CN102774857B - High purity ammonia making in site method and manufacturing installation - Google Patents
High purity ammonia making in site method and manufacturing installation Download PDFInfo
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- CN102774857B CN102774857B CN201210142456.2A CN201210142456A CN102774857B CN 102774857 B CN102774857 B CN 102774857B CN 201210142456 A CN201210142456 A CN 201210142456A CN 102774857 B CN102774857 B CN 102774857B
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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
- C01C1/10—Separation of ammonia from ammonia liquors, e.g. gas liquors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D37/00—Processes of filtration
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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- Inorganic Chemistry (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention relates to high purity ammonia making in site method and manufacturing installation, it is a kind of manufacture and supply of summary of high purity ammonia, the present invention is made up of the device for refining that high purity ammonia (99.999%) is produced ultra-high purity (more than 99.99999%) product by adsorber and the on-the-spot feedway that is supplied to user side after evaporating this product, wherein, this high purity (99.999%) ammonia is by storing low-purity (99.7%) raw material in the jumbo vertical-type tank of multiple more piece; The high-boiling-point impurities such as moisture, hydrogen sulfide, carbonic acid gas are separated by the increasing apparatus being arranged on tank itself; The technique of repeatedly being carried out the liquefaction-lower-boiling impurity such as evaporation technology separation carbon monoxide, methane etc. of ammonia by multiple heat exchanger is extracted.
Description
Technical field
The present invention relates to a kind of high purity ammonia making in site method and manufacturing installation (Methodand apparatus for onsite production of high purity ammonia), particularly relate to and can (Onsite) directly manufacture and the method for supplying high purity ammonia and device at the scene.
Background technology
Along with the development rapidly of domestic and international semiconductor industry and LED manufacturing industry, the usage quantity of high purity ammonia sharply increases.Usual high purity ammonia is filled with supply in various container (container of the container of 47L, the container of 470L, 930L, ISO tank) after being produced by gas manufacturer, and therefore current situation consumes too much container expense and logistics cost.
The refinement mode of the high purity ammonia of usual employing has the mode of the sorbent material utilizing the distillation mode of prilling tower and selectivity applying portion to dissolve.
But aforesaid way causes the rising of unnecessary capital cost, therefore limits economic capability, and builds charging device in addition, supplied by the mode departing from scene (offline), therefore unreasonable, and non-efficiency.
Grant number be 584686 Korean Patent disclose high purity (99.99995%) the Large Copacity process for extracting of metallic impurity, gaseous impurities, moisture and oil content etc. refining raw material ammonia and contain.The method is made up of following technique, stores the technique of low-purity (99.7%) raw material in horizontal type raw material storage tank; To be vaporized by vaporizer the technique of this raw material; It is made to remove the technique of the impurity such as moisture through adsorbent; The technique of high-boiling-point impurity is separated by distillation tower.That is, by 1) horizontal type raw material storage tank (raw material supplying) → 2) vaporizer (evaporation) → 3) sorbent material (adsorbing contaminant) → 4) distillation tower (separation high-boiling-point impurity) → 5) heat exchanger (liquefaction) → 6) vapor-liquid separation → 7) products pot (storage) forms.
But the mode of above-mentioned patent is, owing to there being the phenomenon of contamination precipitation and accumulation in raw material storage tank, therefore consumes too much overheads and cost of upkeep, can be described as irrational mode.
Further, other mode has, grant number be 591521 Korean Patent disclose the method for being refined high purity ammonia by liquid adsorption bed, but the refining technique as ultra-high purity ammonia (99.99999%) is not talkative is reasonable manner.
Summary of the invention
The technical issues that need to address
Therefore, the present invention is to solve the technical scheme that in prior art, irrational problem discloses, its object is to, a kind of making in site method and manufacturing installation of high purity ammonia are provided, apply in ground using the user of a certain amount of above high purity ammonia or adjacent deposited ground builds the manufacturing installation of high purity ammonia, can scene (Online) supplying high purity ammonia by streamline (Pipe line).
