CN106766672A - Device based on swell refrigeration purification ammonia and the method with device purification ammonia - Google Patents
Device based on swell refrigeration purification ammonia and the method with device purification ammonia Download PDFInfo
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- CN106766672A CN106766672A CN201611001322.3A CN201611001322A CN106766672A CN 106766672 A CN106766672 A CN 106766672A CN 201611001322 A CN201611001322 A CN 201611001322A CN 106766672 A CN106766672 A CN 106766672A
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- heat exchanger
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- liquid separator
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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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0276—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of H2/N2 mixtures, i.e. of ammonia synthesis gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/20—Ammonia synthesis gas, e.g. H2/N2 mixture
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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
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Separation Of Gases By Adsorption (AREA)
- Sorption Type Refrigeration Machines (AREA)
Abstract
A kind of method that ammonia is purified the invention discloses device based on swell refrigeration purification ammonia and with the device, device includes the surge tank, primary adsorption system, Primary filter system, compressor, expansion refrigeration system, gasifier, depth adsorption system, depth-type filtration system, the rectifying column that are sequentially connected, can also include low-temperature liquid filling pump, finished pot, handpiece Water Chilling Units, nitrogen purger and heater.The apparatus and method of the utilization swell refrigeration method Ammonia recovery high purity ammonia of present invention exploitation, it is especially effective to LED factories tail gas recycle high purity ammonia, carry out recycling for the energy.
Description
Technical field
The present invention relates to a kind of ammonia purification technique, and in particular to a kind of device and use based on swell refrigeration purification ammonia
The method that the device purifies ammonia, can be used for the Ammonia recovery purification of LED industry.
Background technology
High-purity ammon acts on big sun can be in industry for silicon nitride film provides nitrogen source and IC manufacturing, compound
Semiconductor, liquid crystal display and preferably provided for cleaning silicon chip cleaning process gas ammonia；High-purity ammon is used as electronics row
The raw material of industry, the quality of its product is most important, is directly connected to the yield of final products, quality for raw material and into
The development of sheet and industry is all have close relationship.The ultrapure ammonia conduct produced using extensive process more than existing market
The source of goods, and the method price eighteenth of the twenty is expensive, product-specific investments are big, and unit price is high.Meanwhile, ammonia（NH4）It is largely used in LED production technologies,
And a large amount of recovery waste gas are produced, polluted the environment if not being used and also result in the wasting of resources；Therefore need to provide new
Method can especially purify recovery ammonia to purify ammonia.
The content of the invention
Ammonia is purified it is an object of the invention to provide a kind of device based on swell refrigeration purification ammonia and with the device
Method, especially suitable recovery ammonia purification pure for raw material ammonia air lift.
To achieve the above object of the invention, the technical solution adopted by the present invention is：It is a kind of that ammonia is purified based on swell refrigeration
Device, including surge tank, primary adsorption system, Primary filter system, compressor, expansion refrigeration system, the gasification being sequentially connected
Device, depth adsorption system, depth-type filtration system, rectifying column；The primary adsorption system includes primary absorber；The primary mistake
Filter system includes primary filter；The first order heat exchange that the expansion refrigeration system includes blower fan braking expanding machine, is sequentially connected
Equipment, second level heat transmission equipment, third level heat transmission equipment；The depth adsorption system includes depth absorber；The depth mistake
Filter system includes deep filter；The rectifying column tower top is provided with condenser, bottom and is provided with tower reactor；The rectifying column is provided with treats essence
Evaporate ammonia feed mouthful and high-purity ammonia discharging opening；The first order heat transmission equipment is by First Heat Exchanger and the first gas-liquid separator group
Into；The second level heat transmission equipment is made up of the second heat exchanger with the second gas-liquid separator；The third level heat transmission equipment is by
Three heat exchangers and the 3rd gas-liquid separator are constituted；The compressor is connected with First Heat Exchanger；The gasifier and the first heat exchange
Device is connected；It is described to treat that rectifying ammonia feed mouthful is located at high-purity ammonia discharging opening lower section；It is described treat rectifying ammonia feed mouthful with it is high-purity
The distance of ammonia discharging opening is the 20~30% of rectifying tower height degree；High-purity ammonia discharging opening is apart from the distance of rectifying tower top
The 10~20% of rectifying tower height degree；Blower fan braking expanding machine successively with the 3rd heat exchanger, the second heat exchanger, First Heat Exchanger
Connection.
In above-mentioned technical proposal, the connection refers to connection between each equipment, is conveyed for gas or liquid, if gas
Body transmission is then tracheae connection, is liquid pipe connection if liquid is transmitted；Pipeline is existing mode with the connected mode of each part,
Do not reveal；Some parts connect multiple miscellaneous parts simultaneously in the present invention, reach save energy, are reached most with minimal consumption
Good refining effect, those skilled in the art may be referred to embodiment of the present invention understanding.
