CN106315620A - Ultra-pure ammonia purification device and purification method thereof - Google Patents
Ultra-pure ammonia purification device and purification method thereof Download PDFInfo
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- CN106315620A CN106315620A CN201610914703.4A CN201610914703A CN106315620A CN 106315620 A CN106315620 A CN 106315620A CN 201610914703 A CN201610914703 A CN 201610914703A CN 106315620 A CN106315620 A CN 106315620A
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
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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
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Abstract
The invention relates to an ultra-pure ammonia purification device and a purification method thereof. A raw material liquid ammonia is subjected to gasification through a raw material pre-treatment system to form ammonia gas; then after oil removal and filtering are carried out, the ammonia gas is conveyed into a first rectification column; the ammonia gas output by the raw material pre-treatment system is conveyed into the middle part of the first rectification column and separation of ammonia and heavy-component water is carried out; ammonia gas with the moisture content of being smaller than 10ppb is obtained from the column top of the first rectification column; the ammonia gas with the moisture content of being smaller than 10ppb enters a second rectification column through a first condenser, and separation of the ammonia and light-component water is carried out; liquid ammonia with the purity of 7N is obtained from the second rectification column to form product liquid ammonia; the product liquid ammonia of the second rectification column is conveyed into a product storage and filling system; the product liquid ammonia is filled according to filling coefficients of a product tank car and a product T bottle in the product storage and filling system. The ultra-pure ammonia purification device has the beneficial effects that the raw material liquid ammonia is purified through the raw material pre-treatment system, a rectification and purification system and the product storage and filling system, and the liquid ammonia with the purity of 7N is obtained.
Description
Technical field
The present invention relates to industrial gases produce and field of purification, particularly relate to a kind of ultra-pure ammonia purifier and purification side thereof
Method.
Background technology
Electronic grade ultrapure ammonia is a kind of very important industrial foundation material, be widely used in semiconductor integrated circuit IC,
The industries such as liquid crystal display LCD, light emitting semiconductor device LED and solaode PV.In recent years, along with energy such as Global Oils
Source resource gradually decreases and environmental pollution, the greenhouse effect impact on weather, and clean energy resource and joint are greatly developed in countries in the world
Energy technology, pays close attention to low-carbon economy.Under this background, the solaode of China and light emitting semiconductor device and relevant product
Industry has obtained fast development.During manufacturing, being required for using substantial amounts of ultra-pure ammonia as nitrogen source, especially LED is brilliant
Sheet is when growth, and the purity of ammonia used is the highest, and the LED power consumption of preparation is the least, and luminous intensity is the biggest.Therefore, electron level is produced
Ultra-pure ammonia will have wide market prospect in future.
Summary of the invention
It is an object of the invention to for above weak point, it is provided that a kind of ultra-pure ammonia purifier and purification method thereof,
Carry out liquefied ammonia rectification purification, improve purification efficiency and the clean-up effect of liquefied ammonia.
The present invention solves the scheme that technical problem used: a kind of ultra-pure ammonia purifier, including being sequentially communicated setting
Feedstock pre-processing system, rectification cleaning system and product store charging system, described feedstock pre-processing system, rectification purify system
Unite and be all connected with a hot and cold water supply system with product storage charging system；Described rectification cleaning system includes one for by weight
First rectifying column of component water and ammonia separation and for by the Second distillation column of light component Yu ammonia separation, described first rectifying column
Top and bottom are respectively communicated with and are provided with the first condenser and the first reboiler, and top and the bottom of described Second distillation column connect respectively
Logical being provided with the second condenser and the second reboiler, described first condenser is connected with described Second distillation column, described first cold
Condenser and the second condenser are connected through an emission intensity regulation valve and ammonia condenser that gives up that gives up the most respectively, described useless ammonia condenser
A port of export and one ammonia groove and ammonia absorber that gives up that gives up is connected, and described useless ammonia groove gives up the connection of ammonia tank through the ammonia pump and that gives up, described
Useless ammonia absorber is connected for holding the ammonia accumulator tank of ammonia through an aqua ammonia pump and, is provided with Sheng in described useless ammonia absorber
It is placed with water for absorbing the tank of useless ammonia；The described top of the first rectifying column and the bottom of Second distillation column further respectively have a use
In detecting the moisture monitor of light constituent content in moisture and Second distillation column in the first rectifying column and helium ionized gas phase
Chromatograph, described moisture monitor, helium ionized gas phase chromatographic instrument and useless emission intensity regulation valve and a controller are electrically connected.