Technical scheme
A kind of high purity ammonia making in site device is the invention provides in order to reach above-mentioned purpose, it comprises: raw material storage tank, and it stores and stabilization low-purity ammonia liquid raw material, thus forms impurity layer, and itself has heater means, therefore carry out first time impurity refinement by distillation; First heat exchanger, it is connected to the steam state raw material that raw material storage tank liquefaction is refined for the first time; First reboiler, it is connected to the first heat exchanger, stores the liquid raw material that also stabilization is refined for the first time, thus forms impurity layer, and have heater means due to itself, therefore carries out second time impurity by distillation and refines; Adsorber, it is connected to the first reboiler, and the raw material be refined by absorption second time carries out third time impurity refinement; Second heat exchanger, it is connected to the steam state raw material that adsorber liquefaction is refined for the third time; Second reboiler, it is connected to the second heat exchanger and stores and the stabilization liquid raw material that is refined of third time, thus forms impurity layer, and has heater means due to itself, therefore carries out the 4th impurity by distillation and refines; And product storage tank, it is connected to the second reboiler and stores and the raw material that is refined for the 4th time of stabilization, thus forms impurity layer, and has heater means due to itself, therefore carries out the 5th impurity by distillation and refines.
According to device for refining Large Copacity vertical-type storage tank itself of the present invention, impurity, oil content and the metallic impurity such as hydrogen sulfide, carbon monoxide, carbonic acid gas, moisture, oxygen and the nitrogen comprised in the feed are stably isolated with simple technique and cheap expense, thus produce ultra-high purity (99.99999%) ammonolysis product, and this product stably can be supplied to a large amount of client using ultra-high purity ammonia by on-the-spot (Onsite) mode.
Manufacturing installation according to present pre-ferred embodiments also comprises waste gas recovery tank, and it is connected to raw material storage tank and reclaims waste gas; 3rd reboiler, it is connected to the second reboiler, again carries out impurity refinement by distillation; For reclaiming heat exchanger and the impurity withdrawing can of impurity, it is connected to the first reboiler, the second reboiler, the 3rd reboiler and product storage tank and reclaims impurity; Heating medium feeder, it is connected to raw material storage tank, the first reboiler, the second reboiler, the 3rd reboiler and product storage tank, supply heating medium; Vaporizer, it is connected to product storage tank, vaporization high purity ammonia product; Vapour liquid separator, it is connected to vaporizer, the liquid state in product separation; And streamline, it is connected to vapour liquid separator and is directly supplied to user.
In the deposited ground being arranged on user according to all devices of manufacturing installation of the present invention or adjacent depositedly for better, thus can directly be supplied to user side high purity ammonia at the scene.
According in manufacturing installation of the present invention, raw material storage tank, the first reboiler, the second reboiler and product storage tank can by first groups, and it realizes raw material storage and stabilization; And second group, it realizes multiple groups of formations of distillation, and adsorber also can by first group, and it realizes the absorption of hydrogen sulfide; And second group, it realizes multiple groups of formations of the absorption of carbonic acid gas.
According in manufacturing installation of the present invention, in raw material storage tank and the first reboiler, the preferred temperature of heating medium is 30 to 40 DEG C, and the better pressure of container is 130 to 150psig; In first heat exchanger, the preferred temperature of heat-eliminating medium is-15 to-20 DEG C; In second heat exchanger, the preferred temperature of heat-eliminating medium is-5 to-10 DEG C.