In above-mentioned technical proposal, first order heat transmission equipment, second level heat transmission equipment, the third level heat transmission equipment being sequentially connected
Composition multilevel heat exchanger, the ammonia purity after series more high disposal is higher；Every grade of heat transmission equipment is all by heat exchanger and gas-liquid
Separator is constituted, and heat exchanger includes that the cold source gas gateway for heat exchange, the raw material gateway for separation, liquid ammonia come in and go out
Mouthful, gas-liquid separator includes feed(raw material)inlet, gas vent and liquid outlet；Raw material after heat exchange（Gas-liquid mixture）Into gas
Liquid/gas separator realizes gas-liquid separation, obtains gas and liquid ammonia, enters back into respective transmission path.
In above-mentioned technical proposal, expansion refrigeration system is constituted for crucial, plays the effect of refrigerated separation, and front end receives compression
Mixed gas afterwards, the ammonia after the output liquefaction separation of rear end purifies path according to ammonia, and specific connected mode is the first heat exchange
Device material outlet, the first gas-liquid separator feed(raw material)inlet, the first gas-liquid separator gas vent, the second heat exchanger feed(raw material)inlet,
Second gas-liquid separator feed(raw material)inlet, the second gas-liquid separator gas vent, the 3rd heat exchanger feed(raw material)inlet, the 3rd gas-liquid separation
Device feed(raw material)inlet is sequentially connected；3rd gas-liquid separator liquid outlet is connected with the second heat exchanger liquid ammonia entrance；Second gas-liquid
Separator liquid outlet is connected with the second heat exchanger liquid ammonia entrance；First gas-liquid separator liquid outlet and First Heat Exchanger liquid
Body ammonia entrance is connected；The outlet of second heat exchanger liquid ammonia is connected with First Heat Exchanger liquid ammonia entrance.Preferably, the 3rd gas-liquid point
From device liquid outlet converge with the second gas-liquid separator liquid outlet after be connected with the second heat exchanger liquid ammonia entrance again；Second changes
Hot device liquid ammonia outlet is connected with First Heat Exchanger liquid ammonia entrance again after converging with the first gas-liquid separator liquid outlet；First
The outlet of heat exchanger liquid ammonia is connected with gasifier.So as to by gas-liquid separator separates at different levels liquid ammonia by entering after re-heat
Gasifier, gasify laggard adsorption system, carries out depth absorption, and now ammonia purity is more than 99.1%.
In preferred technical scheme, each gas-liquid separator liquid outlet is connected to fluid pressure valve, for adjusting liquid
The pressure of ammonia is 0.25 MPa；Beneficial to depth absorption and depth-type filtration treatment.
In above-mentioned technical proposal, blower fan braking expanding machine is that oil-free lubrication blower fan brakes expanding machine, for heat exchanger provides cold
Source, blower fan braking expander outlet temperature control is -70 ~ -75 DEG C.Preferably, blower fan braking expanding machine is successively with the 3rd
Heat exchanger, the second heat exchanger, First Heat Exchanger form circulation connection, and the low-temperature receiver of depleted of energy can be returned as the promotion of blower fan
Gas；3rd gas-liquid separator gas vent is sequentially connected with the second heat exchanger, blower fan braking expanding machine, the 3rd gas-liquid separator
By the laggard expansion unit of the second heat exchanger re-heat, reflux heat exchanger makees cold to the cryogenic gas after expansion to light component step by step successively
Source, goes out to reclaim low-temperature receiver after heat exchanger, while light component can also pass into expansion unit does between centers protector；Blower fan braking expansion
Machine is connected with tower bottom of rectifying tower, and between centers protector can be used as tower reactor thermal source；Low-temperature receiver energy can be at utmost utilized, energy-conservation subtracts
Row, reduces energy consumption.
In above-mentioned technical proposal, primary adsorption system is many primary absorbers of series connection, the absorption depth of primary absorber
Spend for oxycarbide less than 10ppm, moisture less than 10ppm, in preferably primary absorber, bottom is aluminum oxide, and top is 5A points
Son sieve；Ensure the precision of successive depths absorption.Depth adsorption system is two groups of depth absorbers in parallel, one group during one group of work
Regeneration is processed, it is ensured that propose that work is continuous, and every group of depth absorber includes many depth adsorption columns of series connection, depth absorption
The adsorption deeply of post is that oxycarbide is less than 1ppm less than 1ppm, moisture；Ammonia after depth absorption is delivered to depth-type filtration.
In above-mentioned technical proposal, regeneration treatment is carried out to depth absorber using nitrogen purging, nitrogen purger includes
Nitrogen heater, noise reduction venting device, nitrogen stream gauge；Nitrogen heater is connected with depth adsorption column, the nitrogen purging after heating
Depth adsorption column realizes that regeneration is processed, and Efficient Cycle is utilized, energy-saving and emission-reduction, the nitrogen discharge after purging.
