CN109231238A - A kind of high-purity ammon continuous process system and its production technology - Google Patents
A kind of high-purity ammon continuous process system and its production technology Download PDFInfo
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- CN109231238A CN109231238A CN201811001607.6A CN201811001607A CN109231238A CN 109231238 A CN109231238 A CN 109231238A CN 201811001607 A CN201811001607 A CN 201811001607A CN 109231238 A CN109231238 A CN 109231238A
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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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- Inorganic Chemistry (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of high-purity ammon continuous process system and its production technologies, production system includes raw material ammonia storage tank, feed pump, vaporizer, filter, two-stage ammonia device of spiral-screen column, first surge tank, second surge tank, products pot, liquid pouring pump, analysis detection instrument, the raw material ammonia storage tank is connected with charging pump intake, charging pump discharge is connected with vaporizer entrance, vaporizer gaseous phase outlet is connected with filter by ammonia pipeline, filter is connected with two-stage ammonia device of spiral-screen column, analysis detection instrument, first surge tank and the second surge tank are connected in turn on the liquefied ammonia pipeline connecting with product extraction mouth, first surge tank, the outlet of second surge tank connects products pot and liquid pouring pump by liquefied ammonia pipeline, the outlet of liquid pouring pump is connected with raw material ammonia storage tank.Using double buffering tank, when product fluctuation/exception, product is adjusted to the second surge tank in time, is back to raw material ammonia storage tank and re-works, and improves liquefied ammonia purity in products pot.
Description
Technical field
The present invention relates to ammonia production fields, and in particular to a kind of high-purity ammon continuous process system and its production technology.
Background technique
High-purity ammon (NH3) 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 solar battery PV.
The production of high-purity ammon obtains high purity product by means of purification mainly using industrial ammonia as raw material.Contain in raw material ammonia
There are solid particle, hydro carbons, water, carbon dioxide, carbon monoxide, oxygen etc..The common production method of high-purity ammon is absorption at present
The mode of mode, the mode of rectifying or absorption in conjunction with rectifying, but this method energy consumption is very high and exhaust emissions amount is big, and
And it is difficult to be purified to very high purity.Therefore it provides continuous process system and the technology controlling and process side of a kind of high-purity ammon of high quality
Method is this field technical issues that need to address.
Summary of the invention
The purpose of the present invention is there is the above problem in view of the prior art, the high-purity ammon for proposing a kind of high quality is continuous
Production system and its production technology are greatly improved the serious forgiveness in production process, are reached more using two-tower rectification and double buffering tank
High product purity, purity reach 99.99999%.
Object of the invention can be realized by the following technical scheme:
A kind of high-purity ammon continuous process system, which is characterized in that including raw material ammonia storage tank, feed pump, vaporizer, filtering
Device, two-stage ammonia device of spiral-screen column, the first surge tank, the second surge tank, products pot, liquid pouring pump, analysis detection instrument, the raw material ammonia
Storage tank is connected with charging pump intake, and charging pump discharge is connected with vaporizer entrance, and vaporizer gaseous phase outlet and filter pass through ammonia
Feed channel is connected, and filter is connected with two-stage ammonia device of spiral-screen column, and the product extraction mouth of two-stage ammonia device of spiral-screen column is connected with liquid
Ammonia pipeline, analysis detection instrument, the first surge tank and the second surge tank are connected to the liquefied ammonia pipeline connecting with product extraction mouth in turn
On, the outlet of the first surge tank, the second surge tank connects products pot and liquid pouring pump, the outlet and original of liquid pouring pump by liquefied ammonia pipeline
Expect that ammonia storage tank is connected, two-stage ammonia device of spiral-screen column includes first rectifying column and Second distillation column, the top of the first rectifying column
Equipped with the first condenser, the top of Second distillation column is equipped with the second condenser, first rectifying column, Second distillation column bottom connect
It is connected to reboiler, the import of the gaseous phase outlet and Second distillation column of the first condenser connects, and the gaseous phase outlet of the second condenser connects
Connect exhaust treatment system.