Further, the invention provides a kind of high purity ammonia making in site method, it is included in raw material storage tank and stores and stabilization low-purity ammonia liquid raw material, thus after forming impurity layer, carries out by distillation the step that first time refines impurity; The step of the steam state raw material that liquefaction is refined for the first time in the first heat exchanger; In the first reboiler, store the liquid raw material that also stabilization is refined for the first time, thus after forming impurity layer, carried out the step of second time refinement impurity by distillation; The raw material be refined by absorption second time in adsorber carries out the step of third time refinement; The step of the steam state raw material that liquefaction is refined for the third time in the second heat exchanger; In the second reboiler, store the liquid raw material that also stabilization is refined for the third time, thus after forming impurity layer, carry out the 4th impurity step of refining by distillation; And store in product storage tank and the raw material that is refined for the 4th time of stabilization, thus after forming impurity layer, carry out by distillation the step that the 5th time is refined impurity.
According to the manufacture method of present pre-ferred embodiments, also comprise the step of the waste gas reclaiming raw material storage tank with waste gas recovery tank; The step of refining impurity is again carried out by distillation in the 3rd reboiler; The step of impurity is reclaimed from the first reboiler, the second reboiler, the 3rd reboiler and product storage tank; To the step of raw material storage tank, the first reboiler, the second reboiler, the 3rd reboiler and product storage tank supply heating medium; The step of high purity ammonia of vaporizing in vaporizer product; The step of liquid in product is isolated in vapour liquid separator; And by the step of streamline to user side supplying products.
Manufacturing method according to the invention, in raw material storage tank, the first reboiler, the second reboiler and product storage tank, stabilization more than 24 hours is better.Thus, isolate impurity layer in raw material, can separation efficiency be improved.
Beneficial effect
The present invention can according to simple technique, low-purity (about 99.7%) ammonia is refined the product stage to ultra-high purity (99.99999%) by cheap expense.
Especially, eliminate and the product that completes extracted as mentioned above is filled with the irrationality supplied to various container class, user side is supplied to according to on-the-spot (Onsite) mode, thus contribute to the minimizing of physical distribution expenses, the minimizing of capital cost, the stability of supplying products, therefore can make the supplier of high purity product and the competitive power multiplication of user.
Accompanying drawing explanation
Fig. 1 is the integrally-built schematic diagram of the high purity ammonia making in site device according to present pre-ferred embodiments;
Fig. 2 is the enlarged view of tank car, raw material storage tank and waste gas recovery tank in Fig. 1;
Fig. 3 is the enlarged view for the heat exchanger and impurity withdrawing can that reclaim impurity in Fig. 1;
Fig. 4 is the enlarged view of the first heat exchanger in Fig. 1 and the first reboiler;
Fig. 5 is the enlarged view of adsorber, the second heat exchanger, the second reboiler and the 3rd reboiler in Fig. 1;
Fig. 6 is the enlarged view of product storage tank, vaporizer and vapour liquid separator in Fig. 1.
Embodiment
Below, the present invention is described in detail with reference to accompanying drawing.
Fig. 1 is the integrally-built schematic diagram of the high purity ammonia making in site device according to present pre-ferred embodiments; Fig. 2 to Fig. 6 is the enlarged view of each several part.
By for the tank car 1 of base feed, raw material storage tank 2, waste gas recovery tank 3, first heat exchanger 4, first reboiler 5, first adsorber 6, second adsorber 7, second heat exchanger 8, second reboiler 9, the 3rd reboiler 10, product storage tank 11, vaporizer 12, vapour liquid separator 13, for reclaiming the heat exchanger 14 of impurity, impurity withdrawing can 15 and heating medium feeder 16 etc. form according to the high purity ammonia making in site device of present pre-ferred embodiments.
Tank car 1 for base feed is as feedstock transportation and supply mean, and carrying low-purity ammonia raw material supplying is to raw material storage tank 2.
Raw material storage tank 2 plays the effect storing low-purity ammonia liquid raw material, also plays stabilization raw material simultaneously, thus form the effect of impurity layer, and have heater means due to itself, therefore also plays by distilling the effect of carrying out refining for the first time.That is, as shown in table 1, raw material storage tank 2 is except having the function as storage tank, and the part as refining technique also plays the effect of stabilization device, distiller.