In above-mentioned technical proposal, can be braked in blower fan and heater is set between expanding machine and tower bottom of rectifying tower, from blower fan
The between centers protection gas that braking expanding machine goes out enters tower reactor after can heating；Further, it is provided with heater ratio in tower reactor lateral wall
Such as electric heater unit, in case between centers protection temperature degree is not enough, strengthening action is played.
In above-mentioned technical proposal, it is described based on swell refrigeration purification ammonia device also include low-temperature liquid filling pump, into
Product tank, handpiece Water Chilling Units, preferably handpiece Water Chilling Units include cold water storage cistern and water pump；Handpiece Water Chilling Units are provided with condenser company with rectifying column tower top
Connect, rectifying tower top condenser low-temperature receiver is provided by handpiece Water Chilling Units, rectifier goes out product high-purity ammon gas, the high-purity ammonia of product passes through
Low-temperature liquid filling pump fill into finished pot, can be used for industrial production.
In above-mentioned technical proposal, surge tank plays cushioning effect to reclaim raw material ammonia；Primary filter system is by primary mistake
Filter is constituted, and treatment, primary filter are compressed to gas into oil-free lubricating piston compressor after filtering out solid impurity
Precision be 1 micron；Compressor is middle pressure piston oil-free lubrication compressor, can be equipped with two groups, and one opens one for being used alternatingly.
Preferred depth filtration system is made up of many deep filters connected, and the precision of deep filter is 0.1 micron.
In above-mentioned technical proposal, limit and treat that rectifying ammonia feed mouthful is rectifying tower height degree with the distance of high-purity ammonia discharging opening
20~30%；High-purity ammonia discharging opening is the 10~20% of rectifying tower height degree apart from the distance of rectifying tower top, and rectifying column is middle pressure
Cryogenic rectification operation, the tower charging in, upper tower discharging, middle part charging, liquid lower floor to tower reactor is light by tower reactor heating
Component rises carries out heat exchange with sinking heavy constituent liquid, and tower top light component removes tail gas absorbing system, can be with maximally effective
Purification ammonia, the high-purity ammonia for obtaining fill into finished pot by low-temperature liquid filling pump, can be used for industrial production.
Device based on swell refrigeration purification ammonia of the invention is directed to technical grade ammonia, and especially LED enterprises reclaim ammonia
The pure high purity ammonia of air lift, therefore, the invention also discloses the above-mentioned device based on swell refrigeration purification ammonia in purification ammonia
Application in gas.
Method the present invention further discloses ammonia is purified using the above-mentioned device based on swell refrigeration purification ammonia, bag
Include following steps：
（1）Entering primary adsorption system after the buffered tank of unstrpped gas carries out primary adsorption treatment；
（2）Gas after primary adsorption treatment carries out primary filter treatment into Primary filter system；
（3）The first gas-liquid separator is entered back into after entering First Heat Exchanger after gas compression after primary filter；First gas-liquid point
Gas from device output is into entering back into the second gas-liquid separator after the second heat exchanger；The gas of the second gas-liquid separator output enters
The 3rd gas-liquid separator is entered back into after entering the 3rd heat exchanger；
The liquid of the first gas-liquid separator output enters gasifier after entering First Heat Exchanger；The liquid of the second gas-liquid separator output
Body enters gasifier after sequentially entering the second heat exchanger, First Heat Exchanger；The liquid of the 3rd gas-liquid separator output is sequentially entered
Enter gasifier after second heat exchanger, First Heat Exchanger；
（4）Gas after gasifier gasification after depth absorption by entering depth-type filtration；
（5）Gas after depth-type filtration treats that rectifying ammonia feed mouthful carries out rectification process into rectifying column from rectifying column；It is last from
Ammonia after the high-purity ammonia discharging opening output purification of rectifying column.
In above-mentioned technical proposal, the unstrpped gas is that ammonia is reclaimed in LED productions；The unstrpped gas volume constituents are：
NH3：8.13%、CH4：29.9%、H2：10.49%、N2：42.18%、O2：8.19%, remaining is moisture and beavy metal impurity.
In above-mentioned technical proposal, First Heat Exchanger is entered after gas compression after primary filter to 2.2MPa；The pressure has
Separated beneficial to expansion, can effectively remove the most of impurity in unstrpped gas, collaboration link is played to successive depths adsorption system
Effect.
In above-mentioned technical proposal, the temperature of the 3rd heat exchanger is -70 ~ -75 DEG C；The temperature of the 3rd heat exchanger is changed less than second
The temperature of hot device；Temperature of the temperature of the second heat exchanger less than First Heat Exchanger；The temperature being stepped up is beneficial to different in ammonia
The separation of component.