Exhaust treatment system is highly soluble in the characteristic of water using ammonia, is absorbed by the way of water absorption, reaches qualified
Exhaust emissions index.
Further, first rectifying column, Second distillation column tower in be filled with ripple silk net filler.
Further, the raw material ammonia storage tank, vaporizer, first rectifying column, Second distillation column, the first surge tank, second
Pressure gauge, thermometer and safety valve are provided on surge tank, products pot.
Further, with the heating coil of energy heating water bath in the vaporizer.
Further, the products pot, the first surge tank, the second surge tank are equipped with freezing water leg.Freeze water leg
Effect be to control the pressure of products pot and surge tank, it is ensured that infusion ammonia pipeline and they between there are pressure differences, passing through pressure difference will
Material is delivered to surge tank and products pot.
A kind of high-purity ammon continuous production processes, which is characterized in that specific step is as follows:
S1: raw material ammonia is after the assay was approved through liquefied ammonia pipeline discharging to raw material ammonia storage tank, and raw material ammonia pressure of storage tank is generally in 3-
13Bar；
S2: raw material is delivered to vaporizer through feed pump by raw material ammonia storage tank, and the feed pump need to use oil free type delivery pump；
S3: raw material is in vaporizer, pressure build up, it is ensured that enough pressure, vaporizer boosting principle are as follows: have in vaporizer
Hot-water coil pipe, raw material ammonia carry out pressure build up by the heat that hot-water coil pipe provides, and hot water temperature controls at 30-45 DEG C, normally
Vaporizer control pressure is 8-12Bar in operational process；
S4: ammonia becomes gaseous state from liquid in vaporizer, and gaseous ammonia enters filter through ammonia pipeline by vaporizer and removes
Partial particulate substance and oil；
S5: the ammonia for removing oil and particulate matter enters first rectifying column, cold by being equipped at the top of first rectifying column
Condenser provides decline condensate liquid, and the reboiler that first rectifying column bottom is equipped with provides upflowing vapor, and ammonia realizes gas in rectifying column
Mass transfer in liquid phase, heat transfer, except the heavy constituent impurity in deammoniation, heavy constituent impurity is water, and water impurity can be removed within 20ppb；
S6: the ammonia of heavy constituent is removed by the first condenser overhead of first rectifying column, Second distillation column is entered, passes through
The second condenser being equipped at the top of Second distillation column provides decline condensate liquid, in the reboiler offer that Second distillation column bottom is equipped with
Steam is risen, ammonia realizes liquid phase mass transfer, heat transfer in Second distillation column, except the light component impurity in deammoniation, light component impurity packet
Include methane, carbon monoxide, carbon dioxide, oxygen, nitrogen, hydrogen；
S7: the product extraction mouth of Second distillation column is provided with analytical sampling pipeline, analysis detection instrument is directly connected to, to production
Product quality carry out 24 hours, Always Online" monitoring, monitoring group be divided into water, methane, carbon monoxide, carbon dioxide, oxygen, nitrogen,
Hydrogen；
S8: the ammonia purity after the detection of analysis detection instrument is qualified reaches 99.99999%, and the product through Second distillation column is adopted
Outlet enters the first surge tank by top, and the first surge tank is equipped with cooling water jecket, and the first buffer tank pressure is 5-8Bar；
Liquefied ammonia in S9: the first surge tank is produced through bottom to products pot by pressure difference；
S10: when there is exception or product quality exception in production line, the product extraction mouth switching of two-stage ammonia device of spiral-screen column
It is connected to the second surge tank, production-line technique is checked, when production line restores normal, it is slow that product extraction mouth switches back into first
Tank is rushed, the liquefied ammonia in the second surge tank can be through liquid pouring pump, batch turning to raw material ammonia storage tank.
Further, in above-mentioned step S5, first rectifying column mainly passes through pressure control, and control tower pressure is 6-
9bar, pressure control is by adjusting the control of reboiler hot water.
Further, in above-mentioned step S6, Second distillation column mainly passes through pressure control, and control tower pressure is 5-
8bar, pressure control is by adjusting the control of reboiler hot water.