Table 1
Raw material storage tank 2 is classified according to above-mentioned 3 kinds of effects, can be made up of multiple.Such as, can be made up of the tank of more than at least 2, it comprises the first tank of storage and the stabilization realizing raw material, realizes the second tank of distillation, and above-mentioned tank preferably mode of connection is connect side by side.As mentioned above, raw material storage tank 2 can be made up of the jumbo vertical-type tank of multiple more piece, can be separated the high-boiling-point impurities such as moisture, hydrogen sulfide, carbonic acid gas by the increasing apparatus being arranged on tank itself.In addition, in order to separating impurity, stablize and within more than 24 hours, be filled with to the low-purity ammonia in raw material storage tank 2 as better.
Heater means in order to distill can be set in the inside of raw material storage tank 2 and/or outside, such as heating jacket.This heater means can pass through the heating medium heating raw storage tanks 2 such as circulation warm water, hot water and steam, and heating medium can be supplied by heating medium feeder 16.The supplying temperature of heating medium should 30 to 40 DEG C of scope supplies, and the maintenance pressure of raw material storage tank 2 should maintain the scope of 130 to 150psig.As mentioned above, raw material storage tank 2 is constructed by the steam/vapourizing unit of warm water or steam, and the function that can be applied as distillation tower is refined.
Waste gas recovery tank 3 is connected to raw material storage tank 2 etc., reclaims the waste gas that it produces.
First heat exchanger 4 is connected to raw material storage tank 2, plays the effect of the steam state raw material that liquefaction is refined for the 1st time.The general heat exchanger flowing through the heat-eliminating mediums such as water coolant can be used as the first heat exchanger 4.The water coolant be supplied on the first heat exchanger 4 supplies with the temperature of-15 to-20 DEG C, makes the moisture of solidification or liquefaction steam-like, can realize refining function with this.
First reboiler 5 is connected to the first heat exchanger 4, plays the liquid raw material storing also stabilization and be refined for the first time, thus forms impurity layer, and have heater means due to itself, therefore carried out the effect of impurity refinement for the second time by distillation.That is, the first reboiler 5 plays 3 kinds of effects of storage tank, stabilizer and distiller as raw material storage tank 2, therefore can have the structure identical or similar with raw material storage tank 2.Should supply with 30 to 40 DEG C of scopes the supplying temperature of the heating medium of the first reboiler 5, maintain pressure and should maintain 130 to 150psig scope.
From raw material storage tank 2 to the first reboiler 5, the impurity component evaporated by stabilization and distilation steps is as shown in table 2.
Table 2
First adsorber 6 and the second adsorber 7 are connected to the first reboiler 5, play the effect that the raw material be refined by absorption second time carries out third time refinement.As shown in the figure, adsorber provided by the invention is configured to better according to effect is different by more than at least 2 adsorbers, and such as, the first adsorber 6 can realize the absorption of hydrogen sulfide; Second adsorber 7 can realize the absorption of carbonic acid gas, and as shown in the figure, the first above-mentioned adsorber 6 and the preferably mode of connection of the second adsorber 7 are for being connected in series.Sorbent material as hydrogen sulfide can use the mixture and molecular sieve (molecular sieve) 5A etc. of single metal oxide, metal oxide; Sorbent material as carbonic acid gas can use molecular sieve 13X etc.
Second heat exchanger 8 is connected to the second adsorber 7, plays the effect of the steam state raw material that liquefaction third time is refined.Second heat exchanger 8 can have the structure identical or similar with the first heat exchanger 4.In second heat exchanger 8, the preferred temperature of heat-eliminating medium is-5 to-10 DEG C.
Second reboiler 9 is connected to the second heat exchanger 8, plays the liquid raw material storing also stabilization and be refined for the third time, thus forms impurity layer, and have heater means due to itself, therefore carried out the effect of the 4th impurity refinement by distillation.Second reboiler 9 plays 3 kinds of effects of storage tank, stabilizer and distiller as the first reboiler 5, therefore can have the structure identical or similar with the first reboiler 5.