Further, described first reboiler and the second reboiler are connected with the output end of hot water of hot and cold water supply system
Logical, described first condenser and the second condenser are connected with the cold water outfan of hot and cold water supply system.
Further, described hot and cold water supply system use PHNIX source pump, including some groups for export cold water and
The cold and heat combined supply unit of hot water, some groups for exporting the refrigeration module units of cold water and being respectively used to the cold water of storage backflow
With cold water storage cistern and the boiler of hot water, described cold water storage cistern and boiler respectively through a cold water circulation pump and a hot water circulating pump with cold
Hot alliance unit is connected, and described refrigeration module unit is connected with cold and heat combined supply unit.
Further, described feedstock pre-processing system includes one for holding the liquefied ammonia tank vehicle of liquefied ammonia, for storing liquefied ammonia
Head tank, for storing the gasification tank of liquefied ammonia after gasification, be provided with and communicated with one first between described liquefied ammonia tank vehicle and head tank
Ammonia pump, is also provided with and communicated with one second ammonia pump between described head tank and gasification tank, the port of export of described gasification tank is successively
It is connected in the middle part of filter and the first rectifying column through grease trap.
Further, also around being provided with a hot-water line in described gasification tank, arrival end and the port of export of described hot-water line are equal
Be arranged at outside gasification tank, and at the arrival end of hot-water line and at the port of export, be respectively equipped with a regulation valve, described hot-water line with
Described hot and cold water supply system is connected, and described regulation valve is electrically connected with described controller.
Further, described product storage charging system includes more than one products pot and surge tank, described products pot
All being connected with Second distillation column with surge tank, the port of export of each products pot is all connected with product tank car, each products pot
The port of export at be additionally provided with a switch valve, each surge tank is connected through a product pump and a product T respectively, described product groove
The lower end of car and product T is equipped with an electronic scale, described electronic scale and switch valve and is electrically connected with described controller.
Further, described products pot and surge tank are by composition sheathed inside and outside inner core and urceolus, and inner core and urceolus
Between formed one sealing interlayer, described interlayer connects a water inlet pipe, and described water inlet pipe is connected with described hot and cold water supply system
Logical.
Further, described product T is connected with respective surge tank through a utilidor respectively, described product pump pair
Should be arranged on utilidor.
The present invention also provides for the purification method of a kind of ultra-pure ammonia purifier as described above, comprises the following steps:
Step S1: raw materials ammonia through feedstock pre-processing system advanced person's circulation of qi promotingization formed ammonia, then through oil removing, filter after input to
First rectifying column；
Step S2: first input in the middle part of the first rectifying column by the ammonia that feedstock pre-processing system exports, carries out ammonia and heavy constituent water
Separate, obtain the aqueous ammonia less than 10ppb at the first rectifying column tower top；
Step S3: the aqueous ammonia less than 10ppb enters Second distillation column through the first condenser, carry out ammonia and light component point
From, obtaining purity at Second distillation column is the liquefied ammonia of 7N, forms product liquefied ammonia；
Step S4: the product liquefied ammonia of Second distillation column is inputted and stores charging system to product, store charging system according to product
The filling ratio of middle product tank car and product T carries out filling of product liquefied ammonia.
Further, in step s 2, the aqueous ammonia less than 10ppb is obtained at the first rectifying column tower top, including following
Step:
Step S21: the ammonia exported by feedstock pre-processing system and the first condenser of the first rectifying column tower top carry out caloic friendship
Change；
Step S22: wherein part ammonia is in the first condenser is liquefied as the tower that liquefied ammonia is back to the first rectifying column, first
In at the bottom of the tower of rectifying column under the effect of the first reboiler, part liquid ammonia gasification, participate in rectification as upflowing vapor from bottom to top；
Step S23: in liquefied ammonia, heavy constituent water is not remained in the first rectifying tower by gasification, is interrupted and opens at the bottom of the first rectifying tower
Useless emission intensity regulation valve, outside in liquefied ammonia, heavy constituent water is expelled to the first rectifying tower；
Step S24: purified by the rectification of the first rectifying column, it is thus achieved that the aqueous ammonia less than 10ppb.