In the present invention, absorber carries out adsorption treatment, carbon dioxide and moisture, mistake in absorption unstrpped gas to unstrpped gas
Filter filtering solid particles thing；By volume, carbon oxides in gas is less than 10ppm after primary adsorption treatment, and moisture is less than
10ppm, after depth absorption, oxycarbide is less than 1ppm less than 1ppm, moisture；Solid particulate matter grain after primary filter in gas
Footpath is less than 1 micron, and the solid particulate matter particle diameter after depth-type filtration in gas is less than 0.1 micron.
In above-mentioned technical proposal, the first gas-liquid separator, the second gas-liquid separator, the liquid of the 3rd gas-liquid separator output
Pressure is all 0.25MPa, purity 99.1%.
In above-mentioned technical proposal, the gas after compression enters the first gas-liquid separator, light component after entering First Heat Exchanger
Into the second heat exchanger, the liquefied ammonia for dividing ammonia to get off is liquefied after expenditure and pressure valve is decompressed to 0.25MPa, with the second gas-liquid separation
After device liquid composition converges return first order heat exchanger re-heat, gasifier is removed；From the first gas-liquid separator gaseous component out gas
Body enters the second gas-liquid separator after entering the second heat exchange, and wherein light component enters the 3rd heat exchanger, and the liquefied ammonia for liquefying is through celebrating a festival
The liquid composition that stream valve is decompressed to after 0.25MPa with the 3rd gas-liquid separator separates out is converged, sequentially enter the second heat exchanger,
Enter gasifier after First Heat Exchanger；Enter the 3rd heat exchanger gas by after heat exchange, into the 3rd gas-liquid separator, wherein ammonia
By being decompressed to 0.25MPa by choke valve after liquefaction point ammonia, converge with the liquefied ammonia of the second gas-liquid separator and sequentially enter second
Enter gasifier after heat exchanger, First Heat Exchanger, light component is low after expansion by the laggard expansion unit of the second heat exchanger re-heat
Reflux heat exchanger makees low-temperature receiver to wet body step by step successively, and heat exchanger is gone out after reclaiming low-temperature receiver.
In above-mentioned technical proposal, from expanding machine gas temperature out reach -70 ~ -75 DEG C, sequentially pass through the 3rd heat exchanger,
Second heat exchanger, First Heat Exchanger；From First Heat Exchanger out laggard expansion unit blower fan as brake gas, then blowing machine
With the 3rd gas-liquid separator separates go out as bearing protection gas all the way light component converge, going out to expand unit can be used as rectifying tower
Kettle thermal source is used.
In above-mentioned technical proposal, depth adsorption system is entered by the ammonia of gasifier gasification, carry out depth absorption.Absorption system
It is two groups of depth adsorbers parallel compositions to unite, wherein, one group of work, one group of regeneration, regeneration gas is high pure nitrogen, carbon oxygen to be adsorbed
Compound and moisture to 1ppm and it is following after, by thtee-stage shiplock deep filter, filtering solid particles thing is to after less than 0.1 micron
Into rectifying column middle part.
In above-mentioned technical proposal, rectifying column is to press distillation process in low temperature, middle part charging, liquid lower floor to tower reactor,
Rise by tower reactor heating light component carries out heat exchange with sinking heavy constituent liquid, and overhead condenser low-temperature receiver is by handpiece Water Chilling Units
There is provided, tower top light component removes tail gas absorbing system；Rectifier goes out product high-purity ammon, the remaining industry recyclable conduct of ammonia of bottom of towe
Industrial ammonia is used, and product high-purity ammon carries out filling into finished pot by low-temperature liquid filling pump.
In above-mentioned technical proposal, the exhaust gas composition in the flow includes light component and heavy constituent, and wherein light component is oxygen
Gas, nitrogen, hydrogen, oxycarbide etc., restructuring are divided into water, heavy metal substance etc..
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1. the present invention develops a kind of device and method of utilization swell refrigeration method Ammonia recovery high purity ammonia, creative
Combination multi-stage absorption, multistage filtering and swell refrigeration high purity ammonia, energy is fully utilized, both saved
Can environmental protection again；
2. the present invention first uses preliminary adsorption treatment, then carries out depth absorption, the impurity composition in tail gas is had
The control of effect, with accurately reliability, so as to obtain high purity ammonia gas；
3. the present invention can carry out effective recovery to rectifying tower basic skill or training's industry ammonia, to producing cost-effective control；And
The purification efficiency of purifying plant of the invention is high, and easily operated, cost is relatively low, is suitable to popularization and application.
Brief description of the drawings
Fig. 1 is the structural representation of the device that embodiment one is based on swell refrigeration purification ammonia.