3rd reboiler 10 is connected to the second reboiler 9, plays and again carries out by distillation the effect that impurity refines impurity.
Product storage tank 11 is connected to the second reboiler 9, plays the raw material storing also stabilization and be refined for the 4th time, thus forms impurity layer, and have heater means due to itself, therefore carry out by distillation the effect that the 5th time impurity refines.That is, product storage tank 11 plays 3 kinds of functions of storage tank, stabilizer and distiller as raw material storage tank 2, therefore can have the structure identical or similar with raw material storage tank 2.
Vaporizer 12 is connected to product storage tank 11, plays the effect carrying out vaporizing before high purity ammonia supplying products to user.
Vapour liquid separator 13 is connected to vaporizer 12, plays effect liquid in product separation.Concrete, play the effect being separated from the finished product and removing liquid ammonia.Buffer tube (Buffer Tube) can be used as vapour liquid separator 13.
Being be connected to the first reboiler 5, second reboiler 9, the 3rd reboiler 10 and product storage tank 11 etc. as recovering means for reclaiming heat exchanger 14 and the impurity withdrawing can 15 of impurity, playing the effect of reclaiming impurity.As mentioned above, be recovered in by recovery system 14,15 impurity produced in refining technique, can improve and refine efficiency, increase yield.
Heating medium feeder 16 is connected to raw material storage tank 2, first reboiler 5, second reboiler 9, the 3rd reboiler 10 and product storage tank 11, plays the effect of supply and circulating-heating medium.
Finally, streamline is connected to vapour liquid separator 13, will directly to user's supplying products.
Above-mentioned all devices be arranged at a large amount of to use in the deposited ground of user's (client company) of high purity ammonia or adjacent be better setting depositedly, therefore can at the scene directly to user's supplying high purity ammonia.
Said apparatus is utilized to manufacture being described as follows of the manufacture method of high purity ammonia.
One, the first step refining technique (as Fig. 1 and Fig. 2): inject low-purity (about 99.7%) raw material to multiple raw material storage tank 2 intersection by tank car 1.Now, such as, in first raw material storage tank, realize evaporation (Vaporizing) distillation, realize storing and stabilization in second raw material storage tank, thus form impurity layer.Under the state injecting raw material in raw material storage tank 2, in order to form impurity layer, stabilization 24 hours.Warm water or steam raising/vaporization raw material are utilized to the raw material storage tank 2 being formed with impurity layer.Now, the impurity such as distillation metallic impurity, oil component, moisture, hydrogen sulfide and carbonic acid gas, thus refine the purity to 99.95%.
Two, second step refining technique (as Fig. 1 and Fig. 4): liquefy after the purity of producing in the first step refining technique is the ammonia of 99.95% by the first heat exchanger 4, be stored in the first reboiler 5.First reboiler 5 can crossing operation, such as, in first and second reboiler, realizes distillation, realizes storing and stabilization, thus form impurity layer in the 3rd and the 4th reboiler.In the first reboiler 5 liquefied ammonia state under, in order to form impurity layer, then stablize 24 hours.To the first reboiler 5 being formed with impurity layer, utilize warm water or steam raising/ammonia vaporised raw material.Now, second time distills the impurity such as metallic impurity, oil component, moisture, hydrogen sulfide and carbonic acid gas, thus refines the purity to 99.995%.Then deliver to after magazins' layout for reclaiming in the heat exchanger 14 of impurity.
Three, the 3rd step refining technique (as Fig. 1 and Fig. 5): contain residual impurity in moderate purity (99.9995%) ammonia of second step refining technique, in order to remove hydrogen sulfide in this residual impurity and carbonic acid gas, make its first adsorber 6 and the second adsorber 7 through being made up of adsorption column.Sorbent material containing specific blend metal oxide component or molecular sieve 5A can be used to remove hydrogen sulfide; Molecular sieve 13X can be used to remove carbonic acid gas.Now, due to conventional most of sorbent material, from its performance, generally realize the removal of moisture simultaneously.