Further, in step s3, it is thus achieved that purity is the liquefied ammonia of 7N, comprises the following steps:
Step S31: by the aqueous ammonia less than 10ppb input to Second distillation column；
Step S32: the aqueous ammonia less than 10ppb produces liquefied ammonia through the second condenser and is back in Second distillation column, with second
In reboiler, upflowing vapor packing layer in Second distillation column tower constantly carries out caloic exchange:
Step S33: opening the useless emission intensity regulation valve of the second condenser, light component is from the second condenser of Second distillation column tower top
Discharging, it is the liquefied ammonia of 7N that Second distillation column tower reactor obtains purity.
Compared with prior art, the present invention has a following beneficial effect: by feedstock pre-processing system, rectification cleaning system and
Product stores charging system and realizes purifying raw materials ammonia, it is thus achieved that purity is the liquefied ammonia of 7N.Simultaneously by useless ammonia absorber
With the useless ammonia produced during useless ammonia tank reclaiming clean, it is achieved useless recovery ammonia；Raw material is provided to locate in advance by hot and cold water supply system
Reason system, rectification cleaning system and product store the circulation-supplied of hot and cold water, wherein feedstock pre-processing system, essence in charging system
Evaporate and controlled by controller intelligence between recovery and the hot and cold water supply system of cleaning system, product storage charging system, useless ammonia
System, improves purification efficiency and the clean-up effect of liquefied ammonia.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings patent of the present invention is further illustrated.
Fig. 1 is the structural representation of embodiment of the present invention ultra-pure ammonia purifier.
The structural representation of Fig. 2 embodiment of the present invention rectification cleaning system.
Fig. 3 is the structural representation of embodiment of the present invention feedstock pre-processing system.
Fig. 4 is the structural representation that embodiment of the present invention product stores charging system.
Fig. 5 is the water supply flow chart of embodiment of the present invention hot and cold water supply system.
In figure: 1-the first rectifying column；2-Second distillation column；3-the first condenser；4-the second condenser；5-first boils again
Device；6-the second reboiler；7-gives up ammonia condenser；8-gives up ammonia groove；9-gives up ammonia absorber；10-ammonia accumulator tank；11-gives up ammonia tank；
12-aqua ammonia pump；13-gives up ammonia pump；14-give up emission intensity regulation valve；15-liquefied ammonia tank vehicle；16-raw material tank；17-gasification tank；170-heat
Water pipe；18-grease trap；19-filter；20-the first ammonia pump；21-the second ammonia pump；22-products pot；23-surge tank；24-
Product pump；25-product T；26-product tank car.
Detailed description of the invention
The present invention is further described with detailed description of the invention below in conjunction with the accompanying drawings.
