be removed by the inventive method
The objectionable impurities such as oxygen in raw material ammonia (99.8%), nitrogen, carbon dioxide, water, sulfide, the high-purity ammonia total impurities after removal
Content is less than 5ppm, can meet the demand of client, the most also can purify for the ammonia of higher purity and prepare.
Claims (10)
1. one kind adsorbs the device purifying ammonia step by step, it is characterised in that: include an adsorption column, No. two adsorption columns, No. three suctions
Attached column, No. four adsorption columns, No. five adsorption columns, No. six adsorption columns；
A described adsorption column connects with No. two adsorption columns, No. three adsorption columns, No. four adsorption columns respectively；Described No. two adsorption columns divide
Do not connect with No. three adsorption columns, No. four adsorption columns；Described No. three adsorption columns respectively with No. four adsorption columns, No. five adsorption columns, No. six
Adsorption column connects；Described No. four adsorption columns connect with No. five adsorption columns, No. six adsorption columns respectively；Described No. five adsorption columns and No. six
Adsorption column connects；
A described adsorption column includes an adsorption column housing and is positioned at the porous ceramics absorption dress of an adsorption column housing
Put；Described No. two adsorption columns include No. two adsorption column housings and are positioned at the porous ceramics absorption dress of No. two adsorption column housings
Put；Described No. three adsorption columns include No. three adsorption column housings and are positioned at the first molecular sieve of No. three adsorption column housings；Described
No. four adsorption columns include No. four adsorption column housings and are positioned at the second molecular sieve of No. four adsorption column housings；Described No. five absorption
Post includes No. five adsorption column housings and is positioned at the type three-molecular screen alternating of No. five adsorption column housings；Described No. six adsorption columns include six
Number adsorption column housing and be positioned at the 4th molecular sieve of No. six adsorption column housings；
A described adsorption column, No. two adsorption columns are connected to raw material ammonia inlet pipe respectively；Described No. five adsorption columns, No. six adsorption columns divide
It is not connected to high-purity ammonia and goes out pipe；Each adsorption column is respectively equipped with sewage draining exit, regeneration ammonia entrance and hot nitrogen entrance；
The aperture of described first molecular sieve is more than or equal to the aperture of described second molecular sieve；The aperture of described second molecular sieve is more than
The aperture of described type three-molecular screen alternating；The aperture of described type three-molecular screen alternating is more than or equal to the aperture of described 4th molecular sieve.
Absorption step by step the most according to claim 1 purifies the device of ammonia, it is characterised in that: described hot nitrogen entrance and blowdown
Mouth is respectively at the top and bottom of each adsorption column.
The most according to claim 1 step by step absorption purify ammonia device, it is characterised in that: described regeneration ammonia entrance with
High-purity ammonia goes out pipe connection.
The most according to claim 1 step by step absorption purify ammonia device, it is characterised in that: described raw material ammonia inlet pipe with
And high-purity ammonia goes out pipe and is respectively equipped with valve；It is provided with valve between the adsorption column of two connections.
Absorption step by step the most according to claim 1 purifies the device of ammonia, it is characterised in that: a described adsorption column top
Respectively with bottom No. two adsorption columns, bottom No. three adsorption columns, connect bottom No. four adsorption columns；Described No. two adsorption column tops are respectively
With bottom No. three adsorption columns, connect bottom No. four adsorption columns；Described No. three adsorption column tops respectively with No. four adsorption columns bottom, five
Connect bottom number adsorption column, bottom No. six adsorption columns；Described No. four adsorption column tops respectively with No. five adsorption columns bottom, No. six suctions
Connect bottom attached column；Described No. five adsorption column tops connect bottom No. six adsorption columns；Described raw material ammonia inlet pipe is respectively with one
Connecting bottom number adsorption column, No. two adsorption columns, described high-purity ammonia goes out pipe respectively with No. five adsorption columns, No. six adsorption column tops even
Connect.
Absorption step by step the most according to claim 1 purifies the device of ammonia, it is characterised in that: described adsorption column lateral wall sets
There is attemperator；Described adsorption column is provided with temperature sensor.
Absorption step by step the most according to claim 1 purifies the device of ammonia, it is characterised in that: described porous ceramics absorption dress
The filtering accuracy put is 0.05～0.1 micron, and the model of the first molecular sieve and the second molecular sieve is all 13X, type three-molecular screen alternating with
The model of the 4th molecular sieve is all 4A.