Four, the 4th step refining technique (as Fig. 1 and Fig. 5): liquefy after the high purity ammonia (99.9999%) that adsorber 6,7 is refined by the second heat exchanger 8, be stored in the second reboiler 9.Second reboiler 9 can crossing operation, such as, realizes distillation in first reboiler, realizes storing and stabilization, thus form impurity layer in second reboiler.Utilize warm water or steam raising/vaporization to be stored in ammonia in the second reboiler 9, thus isolate oxygen, nitrogen, carbon monoxide, methane and the hydrogen etc. in residual impurity, and deliver to for reclaiming in the heat exchanger 14 of impurity.Now, a certain amount of liquefied ammonia in the second reboiler 9 is transplanted in the 3rd reboiler 10, again refines or deliver in retrieving arrangement 14,15.
Five, the 5th step refining technique (as Fig. 1 and Fig. 6): transfer to product storage tank 11 and store the ultra-high purity ammonia (99.99999%) having reclaimed impurity.Product storage tank 11 can crossing operation, such as, realizes distillation in first product storage tank, realizes storing and stabilization, thus form impurity layer in second product storage tank.Warm water or steam raising/vaporization is utilized to be stored in the liquefied ammonia of the ultra-high purity ammonia (99.99999%) in product storage tank 11, thus oxygen, nitrogen, carbon monoxide, methane and the hydrogen etc. isolated in residual impurity, deliver to for reclaiming in the heat exchanger 14 of impurity.
According to the product that above-mentioned technique extracts, its main quality is as shown in table 3.
Table 3
Six, on-the-spot supplying step (as Fig. 1 and Fig. 6): evaporated the ultra-high purity ammonia (99.99999%) finally eliminating impurity by vaporizer 12.The ammonia of liquefaction can be comprised by the ammonia of vaporizer 12, in order to prevent being mixed into of the ammonia of this liquefaction, making it through vapour liquid separator 13, thus after separation of liquid, being directly supplied to user side eventually through streamline.
Bis explanation
1, for the tank car of base feed; 2, raw material storage tank; 3, waste gas recovery tank; 4, the first heat exchanger; 5, the first reboiler; 6, the first adsorber; 7, the second adsorber; 8, the second heat exchanger; 9, the second reboiler; 10, the 3rd reboiler; 11, product storage tank; 12, vaporizer; 13, vapour liquid separator; 14, for reclaiming the heat exchanger of impurity; 15, impurity withdrawing can; 16, heating medium feeder.
Claims (11)
1. a high purity ammonia making in site device, it comprises:
Raw material storage tank, it stores and stabilization low-purity ammonia liquid raw material, thus forms impurity layer, and itself has heater means, therefore carries out first time impurity refinement by distillation;
First heat exchanger, it is connected to the steam state raw material that raw material storage tank liquefaction is refined for the first time;
First reboiler, it is connected to the first heat exchanger, stores the liquid raw material that also stabilization is refined for the first time, thus forms impurity layer, and have heater means due to itself, therefore carries out second time impurity by distillation and refines;
Adsorber, it is connected to the first reboiler, and the raw material be refined by absorption second time is carried out third time and refines;
Second heat exchanger, it is connected to the steam state raw material that adsorber liquefaction is refined for the third time;
Second reboiler, it is connected to the second heat exchanger, stores the liquid raw material that also stabilization is refined for the third time, thus forms impurity layer, and have heater means due to itself, therefore carries out the 4th impurity by distillation and refines; And
Product storage tank, it is connected to the second reboiler, stores the raw material that also stabilization is refined for the 4th time, thus forms impurity layer, and have heater means due to itself, therefore carries out the 5th impurity by distillation and refines,
It is characterized in that,
Described adsorber is formed by following multiple groups:
First group, it realizes the absorption of hydrogen sulfide; And
Second group, it realizes the absorption of carbonic acid gas.