The liquefied ammonia for remaining in first rectifying column and Second distillation column bottom is low-purity liquefied ammonia, directly from the discharge of tower bottom
Pipe is discharged and collects re-using.
Compared with prior art, the present invention has the effect of positive:
1. high-purity ammon continuous process system uses two-tower rectification, big flow production on the one hand can satisfy, on the other hand
According to one tower of impurity composition in raw material except the other tower of heavy constituent removes light component, higher product purity, purity can achieve
Reach 99.99999%.
2., using double buffering tank, may be implemented when product fluctuation/exception, product is adjusted in time because of product purity height
Second surge tank is back to raw material ammonia storage tank and re-works, and adjusts back the first surge tank again after abnormal conditions processing, in this way can be with
It avoids product not up to standard from entering products pot, polluted products pot, realize that product is continually and steadily produced to the purpose of products pot.
Fig. 1 is the structural schematic diagram of high-purity ammon continuous process system.
In figure, 1, raw material ammonia storage tank；2, feed pump；3, vaporizer；4, filter；5, the first surge tank；6, the second buffering
Tank；7, products pot；8, liquid pouring pump；9, analysis detection instrument；10, first rectifying column；11, Second distillation column；12, reboiler；13,
One condenser；14, the second condenser；15, exhaust treatment system.
Specific embodiment
Following is a specific embodiment of the present invention in conjunction with the accompanying drawings, technical scheme of the present invention will be further described,
However, the present invention is not limited to these examples.
As shown in Figure 1, this high-purity ammon continuous process system, including raw material ammonia storage tank 1, feed pump 2, vaporizer 3, filter
4, two-stage ammonia device of spiral-screen column, the first surge tank 5, the second surge tank 6, products pot 7, liquid pouring pump 8, analysis detection instrument 9, the original
Material ammonia storage tank 1 is connected with 2 entrance of feed pump, and the outlet of feed pump 2 is connected with 3 entrance of vaporizer, 3 gaseous phase outlet of vaporizer and filtering
Device 4 is connected by ammonia pipeline, and filter 4 is connected with two-stage ammonia device of spiral-screen column, the product extraction of two-stage ammonia device of spiral-screen column
Mouth is connected with liquefied ammonia pipeline, and analysis detection instrument 9, the first surge tank 5 and the second surge tank 6 are connected in turn to be connected with product extraction mouth
On the liquefied ammonia pipeline connect, the outlet of the first surge tank 5, the second surge tank 6 connects products pot 7 and liquid pouring pump 8 by liquefied ammonia pipeline,
The outlet of liquid pouring pump 8 is connected with raw material ammonia storage tank 1, and two-stage ammonia device of spiral-screen column includes first rectifying column 10 and Second distillation column
11, the top of the first rectifying column 10 is equipped with the first condenser 13, and the top of Second distillation column 11 is equipped with the second condenser 14,
First rectifying column 10, Second distillation column 11 bottom be respectively connected with reboiler 12, the gaseous phase outlet and second of the first condenser 13
The import of rectifying column 11 connects, and the gaseous phase outlet of the second condenser 14 connects exhaust treatment system 15.
First rectifying column 10, Second distillation column 11 tower in be filled with ripple silk net filler.The raw material ammonia storage tank 1, vaporization
Device 3, Second distillation column 11, the first surge tank 5, the second surge tank 6, is provided with pressure on products pot 7 at first rectifying column 10
Table, thermometer and safety valve.Heating coil in the vaporizer 3 with energy heating water bath.The products pot 7, first buffers
Tank 5, the second surge tank 6 are equipped with freezing water leg.The effect of freezing water leg is to control the pressure of products pot 7 and surge tank,
Ensure be infused ammonia pipeline and they between there are pressure differences, material is delivered to by surge tank and products pot 7 by pressure difference.