8. utilize the absorption step by step described in claim 1 to purify the method that the device of ammonia carries out ammonia purification, it is characterised in that
Comprise the following steps:
(1) with an adsorption column and/or No. two adsorption columns as first class absorber；With No. three adsorption columns and/or No. four adsorption columns it is
Second class absorber；It is three grades of adsorbers with No. five adsorption columns and/or No. six adsorption columns；Respectively to an adsorption column, No. two absorption
Post, No. three adsorption columns, No. four adsorption columns, No. five adsorption columns, No. six adsorption columns carry out Regeneration Treatment；
The Regeneration Treatment of a described adsorption column is, in utilizing the heating of hot nitrogen to make an adsorption column, temperature reaches 250 DEG C, then
It is incubated 4 hours；Then, under in an adsorption column, gas pressure is 15psig, adjusting temperature in an adsorption column is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in a number adsorption column is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of an adsorption column；
The Regeneration Treatment of described No. two adsorption columns is, in utilizing the heating of hot nitrogen to make No. two adsorption columns, temperature reaches 250 DEG C, then
It is incubated 4 hours；Then, under in No. two adsorption columns, gas pressure is 15psig, adjusting temperature in No. two adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. two adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. two adsorption columns；
The Regeneration Treatment of described No. three adsorption columns is, in utilizing the heating of hot nitrogen to make No. three adsorption columns, temperature reaches 150 DEG C, then
It is incubated 2 hours；Then, under in No. three adsorption columns, gas pressure is 15psig, adjusting temperature in No. three adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. three adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. three adsorption columns；
The Regeneration Treatment of described No. four adsorption columns is, in utilizing the heating of hot nitrogen to make No. four adsorption columns, temperature reaches 150 DEG C, then
It is incubated 2 hours；Then, under in No. four adsorption columns, gas pressure is 15psig, adjusting temperature in No. four adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. four adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. four adsorption columns；
The Regeneration Treatment of described No. five adsorption columns is, in utilizing the heating of hot nitrogen to make No. five adsorption columns, temperature reaches 250 DEG C, then
It is incubated 2 hours；Then, under in No. five adsorption columns, gas pressure is 15psig, adjusting temperature in No. five adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. five adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. five adsorption columns；
The Regeneration Treatment of described No. six adsorption columns is, in utilizing the heating of hot nitrogen to make No. six adsorption columns, temperature reaches 250 DEG C, then
It is incubated 4 hours；Then, under in No. six adsorption columns, gas pressure is 15psig, adjusting temperature in No. six adsorption columns is 35 DEG C～45
℃；Then passing to regenerate ammonia, keeping gas pressure in No. six adsorption columns is 50psig, until temperature in adsorption column be 35 DEG C～
45℃；Finally discharge regeneration ammonia, complete the Regeneration Treatment of No. six adsorption columns；
(2) first class absorber after raw material ammonia sequentially enters Regeneration Treatment, the second class absorber after Regeneration Treatment, Regeneration Treatment
After three grades of adsorbers, complete ammonia purify.
Method the most according to claim 8, it is characterised in that: utilize the heating of hot nitrogen ladder to make temperature in an adsorption column
Reaching 250 DEG C, ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C；The heating of hot nitrogen ladder is utilized to make No. two
In adsorption column, temperature reaches 250 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C；Utilize hot nitrogen ladder
In heating makes No. three adsorption columns, temperature reaches 150 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C；Utilize hot nitrogen ladder
In heating makes No. four adsorption columns, temperature reaches 150 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C；Utilize hot nitrogen ladder
In heating makes No. five adsorption columns, temperature reaches 250 DEG C, and ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C；
In utilizing the heating of hot nitrogen ladder to make No. six adsorption columns, temperature reaches 250 DEG C, ladder heating-up temperature is 50 DEG C, 100 DEG C, 150 DEG C,
200℃、250℃。
Method the most according to claim 8, it is characterised in that: all adsorption columns are passed through regeneration ammonia the most in seven times；Described
Be passed through for seven times regeneration ammonia pressure be followed successively by 5psig, 15psig, 30psig, 50psig, 75psig, 90psig,
90psig。
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Application publication date: 20170111 |