2. a kind of high purity ammonia making in site device according to claim 1, also comprises: waste gas recovery tank, and it is connected to raw material storage tank and reclaims waste gas;
3rd reboiler, it is connected to the second reboiler, again carries out impurity refinement by distillation;
For reclaiming heat exchanger and the impurity withdrawing can of impurity, it is connected to the first reboiler, the second reboiler, the 3rd reboiler and product storage tank and reclaims impurity;
Heating medium feeder, it is connected to raw material storage tank, the first reboiler, the second reboiler, the 3rd reboiler and product storage tank, supply heating medium;
Vaporizer, it is connected to product storage tank, vaporization high purity ammonia product;
Vapour liquid separator, it is connected to vaporizer, the liquid state in product separation; And
Streamline, it is connected to vapour liquid separator, is directly supplied to user.
3. a kind of high purity ammonia making in site device according to claim 1 and 2, is characterized in that, in the deposited ground that described all devices are arranged on user or adjacent deposited ground.
4. a kind of high purity ammonia making in site device according to claim 1, is characterized in that, described raw material storage tank, the first reboiler, the second reboiler and product storage tank by
First group, it realizes raw material storage and stabilization; And
Second group, it realizes multiple groups of formations of distillation.
5. a high purity ammonia making in site device, it comprises:
Raw material storage tank, it stores and stabilization low-purity ammonia liquid raw material, thus forms impurity layer, and itself has heater means, therefore carries out first time impurity refinement by distillation;
First heat exchanger, it is connected to the steam state raw material that raw material storage tank liquefaction is refined for the first time;
First reboiler, it is connected to the first heat exchanger, stores the liquid raw material that also stabilization is refined for the first time, thus forms impurity layer, and have heater means due to itself, therefore carries out second time impurity by distillation and refines;
Adsorber, it is connected to the first reboiler, and the raw material be refined by absorption second time is carried out third time and refines;
Second heat exchanger, it is connected to the steam state raw material that adsorber liquefaction is refined for the third time;
Second reboiler, it is connected to the second heat exchanger, stores the liquid raw material that also stabilization is refined for the third time, thus forms impurity layer, and have heater means due to itself, therefore carries out the 4th impurity by distillation and refines; And
Product storage tank, it is connected to the second reboiler, stores the raw material that also stabilization is refined for the 4th time, thus forms impurity layer, and have heater means due to itself, therefore carries out the 5th impurity by distillation and refines,
It is characterized in that,
In described raw material storage tank and the first reboiler, the temperature of heating medium is 30 to 40 DEG C, and container pressure is 130 to 150psig,
In described first heat exchanger, the temperature of heat-eliminating medium is-15 to-20 DEG C,
In described second heat exchanger, the temperature of heat-eliminating medium is-5 to-10 DEG C.
6. a kind of high purity ammonia making in site device according to claim 5, also comprises: waste gas recovery tank, and it is connected to raw material storage tank and reclaims waste gas;
3rd reboiler, it is connected to the second reboiler, again carries out impurity refinement by distillation;
For reclaiming heat exchanger and the impurity withdrawing can of impurity, it is connected to the first reboiler, the second reboiler, the 3rd reboiler and product storage tank and reclaims impurity;
Heating medium feeder, it is connected to raw material storage tank, the first reboiler, the second reboiler, the 3rd reboiler and product storage tank, supply heating medium;
Vaporizer, it is connected to product storage tank, vaporization high purity ammonia product;
Vapour liquid separator, it is connected to vaporizer, the liquid state in product separation; And
Streamline, it is connected to vapour liquid separator, is directly supplied to user.
7. a kind of high purity ammonia making in site device according to claim 5 or 6, is characterized in that, in the deposited ground that described all devices are arranged on user or adjacent deposited ground.
8. a kind of high purity ammonia making in site device according to claim 5, is characterized in that, described raw material storage tank, the first reboiler, the second reboiler and product storage tank by
First group, it realizes raw material storage and stabilization; And
Second group, it realizes multiple groups of formations of distillation.