Wherein：1st, surge tank, 2, primary adsorption system, 3, Primary filter system, 4, compressor, 5, expansion refrigeration system,
6th, depth adsorption system, 7, depth-type filtration system, 8, rectifying column, 9, low-temperature liquid filling pump, 10, finished pot, 11, cooling-water machine
Group, 12, primary absorber, 13, primary filter, 14, blower fan braking expanding machine, 15, First Heat Exchanger, the 16, first gas-liquid point
From device, the 17, second heat exchanger, the 18, second gas-liquid separator, the 19, the 3rd heat exchanger, the 20, the 3rd gas-liquid separator, 21, fluid
Pressure-reducing valve, 22, depth absorber, 23, deep filter, 24, nitrogen heater, 25, noise reduction venting device, 26, nitrogen stream gauge,
27th, noise reduction venting device, 28, condenser, 29, tower reactor, 30, cold water storage cistern, 31, water pump, 32, treat rectifying ammonia feed mouthful, 33, high-purity
Ammonia discharging opening, 34, heater, 35, gasifier.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment the invention will be further described：
Embodiment one
Shown in Figure 1, a kind of device based on swell refrigeration purification ammonia includes surge tank 1, primary adsorption system 2, primary
Filtration system 3, compressor 4, swell refrigeration system 5, depth adsorption system 6, depth-type filtration system 7, rectifying column 8, cryogenic liquid fill
Armored pump 9, finished pot 10, handpiece Water Chilling Units 11, gasifier 35；
The primary adsorption system is two primary absorbers 12 of series connection, and adsorption deeply is that oxycarbide is less than 10ppm, moisture
Less than 10ppm；Primary filter system is primary filter 13 that precision is 1 micron；
First order heat transmission equipment, second level heat exchange that the expansion refrigeration system includes blower fan braking expanding machine 14, is sequentially connected
Equipment, third level heat transmission equipment；First order heat transmission equipment is made up of First Heat Exchanger 15 with the first gas-liquid separator 16；The second level
Heat transmission equipment is made up of the second heat exchanger 17 with the second gas-liquid separator 18；Third level heat transmission equipment is by the 3rd heat exchanger 19 and
Three gas-liquid separators 20 are constituted；Heat exchanger includes cold source gas gateway, raw material gateway, liquid ammonia gateway；Gas-liquid separation
Device includes feed(raw material)inlet, gas vent and liquid outlet；Each gas-liquid separator liquid outlet is connected to fluid pressure valve 21；
First Heat Exchanger material outlet, the first gas-liquid separator feed(raw material)inlet, the first gas-liquid separator gas vent, the second heat exchanger are former
Material entrance, the second gas-liquid separator feed(raw material)inlet, the second gas-liquid separator gas vent, the 3rd heat exchanger feed(raw material)inlet, the 3rd
Gas-liquid separator feed(raw material)inlet is sequentially connected；3rd gas-liquid separator liquid outlet is connected with the second heat exchanger liquid ammonia entrance；
Second gas-liquid separator liquid outlet is connected with the second heat exchanger liquid ammonia entrance；First gas-liquid separator liquid outlet and first
Heat exchanger liquid ammonia entrance is connected；The outlet of second heat exchanger liquid ammonia is connected with First Heat Exchanger liquid ammonia entrance；
The depth adsorption system is two groups of depth absorbers 22 in parallel, and every group of depth absorber includes two depth of series connection
Adsorption column, the adsorption deeply of depth adsorption column is less than 1ppm for oxycarbide is less than 1ppm, moisture, and work is controlled by traditional valve
Work group and regeneration group；Depth-type filtration system is the deep filter 23 that three precision connected are 0.1 micron；Also blown including nitrogen
Equipment is swept for the regeneration treatment of adsorption column, is made up of nitrogen heater 24, noise reduction venting device 25, nitrogen stream gauge 26, purged
Nitrogen afterwards is emptied by noise reduction venting device 27；
The compressor is connected with First Heat Exchanger；The gasifier is connected with First Heat Exchanger；Rectifying column tower top is provided with condensation
Device 28, bottom is provided with tower reactor 29, and handpiece Water Chilling Units include cold water storage cistern 30 and water pump 31, handpiece Water Chilling Units and rectifying column tower top condenser
Connection, rectifying tower top condenser low-temperature receiver is provided by handpiece Water Chilling Units；Rectifying column is provided with treats rectifying ammonia feed mouthful 32 and high-purity ammonia
Discharging opening 33；Treat that rectifying ammonia feed mouthful is located at high-purity ammonia discharging opening lower section；Treat that rectifying ammonia feed mouthful goes out with high-purity ammonia
The distance of material mouth is the 22% of rectifying tower height degree；High-purity ammonia discharging opening is rectifying tower height degree apart from the distance of rectifying tower top
18%；
The blower fan braking expanding machine is connected with the 3rd heat exchanger, the second heat exchanger, First Heat Exchanger circulation successively；3rd gas-liquid
Separator gas are exported and are sequentially connected with the second heat exchanger, blower fan braking expanding machine；Blower fan brakes expanding machine and tower bottom of rectifying tower
Connection；Blower fan is braked and heater 34 is set between expanding machine and tower bottom of rectifying tower, from the between centers protection that blower fan braking expanding machine goes out
Gas enters tower reactor after can heating, and heater is provided with evacuation port.