As shown in Fig. 1～5, a kind of ultra-pure ammonia purifier of the present embodiment, locate in advance including the raw material being sequentially communicated setting
Reason system, rectification cleaning system and product store charging system, described feedstock pre-processing system, rectification cleaning system and product storage
Deposit charging system to be all connected with a hot and cold water supply system；Described rectification cleaning system includes one for by heavy constituent water and ammonia
The first rectifying column 1 of separating and for by the Second distillation column 2 of light component Yu ammonia separation, the top of described first rectifying column 1 with
Bottom is respectively communicated with and is provided with the first condenser 3 and the first reboiler 5, and top and the bottom of described Second distillation column 2 are respectively communicated with
Being provided with the second condenser 4 and the second reboiler 6, described first condenser 3 is connected with described Second distillation column 2, and described first
Condenser 3 and the second condenser 4 are connected through emission intensity regulation valve 14 ammonia condenser 7 that gives up with that gives up the most respectively, described useless ammonia
The port of export of a condenser 7 and one ammonia groove 8 and ammonia absorber 9 that gives up that gives up is connected, and described useless ammonia groove 8 gives up through the ammonia pump 13 and that gives up
Ammonia tank 11 connects, and described useless ammonia absorber 9 is connected for holding the ammonia accumulator tank 10 of ammonia with one through an aqua ammonia pump 12, institute
The tank being contained with water for absorbing useless ammonia it is provided with in stating useless ammonia absorber 9；Described first reboiler 5 and the second reboiler 6 are also
Connection one has hot and cold water supply system；The described top of the first rectifying column 1 and the bottom of Second distillation column 2 further respectively have a use
In detecting the moisture monitor of light constituent content in moisture and Second distillation column 2 in the first rectifying column 1 and helium ionized gas
Chromatography, described moisture monitor, helium ionized gas phase chromatographic instrument and useless emission intensity regulation valve 14 are electrically connected with a controller.Will
The ammonia of feedstock pre-processing system output sequentially inputs to the first rectifying column 1 and Second distillation column 2, realizes heavy constituent and ammonia respectively
Separate and light component separate with ammonia.Wherein restructuring is divided into water, light component is hydrogen, nitrogen, argon, oxygen, carbon monoxide, carbon dioxide
And Hydrocarbon etc..Ammonia from feedstock pre-processing system is introduced in the middle part of the first rectifying column 1, with the first condenser 3
The backflow liquefied ammonia of liquefaction carries out caloic exchange at packing layer, enters the part ammonia of tower and is liquefied and is back in the first rectifying column 1 tower,
Under the effect of the first rectifying column 1 tower bottom reboiler, part liquid ammonia gasification participates in rectification as upflowing vapor from bottom to top, and weighs
Component water is not remained in tower reactor by gasification, is interrupted and discharges outside tower.Purified by the rectification of the first rectifying column 1, can obtain from tower top
The aqueous ammonia less than 10ppb.The ammonia of unwatering the first condenser 3 from the first rectifying column 1 top enters the second rectification
Tower 2, carries out ammonia and separates with light component, under the effect of the second reboiler 6 at the bottom of tower top the second condenser 4 and tower, backflow with
Upflowing vapor packing layer in tower constantly carries out caloic exchange, and light component is discharged from overhead condenser with a small amount of ammonia, the
Two rectifying column 2 tower reactors can obtain the liquefied ammonia that purity is 7N.Wherein feedstock pre-processing system, rectification cleaning system, product store and fill
Dress system is all connected with hot and cold water supply system.The first rectification is checked by moisture monitor and helium ionized gas phase chromatographic instrument
The content of the heavy constituent water in tower and Second distillation column ammonia and the content of light component, be monitored by controller, adjusts first
Rectifying column and the parameter of Second distillation column, including flow, pressure, temperature and liquid level.Described controller be DCS control module or
Person passes through Single-chip Controlling, and described controller can also be connected with outer PC.
It is provided with useless emission intensity regulation valve 14, water in the first rectifying column 1 top ammonia at the first condenser 3 and the second condenser 4
When point exceeding standard, control useless emission intensity regulation valve 14 by controller and automatically useless ammonia is discharged；Containing light group in second condenser 4
The useless ammonia divided must be carried out continuously discharge.Useless ammonia condenser 7 part of useless ammonia warp from the first rectifying column 1 and Second distillation column 2
Liquefaction enters useless ammonia groove 8, useless ammonia pump 13 squeeze into useless ammonia tank 11 and reclaim.The useless ammonia not being liquefied containing light component then enters useless ammonia
Absorption tower 9, mixes generation ammonia and inputs to ammonia accumulator tank 10 with water；Fail the light component of mixing and a small amount of ammonia by useless ammonia
In absorption tower 9, the floss hole of high 25 meters discharges.
In the present embodiment, the output end of hot water of described first reboiler 5 and the second reboiler 6 and hot and cold water supply system
Being connected, described first condenser 3 is connected with the cold water outfan of hot and cold water supply system with the second condenser 4.
As it is shown in figure 5, in the present embodiment, described hot and cold water supply system uses PHNIX source pump, including some groups
For exporting the cold and heat combined supply unit of cold water and hot water, some groups for exporting the refrigeration module unit of cold water and being respectively used to
Storing cold water and the cold water storage cistern of hot water and boiler, described cold water storage cistern and boiler are respectively through hot water circulating pump and cold water circulation pump
Being connected with cold and heat combined supply unit, described refrigeration module unit is connected with the cold water outlet of cold and heat combined supply unit.First again
Boiling device 5 connects with the hot water feed water inlet in hot and cold water supply system with in the second reboiler 6, the first condenser 3 and the second condensation
Device 4 is connected with cold water feed water inlet in hot and cold water supply system, it is achieved first reboiler the 5, second reboiler the 6, first condenser 3
Work with the second condenser 4；As shown in Figure 4, feedstock pre-processing system, rectification cleaning system, product store charging system all
Use substantial amounts of cold water and hot water, account for more than the 90% of whole energy expenditure, for saving energy consumption, reduce cost, use PHNIX
Source pump, wherein cold and heat combined supply unit 5, wherein 2 standby；Refrigeration module unit 2, wherein 1 standby；Can produce simultaneously
Raw 65 DEG C～the high-temperature-hot-water of 85 DEG C and 5 DEG C～the cold water of 25 DEG C.In hot and cold water supply system, cold and heat combined supply unit can be given birth to simultaneously
Producing cold water and hot water, the hot water produced because of 5 cold and heat combined supply units is enough, and cold water can not meet needs, so separately configuration 2
Producing the refrigeration module unit of cold water, from hot and cold water supply system, the hot water or cold water of output is respectively through cold water feed water inlet and hot water
Feed water inlet is delivered to products pot 22, surge tank 23, gasification tank the 17, first reboiler the 5, second reboiler the 6, first condenser 3 and
Second condenser 4, then products pot 22, surge tank 23, gasification tank the 17, first reboiler the 5, second reboiler the 6, first condenser
3 and second condenser 4 output cold water or hot water respectively through cold-water return mouth or hot water backwater's mouth be back to enter cold water storage cistern or
Boiler, uses by cold water circulation pump or heat-exchanger pump pressurization cycle.Described boiler and cold water storage cistern are also through a tap water moisturizing
Mouth is connected with running water pipe.The hot water outlet of cold and heat combined supply unit is connected with cold water outlet, and refrigeration module machine
The cold water outlet of group exports to cold water feed water inlet after being connected with the cold water water outlet of cold and heat combined supply unit, cold and heat combined supply unit
Hot water outlet is connected with hot water feed water inlet.
The following is 3 cold and heat combined supply units and 1 refrigeration module unit operation situation in the case of minimum output, 3 cold and hot
Alliance unit electrical power is 106.8kw, and 1 refrigeration module unit electrical power is 31.6kw, and hot and cold water supply system total energy consumption is:
(106.8kw+31.6kw) ÷ 0.9=153.8kw；
Calculating by minimum output 150kg/h, the energy consumption of every kg ultra-pure ammonia is:
153.8kw ÷150kg/h = 1.025kwh/kg。
In the present embodiment, described feedstock pre-processing system includes one for holding the liquefied ammonia tank vehicle 15 of liquefied ammonia, for storing up
The head tank 16 of liquid storage ammonia, gasification tank 17 for liquid ammonia gasification, connect setting between described liquefied ammonia tank vehicle 15 and head tank 16
There is one first ammonia pump 20, between described head tank 16 and gasification tank 17, be also provided with and communicated with one second ammonia pump 21, described gas
The port of export changing tank 17 is connected with filter 19 through grease trap 18 successively in the middle part of the first rectifying column 1.Raw materials ammonia is by liquefied ammonia
Tank car 15 is filled with head tank 16 through the first ammonia pump 20 and stores, then is filled with gasification tank 17 by the second ammonia pump 21.
In the present embodiment, also around being provided with a hot-water line 170, the entrance of described hot-water line 170 in described gasification tank 17
End and the port of export may be contained within outside gasification tank 17, and are respectively equipped with a tune at the arrival end of hot-water line 170 and at the port of export
Joint valve, described hot-water line 170 is connected with described hot and cold water supply system, and described regulation valve is electrically connected with described controller.At gas
Change in tank 17, by hot and cold water supply system input hot water to hot-water line 170, liquefied ammonia is heated to uniform temperature, liquid ammonia gasification
For corresponding saturated vapor pressure, then ammonia inputs to the first rectifying column 1 through grease trap 18, filter 19.