This high-purity ammon continuous production processes, the specific steps are as follows:
S1: after the assay was approved through liquefied ammonia pipeline discharging to raw material ammonia storage tank 1,1 pressure of raw material ammonia storage tank generally exists raw material ammonia
3-13Bar；
S2: raw material is delivered to vaporizer 3 through feed pump 2 by raw material ammonia storage tank 1, and the feed pump 2 need to be defeated using oil free type
Send pump；
S3: raw material is in vaporizer 3, pressure build up, it is ensured that enough pressure, 3 boosting principle of vaporizer are as follows: in vaporizer 3
With hot-water coil pipe, raw material ammonia carries out pressure build up by the heat that hot-water coil pipe provides, and hot water temperature controls at 30-45 DEG C,
It is 8-12Bar that vaporizer 3, which controls pressure, in normal course of operation；
S4: ammonia becomes gaseous state from liquid in vaporizer 3, and gaseous ammonia enters filter 4 through ammonia pipeline by vaporizer 3 and removes
Remove partial particulate substance and oil；
S5: the ammonia for removing oil and particulate matter enters first rectifying column 10, by being equipped at the top of first rectifying column 10
Condenser decline condensate liquid is provided, reboiler 12 that 10 bottom of first rectifying column is equipped with provides upflowing vapor, and ammonia is in rectifying column
Interior realization liquid phase mass transfer, heat transfer, except the heavy constituent impurity in deammoniation, heavy constituent impurity is water, water impurity can except to 20ppb with
It is interior；
S6: the ammonia of heavy constituent is removed by 13 top of the first condenser of first rectifying column 10, enters Second distillation column
11, decline condensate liquid is provided by the second condenser 14 being equipped at the top of Second distillation column 11,11 bottom of Second distillation column is equipped with
Reboiler 12 provide upflowing vapor, ammonia is realized in Second distillation column 11 liquid phase mass transfer, conduct heat, except the light component in deammoniation
Impurity, light component impurity include methane, carbon monoxide, carbon dioxide, oxygen, nitrogen, hydrogen；
S7: the product extraction mouth of two-stage ammonia device of spiral-screen column is provided with analytical sampling pipeline, is directly connected to analysis detection
Instrument 9 carries out product quality 24 hours, and Always Online" monitoring, monitoring group is divided into water, methane, carbon monoxide, carbon dioxide, oxygen
Gas, nitrogen, hydrogen；
S8: analysis detection instrument 9 detects the ammonia purity after qualification and reaches 99.99999%, the product through Second distillation column 11
Mouth is produced, the first surge tank 5 is entered by top, the first surge tank 5 is equipped with cooling water jecket, and 5 pressure of the first surge tank is 5-
8Bar；
Liquefied ammonia in S9: the first surge tank 5 is produced through bottom to products pot 7 by pressure difference；
S10: when there is exception or product quality exception in production line, the product extraction mouth switching connection of Second distillation column 11
To the second surge tank 6, production-line technique is checked, when production line restores normal, product extraction mouth switches back into the first buffering
Tank 5, the liquefied ammonia in the second surge tank 6 can be through liquid pouring pump 8, batch turning to raw material ammonia storage tank 1.
In above-mentioned step S5, first rectifying column 10 is main to be controlled by pressure, and control tower pressure is 6-9bar, pressure control
System is by adjusting the control of 12 hot water of reboiler.
In above-mentioned step S6, Second distillation column 11 is main to be controlled by pressure, and control tower pressure is 5-8bar, pressure control
System is by adjusting the control of 12 hot water of reboiler.
The liquefied ammonia for remaining in 11 bottom of first rectifying column 10 and Second distillation column is low-purity liquefied ammonia, directly from tower bottom
Discharge pipe is discharged and collects re-using.This high-purity ammon continuous process system uses two-tower rectification, on the one hand can satisfy big stream
Amount production, on the other hand can achieve higher according to one tower of impurity composition in raw material except the other tower of heavy constituent removes light component
Product purity, purity reaches 99.99999%.Because product purity height, using double buffering tank, may be implemented when product fluctuation/it is different
Chang Shi, product are adjusted to the second surge tank 6 in time, are back to raw material ammonia storage tank 1 and re-work, adjust again after maintenance and inspection
The first surge tank 5 is returned, products pot 7 can be entered in this way to avoid product not up to standard, polluted products pot 7, realizes that product continues surely
It is fixed to produce to the purpose of products pot 7.