In accompanying drawing, single arrow represents that ammonia purifies direction；Double-head arrow represents low-temperature receiver loop direction；Three arrows represent the 3rd gas
Liquid/gas separator light component direction, supplies as low-temperature receiver all the way, protects gas as between centers all the way；Four arrows represent that between centers protection gas enters
Tower reactor direction；In order to accompanying drawing understands, purging nitrogen direction does not represent that tail gas direction does not represent, condenser water (flow) direction does not have
Have at expression, and same parts mark one, some traditional valve connectors are not marked, and do not influence invention effect.
The method for purifying ammonia using the above-mentioned device based on swell refrigeration purification ammonia, comprises the following steps：
（1）LED factories emission is carried out at primary absorption as primary adsorption system is entered after the buffered tank voltage stabilizing of unstrpped gas
Reason, absorber bottoms are that aluminum oxide top is 5A molecular sieves, by entering primary absorber, oxycarbide in tail gas and moisture are inhaled
It is attached to 10ppm；
（2）Gas after primary adsorption treatment carries out primary filter treatment into Primary filter system, filters out by absorber
Solid impurity after treatment is compressed to gas into oil-free lubricating piston compressor；
（3）Gas compression after primary filter enters the first gas-liquid separator, light group to after entering First Heat Exchanger after 2.2MPa
Divide and enter the second heat exchanger, the liquefied ammonia that liquefaction point ammonia gets off divides after expenditure and pressure valve is decompressed to 0.25MPa with the second gas-liquid
After converging return first order heat exchanger re-heat from device liquid composition, gasifier is removed；From the first gas-liquid separator gaseous component out
Gas enters the second gas-liquid separator after entering the second heat exchange, and wherein light component enters the 3rd heat exchanger, and the liquefied ammonia for liquefying passes through
The liquid composition that choke valve is decompressed to after 0.25MPa with the 3rd gas-liquid separator separates out is converged, and sequentially enters the second heat exchange
Enter gasifier after device, First Heat Exchanger；Enter the 3rd heat exchanger gas by after heat exchange, into the 3rd gas-liquid separator, wherein
Ammonia converges with the liquefied ammonia of the second gas-liquid separator and sequentially enters by being decompressed to 0.25MPa by choke valve after liquefaction point ammonia
After second heat exchanger, First Heat Exchanger enter gasifier, light component by the laggard expansion unit of the second heat exchanger re-heat, after expansion
Cryogenic gas reflux heat exchanger makees low-temperature receiver step by step successively；The temperature of the 3rd heat exchanger is -70 ~ -75 DEG C；The temperature of the second heat exchanger
Degree, the temperature of First Heat Exchanger are raised successively；
- 70 ~ -75 DEG C are reached from expanding machine gas temperature out, the 3rd heat exchanger, the second heat exchanger, the first heat exchange is sequentially passed through
Device；From First Heat Exchanger, out laggard expansion unit blower fan divides as brake gas, then blowing machine and the 3rd gas-liquid separator
Separate out as bearing protection gas all the way light component converge, going out to expand unit can use as tower bottom of rectifying tower thermal source, if necessary
Can be heated by heater；
（4）Enter depth adsorption system by the ammonia of gasifier gasification, carry out depth absorption.Adsorption system is two groups of depth absorption
Device is composed in parallel, wherein, one group of work, one group of regeneration, regeneration gas is high pure nitrogen, oxycarbide to be adsorbed and moisture to 1ppm
And it is following after, by thtee-stage shiplock deep filter, filtering solid particles thing enters rectifying column middle part to less than 0.1 micron afterwards；
（5）Gas after depth-type filtration treats that rectifying ammonia feed mouthful carries out rectification process into rectifying column from rectifying column；It is last from
Ammonia after the high-purity ammonia discharging opening output purification of rectifying column, to press distillation process in low temperature, middle part feeds rectifying column, liquid object
To tower reactor, rise by tower reactor heating light component carries out heat exchange, overhead condenser with sinking heavy constituent liquid for matter lower floor
Low-temperature receiver is provided by handpiece Water Chilling Units, and tower top light component removes tail gas absorbing system；Rectifier goes out product high-purity ammon bulk purity and surpasses
99.9995% is crossed, without metal residual, ammonia is recyclable is used as industrial ammonia for bottom of towe remaining industry, and product high-purity ammon is by Low Temperature Liquid
Body filling pump fill into finished pot.