In the present embodiment, described product storage charging system includes more than one products pot 22 and surge tank 23, institute
State products pot 22 to be all connected with Second distillation column 2 with surge tank 23, the port of export of each products pot 22 all with product tank car 26
Being connected, be additionally provided with a switch valve at the port of export of each products pot 22, each surge tank 23 is respectively through a product pump 24 and
Product T 25 is connected, and the lower end of described product tank car 26 and product T 25 is equipped with an electronic scale, described electronic scale and opening
Close valve to be electrically connected with described controller.The product liquefied ammonia of Second distillation column 2 is respectively enterd products pot 22 and surge tank 23, products pot
22 storages being used for product liquefied ammonia, carry out filling of product tank car 26；Surge tank 23 fills for product T bottle, product liquefied ammonia
It is filled with product T bottle through product pump 24 supercharging, product liquefied ammonia by utilidor from surge tank 23；According to product tank car 26 and product
The filling ratio of T 25 carries out filling of product liquefied ammonia.
In the present embodiment, described products pot 22 and surge tank 23 are by composition sheathed inside and outside inner core and urceolus and interior
Forming the interlayer of a sealing between cylinder and urceolus, described interlayer connects a water inlet pipe, described water inlet pipe and described hot and cold water supply
System is connected.Can be passed through inflow cold water or hot water in described interlayer, during storage, interlayer flows into cold water, beneficially product storage；
When filling product tank car 26, products pot 22 flows into hot water and carries out supercharging, improves pressurising efficiency.
In the present embodiment, described product T 25 is connected with respective surge tank 23 through a utilidor respectively, described
Product pump 24 is correspondingly arranged on utilidor.
In Fig. 1-4, PG is Pressure gauge on the spot, and PY is pressure converter, and PT is pressure transmitter, and TE is temperature detection
Device, LT is fluid level transmitter, and FT is differential pressure transmitter.
The present invention also provides for the purification method of a kind of ultra-pure ammonia purifier as described above, comprises the following steps:
Step S1: raw materials ammonia through feedstock pre-processing system advanced person's circulation of qi promotingization formed ammonia, then through oil removing, filter after input to
First rectifying column 1；
Step S2: first inputted in the middle part of the first rectifying column 1 by the ammonia that feedstock pre-processing system exports, carries out ammonia and heavy constituent water
Separate, obtain the aqueous ammonia less than 10ppb at the first rectifying column 1 tower top；
Step S3: the aqueous ammonia less than 10ppb enters Second distillation column 2 through the first condenser 3, carry out ammonia and light component point
From, obtain, at Second distillation column 2, the liquefied ammonia that purity is 7N, form product liquefied ammonia；
Step S4: the product liquefied ammonia of Second distillation column 2 is inputted and stores charging system to product, store charging system according to product
The filling ratio of middle product tank car 26 and product T 25 carries out filling of product liquefied ammonia.
In the present embodiment, in step s 2, the aqueous ammonia less than 10ppb is obtained at the first rectifying column 1 tower top, including
Following steps:
Step S21: the ammonia exported by feedstock pre-processing system and the first condenser 3 of the first rectifying column 1 tower top carry out heat friendship
Change；
Step S22: wherein part ammonia is in the first condenser 3 is liquefied as the tower that liquefied ammonia is back to the first rectifying column 1,
Under the effect of the first reboiler 5 at the bottom of the tower of one rectifying column 1, part liquid ammonia gasification, participate in rectification as upflowing vapor from bottom to top；
Step S23: in liquefied ammonia, heavy constituent water is not remained in the first rectifying column 1 tower reactor by gasification, is interrupted and opens the first rectifying column 1 tower
The useless emission intensity regulation valve 14 at the end, is expelled to heavy constituent water in liquefied ammonia outside the first rectifying column 1 tower；
Step S24: purified by the rectification of the first rectifying column 1, it is thus achieved that the aqueous ammonia less than 10ppb.