9. a high purity ammonia making in site method, it comprises:
Store and stabilization low-purity ammonia liquid raw material in raw material storage tank, thus after forming impurity layer, carry out by distillation the step that first time refines impurity;
The step of the steam state raw material that liquefaction is refined for the first time in the first heat exchanger;
In the first reboiler, store the liquid raw material that also stabilization is refined for the first time, thus after forming impurity layer, carried out the step of second time refinement impurity by distillation;
The raw material be refined by absorption second time in adsorber carries out the step of third time refinement;
The step of the steam state raw material that liquefaction is refined for the third time in the second heat exchanger;
In the second reboiler, store the liquid raw material that also stabilization is refined for the third time, thus after forming impurity layer, carry out the 4th impurity step of refining by distillation; And
In product storage tank, store the raw material that also stabilization is refined for the 4th time, thus after forming impurity layer, carry out by distillation the step that the 5th time is refined impurity,
It is characterized in that,
In described raw material storage tank and the first reboiler, the temperature of heating medium is 30 to 40 DEG C, and container pressure is 130 to 150psig,
In described first heat exchanger, the temperature of heat-eliminating medium is-15 to-20 DEG C,
In described second heat exchanger, the temperature of heat-eliminating medium is-5 to-10 DEG C.
10. a kind of high purity ammonia making in site method according to claim 9, also comprises: the step reclaiming the waste gas of raw material storage tank with waste gas recovery tank;
The step of refining impurity is again carried out by distillation in the 3rd reboiler;
The step of impurity is reclaimed from the first reboiler, the second reboiler, the 3rd reboiler and product storage tank;
To the step of raw material storage tank, the first reboiler, the second reboiler, the 3rd reboiler and product storage tank supply heating medium;
The step of high purity ammonia of vaporizing in vaporizer product;
The step of liquid in product is isolated in vapour liquid separator; And
By the step of streamline to user side supplying products.
11. a kind of high purity ammonia making in site methods according to claim 9, is characterized in that, stabilization more than 24 hours in described raw material storage tank, the first reboiler, the second reboiler and product storage tank.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| KR10-2011-0045300 | 2011-05-13 | ||
| KR1020110045300A KR101125534B1 (en) | 2011-05-13 | 2011-05-13 | Method and apparatus for onsite production of high purity ammonia |
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| CN102774857A CN102774857A (en) | 2012-11-14 |
| CN102774857B true CN102774857B (en) | 2015-08-26 |
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| KR20180031888A (en) * | 2016-09-20 | 2018-03-29 | 롯데케미칼 주식회사 | Energy Saving of High Purity Ammonia Separation Method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003183021A (en) * | 2001-10-12 | 2003-07-03 | Taiyo Toyo Sanso Co Ltd | Method and apparatus for continuously purifying ammonia gas |
| CN1997594A (en) * | 2004-07-07 | 2007-07-11 | 乔治洛德方法研究和开发液化空气有限公司 | Purification and transfilling of ammonia |
| CN101817540A (en) * | 2010-04-06 | 2010-09-01 | 苏州金宏气体股份有限公司 | Purification method of 7N electronic grade hyperpure ammonia |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003183021A (en) * | 2001-10-12 | 2003-07-03 | Taiyo Toyo Sanso Co Ltd | Method and apparatus for continuously purifying ammonia gas |
| CN1997594A (en) * | 2004-07-07 | 2007-07-11 | 乔治洛德方法研究和开发液化空气有限公司 | Purification and transfilling of ammonia |
| CN101817540A (en) * | 2010-04-06 | 2010-09-01 | 苏州金宏气体股份有限公司 | Purification method of 7N electronic grade hyperpure ammonia |
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| CN102774857A (en) | 2012-11-14 |
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Effective date of registration: 20151207 Address after: Seoul, South Kerean Patentee after: Dacheng Industrial Gas Corporation Address before: North Chungcheong Province Patentee before: Gao Zaiwan |