Embodiment two
Consistent with the structure composition of embodiment one, a kind of device based on swell refrigeration purification ammonia includes the buffering being sequentially connected
Tank, primary adsorption system, Primary filter system, compressor, swell refrigeration system, gasifier, depth adsorption system, depth-type filtration system
System, rectifying column, low-temperature liquid filling pump, finished pot, handpiece Water Chilling Units etc., rectifying column tower top is provided with condenser, bottom and is provided with tower reactor；
Difference is that tower reactor lateral wall sets electric heating cover, is used to supply heat.Using said apparatus, according to carrying for embodiment one
Pure method, rectifier goes out product high-purity ammon bulk purity more than 99.9995%, and without metal residual, the remaining industry ammonia of bottom of towe can
Recovery is used as industrial ammonia, and product high-purity ammon carries out filling into finished pot by low-temperature liquid filling pump.
Embodiment three
Consistent with the structure composition of embodiment one, a kind of device based on swell refrigeration purification ammonia includes the buffering being sequentially connected
Tank, primary adsorption system, Primary filter system, compressor, swell refrigeration system, gasifier, depth adsorption system, depth-type filtration system
System, rectifying column, low-temperature liquid filling pump, finished pot, handpiece Water Chilling Units etc., rectifying column tower top is provided with condenser, bottom and is provided with tower reactor,
It is additionally provided with and treats rectifying ammonia feed mouthful and high-purity ammonia discharging opening；Difference is to treat rectifying ammonia feed mouthful and high-purity ammonia
The distance of discharging opening is the 28% of rectifying tower height degree；High-purity ammonia discharging opening is rectifying tower height degree apart from the distance of rectifying tower top
13%.Using said apparatus, according to the method for purification of embodiment one, rectifier goes out product high-purity ammon bulk purity and exceedes
99.9995%, without metal residual, ammonia is recyclable is used as industrial ammonia for bottom of towe remaining industry, and product high-purity ammon is by cryogenic liquid
Filling pump fill into finished pot.
Example IV
Consistent with the structure composition of embodiment one, a kind of device based on swell refrigeration purification ammonia includes the buffering being sequentially connected
Tank, primary adsorption system, Primary filter system, compressor, swell refrigeration system, gasifier, depth adsorption system, depth-type filtration system
System, rectifying column, low-temperature liquid filling pump, finished pot, handpiece Water Chilling Units etc., rectifying column tower top is provided with condenser, bottom and is provided with tower reactor；
Difference is to be not provided with heater between blower fan braking expanding machine and tower bottom of rectifying tower, from the axle that blower fan braking expanding machine goes out
Between protect gas be directly entered tower reactor.Using said apparatus, according to the method for purification of embodiment one, it is high-purity that rectifier goes out product
, more than 99.9995%, without metal residual, ammonia is recyclable is used as industrial ammonia for bottom of towe remaining industry, and product is high-purity for ammonia bulk purity
Ammonia carries out filling into finished pot by low-temperature liquid filling pump.
Claims (10)
1. it is a kind of based on swell refrigeration purify ammonia device, it is characterised in that：The dress that ammonia is purified based on swell refrigeration
Put including be sequentially connected surge tank, primary adsorption system, Primary filter system, compressor, expansion refrigeration system, gasifier,
Depth adsorption system, depth-type filtration system, rectifying column；The primary adsorption system includes primary absorber；The primary filter
System includes primary filter；The expansion refrigeration system sets including blower fan braking expanding machine, the first order heat exchange being sequentially connected
Standby, second level heat transmission equipment, third level heat transmission equipment；The depth adsorption system includes depth absorber；The depth-type filtration
System includes deep filter；The rectifying column tower top is provided with condenser, bottom and is provided with tower reactor；The rectifying column is provided with treats rectifying
Ammonia feed mouthful and high-purity ammonia discharging opening；The first order heat transmission equipment is by First Heat Exchanger and the first gas-liquid separator group
Into；The second level heat transmission equipment is made up of the second heat exchanger with the second gas-liquid separator；The third level heat transmission equipment is by
Three heat exchangers and the 3rd gas-liquid separator are constituted；The compressor is connected with First Heat Exchanger；The gasifier and the first heat exchange
Device is connected；It is described to treat that rectifying ammonia feed mouthful is located at high-purity ammonia discharging opening lower section；It is described treat rectifying ammonia feed mouthful with it is high-purity
The distance of ammonia discharging opening is the 20~30% of rectifying tower height degree；High-purity ammonia discharging opening is apart from the distance of rectifying tower top
The 10~20% of rectifying tower height degree；Blower fan braking expanding machine successively with the 3rd heat exchanger, the second heat exchanger, First Heat Exchanger
Connection.
2. the device of ammonia is purified based on swell refrigeration according to claim 1, it is characterised in that：The heat exchanger includes cold
Source gas inlet-outlet, raw material gateway, liquid ammonia gateway；The gas-liquid separator include feed(raw material)inlet, gas vent and
Liquid outlet.