In the present embodiment, in step s3, it is thus achieved that purity is the liquefied ammonia of 7N, comprises the following steps:
Step S31: by the aqueous ammonia less than 10ppb input to Second distillation column 2；
Step S32: the aqueous ammonia less than 10ppb produces liquefied ammonia through the second condenser 4 and is back in Second distillation column 2, with
In two reboilers 6, upflowing vapor packing layer in Second distillation column 2 tower constantly carries out caloic exchange:
Step S33: opening the useless emission intensity regulation valve 14 of the second condenser 4, light component is cold from the second of Second distillation column 2 tower top
Condenser 4 is discharged, and it is the liquefied ammonia of 7N that Second distillation column 2 tower reactor obtains purity.
In sum, the present invention provides a kind of ultra-pure ammonia purifier and purification method thereof, it is possible to achieve useless ammonia is automatic
Reclaiming, purification efficiency is high, good purification, it is possible to obtain purity is the liquefied ammonia of 7N.
The object, technical solutions and advantages of the present invention are further described by above-listed preferred embodiment, are answered
It is understood by, the foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (10)
1. a ultra-pure ammonia purifier, it is characterised in that: include being sequentially communicated the feedstock pre-processing system of setting, rectification purifies
System and product store charging system, described feedstock pre-processing system, rectification cleaning system and product store charging system all with
One hot and cold water supply system is connected；Described rectification cleaning system includes one for the first rectification by heavy constituent water Yu ammonia separation
Tower and for by the Second distillation column of light component Yu ammonia separation, the top of described first rectifying column and bottom are respectively communicated with and are provided with the
One condenser and the first reboiler, the top of described Second distillation column and bottom are respectively communicated with and are provided with the second condenser and second again
Boiling device, described first condenser is connected with described Second distillation column, described first condenser and the second condenser warp the most respectively
An one emission intensity regulation valve and ammonia condenser that gives up that gives up is connected, and the port of export and of the described useless ammonia condenser ammonia groove and that gives up gives up ammonia
Absorption tower is connected, described useless ammonia groove through one give up ammonia pump and give up ammonia tank connection, described useless ammonia absorber is through an aqua ammonia pump and
It is connected for holding the ammonia accumulator tank of ammonia, in described useless ammonia absorber, is provided with the water being contained with water for absorbing useless ammonia
Groove；The described top of the first rectifying column and the bottom of Second distillation column further respectively have one in detecting the first rectifying column moisture
The moisture monitor of light constituent content and helium ionized gas phase chromatographic instrument in content and Second distillation column, described moisture monitor,
Helium ionized gas phase chromatographic instrument and useless emission intensity regulation valve and a controller are electrically connected.
A kind of ultra-pure ammonia purifier the most according to claim 1, it is characterised in that: described first reboiler and second is again
Boiling device is connected with the output end of hot water of hot and cold water supply system, described first condenser and the second condenser and hot and cold water supply
The cold water outfan of system is connected.
A kind of ultra-pure ammonia purifier the most according to claim 2, it is characterised in that: described hot and cold water supply system uses
PHNIX source pump, including some groups for exporting the cold and heat combined supply unit of cold water and hot water, some groups for exporting cold water
Refrigeration module unit and be respectively used to store cold water and the cold water storage cistern of hot water and boiler, described cold water storage cistern and boiler respectively
It is connected with cold and heat combined supply unit through a cold water circulation pump and a hot water circulating pump, described refrigeration module unit and cold and heat combined supply machine
Group is connected.
A kind of ultra-pure ammonia purifier the most according to claim 1, it is characterised in that: described feedstock pre-processing system includes
One for holding the liquefied ammonia tank vehicle of liquefied ammonia, for storing the head tank of liquefied ammonia, for the gasification tank of liquid ammonia gasification, described liquefied ammonia groove
It is provided with and communicated with one first ammonia pump between car and head tank, between described head tank and gasification tank, is also provided with and communicated with one second
Ammonia pump, the port of export of described gasification tank is connected in the middle part of filter and the first rectifying column through grease trap successively.
A kind of ultra-pure ammonia purifier the most according to claim 4, it is characterised in that: also around being provided with in described gasification tank
One hot-water line, arrival end and the port of export of described hot-water line may be contained within outside gasification tank, and at the arrival end of hot-water line and
Being respectively equipped with a regulation valve at the port of export, described hot-water line is connected with described hot and cold water supply system, described regulation valve and institute
State controller to be electrically connected.
A kind of ultra-pure ammonia purifier the most according to claim 1, it is characterised in that: described product stores charging system bag
Including more than one products pot and surge tank, described products pot is all connected with Second distillation column with surge tank, each products pot
The port of export be all connected with product tank car, be additionally provided with a switch valve at the port of export of each products pot, each surge tank is respectively
Being connected through a product pump and a product T, the lower end of described product tank car and product T is equipped with an electronic scale, described electricity
Sub-scale and switch valve are electrically connected with described controller.
A kind of ultra-pure ammonia purifier the most according to claim 6, it is characterised in that: described products pot and surge tank by
Sheathed composition inside and outside inner core and urceolus, and between inner core and urceolus, form the interlayer of a sealing, described interlayer connection one water inlet
Pipe, described water inlet pipe is connected with described hot and cold water supply system；Described product T is slow with respective through a utilidor respectively
Rushing tank to be connected, described product pump is correspondingly arranged on utilidor.
8. the purification method of the ultra-pure ammonia purifier as described in any one of claim 1-7, it is characterised in that include with
Lower step:
Step S1: raw materials ammonia through feedstock pre-processing system advanced person's circulation of qi promotingization formed ammonia, then through oil removing, filter after input to
First rectifying column；
Step S2: first input in the middle part of the first rectifying column by the ammonia that feedstock pre-processing system exports, carries out ammonia and heavy constituent water
Separate, obtain the aqueous ammonia less than 10ppb at the first rectifying column tower top；
Step S3: the aqueous ammonia less than 10ppb enters Second distillation column through the first condenser, carry out ammonia and light component point
From, obtaining purity at Second distillation column is the liquefied ammonia of 7N, forms product liquefied ammonia；
Step S4: the product liquefied ammonia of Second distillation column is inputted and stores charging system to product, store charging system according to product
The filling ratio of middle product tank car and product T carries out filling of product liquefied ammonia.
The purification method of ultra-pure ammonia purifier the most according to claim 8, it is characterised in that in step s 2,
One rectifying column tower top obtains the aqueous ammonia less than 10ppb, comprises the following steps: step S21: exported by feedstock pre-processing system
Ammonia and the first condenser of the first rectifying column tower top carry out caloic exchange；
Step S22: wherein part ammonia is in the first condenser is liquefied as the tower that liquefied ammonia is back to the first rectifying column, first
In at the bottom of the tower of rectifying column under the effect of the first reboiler, part liquid ammonia gasification, participate in rectification as upflowing vapor from bottom to top；
Step S23: in liquefied ammonia, heavy constituent water is not remained in the first rectifying tower by gasification, is interrupted and opens the useless of the first rectifying column
Emission intensity regulation valve, outside in liquefied ammonia, heavy constituent water is expelled to the first rectifying tower；
Step S24: purified by the rectification of the first rectifying column, it is thus achieved that the aqueous ammonia less than 10ppb.
The purification method of ultra-pure ammonia purifier the most according to claim 8, it is characterised in that in step s3, it is thus achieved that
Purity is the liquefied ammonia of 7N, comprises the following steps:
Step S31: by the aqueous ammonia less than 10ppb input to Second distillation column；
Step S32: the aqueous ammonia less than 10ppb produces liquefied ammonia through the second condenser and is back in Second distillation column, with second
In reboiler, upflowing vapor packing layer in Second distillation column tower constantly carries out caloic exchange:
Step S33: opening the useless emission intensity regulation valve of the second condenser, light component is from the second condenser of Second distillation column tower top
Discharging, it is the liquefied ammonia of 7N that Second distillation column tower reactor obtains purity.
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| CN113044854A (en) * | 2021-03-23 | 2021-06-29 | 江西江氨科技有限公司 | High-purity ammonia preparation method and system |
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Address after: 350109 Yu Yu 86, Yutian village, Nan Yu Town, Minhou County, Fuzhou, Fujian Patentee after: Fujian jiuce Gas Co., Ltd Address before: 350109, Fujian, Fuzhou province Minhou County town of South Lantau village new bridge Patentee before: FUJIAN JIUCE GAS GROUP Co.,Ltd. |