Claims (8)
1. a kind of high-purity ammon continuous process system, which is characterized in that including raw material ammonia storage tank (1), feed pump (2), vaporizer
(3), filter (4), two-stage ammonia device of spiral-screen column, the first surge tank (5), the second surge tank (6), products pot (7), liquid pouring pump
(8), analysis detection instrument (9), the raw material ammonia storage tank (1) are connected with feed pump (2) entrance, feed pump (2) outlet and vaporizer
(3) entrance is connected, and vaporizer (3) gaseous phase outlet is connected with filter (4) by ammonia pipeline, filter (4) and two-stage ammonia essence
It evaporates tower apparatus to be connected, the product extraction mouth of two-stage ammonia device of spiral-screen column is connected with liquefied ammonia pipeline, and analysis detection instrument (9), first are delayed
It rushes tank (5) and the second surge tank (6) is connected in turn on the liquefied ammonia pipeline connecting with product extraction mouth, the first surge tank (5), the
The outlet of two surge tanks (6) passes through liquefied ammonia pipeline connection products pot (7) and liquid pouring pump (8), the outlet and raw material ammonia of liquid pouring pump (8)
Storage tank (1) is connected, and two-stage ammonia device of spiral-screen column includes first rectifying column (10) and Second distillation column (11), the first rectifying column
(10) top is equipped with the first condenser (13), and the top of Second distillation column (11) is equipped with the second condenser (14), the first rectifying
Tower (10), Second distillation column (11) bottom be respectively connected with reboiler (12), the gaseous phase outlet and second of the first condenser (13)
The import of rectifying column (11) connects, and the gaseous phase outlet of the second condenser (14) connects exhaust treatment system (15).
2. a kind of high-purity ammon continuous process system according to claim 1, which is characterized in that first rectifying column (10),
Ripple silk net filler is filled in the tower of two rectifying columns (11).
3. a kind of high-purity ammon continuous process system according to claim 1, which is characterized in that the raw material ammonia storage tank (1),
Vaporizer (3), first rectifying column (10), Second distillation column (11), the first surge tank (5), the second surge tank (6), products pot (7)
On be provided with pressure gauge, thermometer and safety valve.
4. a kind of high-purity ammon continuous process system according to claim 1, which is characterized in that the vaporizer (3) is included
There is the heating coil of energy heating water bath.
5. a kind of high-purity ammon continuous process system according to claim 1, which is characterized in that the products pot (7), first
Surge tank (5), the second surge tank (6) are equipped with freezing water leg.
6. a kind of high-purity ammon continuous production processes, which is characterized in that specific step is as follows:
S1: after the assay was approved through liquefied ammonia pipeline discharging to raw material ammonia storage tank (1), raw material ammonia storage tank (1) pressure generally exists raw material ammonia
3-13Bar；
S2: raw material is delivered to vaporizer (3) by raw material ammonia storage tank (1) through feed pump (2), and the feed pump (2) need to use oil-free
Formula delivery pump；
S3: raw material is in vaporizer (3), pressure build up, it is ensured that enough pressure, vaporizer (3) boosting principle are as follows: vaporizer (3)
Interior to have hot-water coil pipe, raw material ammonia carries out pressure build up by the heat that hot-water coil pipe provides, and hot water temperature controls in 30-45
DEG C, vaporizer (3) control pressure is 8-12Bar in normal course of operation；
S4: ammonia becomes gaseous state from liquid in vaporizer (3), and gaseous ammonia enters filter (4) through ammonia pipeline by vaporizer (3)
Remove part particulate matter and oil；
S5: the ammonia for removing oil and particulate matter enters first rectifying column (10), by being equipped at the top of first rectifying column (10)
Condenser decline condensate liquid is provided, reboiler (12) that first rectifying column (10) bottom is equipped with provides upflowing vapor, and ammonia is in essence
It evaporates and realizes liquid phase mass transfer, heat transfer in tower, except the heavy constituent impurity in deammoniation, heavy constituent impurity is water, and water impurity can be removed and be arrived
Within 20ppb；
S6: the ammonia of heavy constituent is removed by the first condenser (13) top of first rectifying column (10), enters Second distillation column
(11), decline condensate liquid, Second distillation column (11) are provided by the second condenser (14) being equipped at the top of Second distillation column (11)
The reboiler (12) that bottom is equipped with provides upflowing vapor, and ammonia is realized liquid phase mass transfer, heat transfer in Second distillation column (11), removed
Light component impurity in ammonia, light component impurity include methane, carbon monoxide, carbon dioxide, oxygen, nitrogen, hydrogen；
S7: the product extraction mouth of Second distillation column (11) is provided with analytical sampling pipeline, is directly connected to analysis detection instrument (9),
Product quality is carried out 24 hours, Always Online" monitoring, monitoring group is divided into water, methane, carbon monoxide, carbon dioxide, oxygen, nitrogen
Gas, hydrogen；
S8: the ammonia purity after analysis detection instrument (9) detection is qualified reaches 99.99999%, the product through Second distillation column (11)
Mouth is produced, the first surge tank (5) are entered by top, the first surge tank (5) is equipped with cooling water jecket, the first surge tank (5) pressure
For 5-8Bar；
Liquefied ammonia in S9: the first surge tank (5) is produced through bottom to products pot (7) by pressure difference；
S10: when there is exception or product quality exception in production line, the product extraction mouth switching connection of two-stage ammonia device of spiral-screen column
To the second surge tank (6), production-line technique is checked, when production line restores normal, it is slow that product extraction mouth switches back into first
It rushes tank (5), the liquefied ammonia in the second surge tank (6) can be through liquid pouring pump (8), batch turning to raw material ammonia storage tank (1).
7. a kind of high-purity ammon continuous production processes according to claim 6, which is characterized in that in above-mentioned step S5,
First rectifying column (10) is main to be controlled by pressure, and control tower pressure is 6-9bar, and pressure control is by adjusting reboiler (12) heat
Water management.
8. a kind of high-purity ammon continuous production processes according to claim 6, which is characterized in that in above-mentioned step S6,
Second distillation column (11) is main to be controlled by pressure, and control tower pressure is 5-8bar, and pressure control is by adjusting reboiler (12) heat
Water management.
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| CN201811001607.6A CN109231238B (en) | 2018-08-30 | 2018-08-30 | High-purity ammonia continuous production system and production process thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811001607.6A CN109231238B (en) | 2018-08-30 | 2018-08-30 | High-purity ammonia continuous production system and production process thereof |
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| Publication Number | Publication Date |
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| CN109231238A true CN109231238A (en) | 2019-01-18 |
| CN109231238B CN109231238B (en) | 2023-08-15 |
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ID=65069007
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115215498A (en) * | 2022-08-02 | 2022-10-21 | 苏州思萃同位素技术研究所有限公司 | Device and method for hydrogen isotope wastewater treatment and resource utilization and application |
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| CN208948863U (en) * | 2018-08-30 | 2019-06-07 | 海宁市英德赛电子有限公司 | A kind of high-purity ammon continuous process system |
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| GB713911A (en) * | 1952-08-26 | 1954-08-18 | Permutit Co Ltd | Improvements in the purification of the effluents from gas-producing plants |
| KR20090078214A (en) * | 2008-01-14 | 2009-07-17 | 대성산업가스 주식회사 | Method and apparatus for removing moisture from ammonia gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115215498A (en) * | 2022-08-02 | 2022-10-21 | 苏州思萃同位素技术研究所有限公司 | Device and method for hydrogen isotope wastewater treatment and resource utilization and application |
| CN115215498B (en) * | 2022-08-02 | 2023-09-12 | 苏州思萃同位素技术研究所有限公司 | Device, method and application for hydrogen isotope wastewater treatment and resource utilization |
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| Publication number | Publication date |
|---|---|
| CN109231238B (en) | 2023-08-15 |
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