3. the device of ammonia is purified based on swell refrigeration according to claim 2, it is characterised in that：Each gas-liquid separator liquid
Body outlet is all connected to fluid pressure valve；It is described based on swell refrigeration purification ammonia device also include low-temperature liquid filling pump, into
Product tank, handpiece Water Chilling Units.
4. the device of ammonia is purified based on swell refrigeration according to claim 2, it is characterised in that：First Heat Exchanger raw material goes out
Mouth, the first gas-liquid separator feed(raw material)inlet, the first gas-liquid separator gas vent, the second heat exchanger feed(raw material)inlet, the second gas-liquid
Separator feed(raw material)inlet, the second gas-liquid separator gas vent, the 3rd heat exchanger feed(raw material)inlet, the 3rd gas-liquid separator raw material enter
Mouth is sequentially connected；3rd gas-liquid separator liquid outlet is connected with the second heat exchanger liquid ammonia entrance；Second gas-liquid separator liquid
Body outlet is connected with the second heat exchanger liquid ammonia entrance；First gas-liquid separator liquid outlet and First Heat Exchanger liquid ammonia entrance
Connection；The outlet of second heat exchanger liquid ammonia is connected with First Heat Exchanger liquid ammonia entrance.
5. the device of ammonia is purified based on swell refrigeration according to claim 2, it is characterised in that：The blower fan braking expansion
Machine forms circulation and is connected with the 3rd heat exchanger, the second heat exchanger, First Heat Exchanger successively；3rd gas-liquid separator gas vent with
Second heat exchanger, blower fan braking expanding machine are sequentially connected；Blower fan braking expanding machine is connected with tower bottom of rectifying tower.
6. the device of ammonia is purified based on swell refrigeration according to claim 1, it is characterised in that：The primary adsorption system
It is many primary absorbers of series connection, the adsorption deeply of the primary absorber is less than for oxycarbide is less than 10ppm, moisture
10ppm；The depth adsorption system is two groups of depth absorbers in parallel, and every group of depth absorber includes many depth of series connection
Adsorption column, the adsorption deeply of the depth adsorption column is less than 1ppm for oxycarbide is less than 1ppm, moisture；The primary filter system
System is made up of primary filter, and the precision of the primary filter is 1 micron；The depth-type filtration system is deep by many connected
Filter composition is spent, the precision of the deep filter is 0.1 micron.
7. application of the device based on swell refrigeration purification ammonia in ammonia is purified described in claim 1.
8. the method for purifying ammonia using the device based on swell refrigeration purification ammonia described in claim 1, it is characterised in that bag
Include following steps：
（1）Entering primary adsorption system after the buffered tank of unstrpped gas carries out primary adsorption treatment；
（2）Gas after primary adsorption treatment carries out primary filter treatment into Primary filter system；
（3）The first gas-liquid separator is entered back into after entering First Heat Exchanger after gas compression after primary filter；First gas-liquid point
Gas from device output is into entering back into the second gas-liquid separator after the second heat exchanger；The gas of the second gas-liquid separator output enters
The 3rd gas-liquid separator is entered back into after entering the 3rd heat exchanger；
The liquid of the first gas-liquid separator output enters gasifier after entering First Heat Exchanger；The liquid of the second gas-liquid separator output
Body enters gasifier after sequentially entering the second heat exchanger, First Heat Exchanger；The liquid of the 3rd gas-liquid separator output is sequentially entered
Enter gasifier after second heat exchanger, First Heat Exchanger；
（4）Gas after gasifier gasification after depth absorption by entering depth-type filtration；
（5）Gas after depth-type filtration treats that rectifying ammonia feed mouthful carries out rectification process into rectifying column from rectifying column；It is last from
Ammonia after the high-purity ammonia discharging opening output purification of rectifying column.
9. method according to claim 8, it is characterised in that：Gas compression after primary filter is to entering the after 2.2MPa
One heat exchanger；The temperature of the 3rd heat exchanger is -70 ~ -75 DEG C；The temperature of the 3rd heat exchanger is less than the second heat exchanger
Temperature；Temperature of the temperature of second heat exchanger less than First Heat Exchanger.
10. method according to claim 8, it is characterised in that：By volume, oxidation of coal in gas after primary adsorption treatment
Thing is less than 10ppm, and moisture is less than 10ppm, and after depth absorption, oxycarbide is less than 1ppm less than 1ppm, moisture；After primary filter
Solid particulate matter particle diameter in gas is less than 1 micron, and the solid particulate matter particle diameter after depth-type filtration in gas is less than 0.1 micron；
First gas-liquid separator, the second gas-liquid separator, the fluid pressure of the 3rd gas-liquid separator output are all 0.25MPa.
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215152 No. 6 Anmin Road, Panyang Industrial Park, Huangdi Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |