CN106766672B - 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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- CN106766672B CN106766672B CN201611001322.3A CN201611001322A CN106766672B CN 106766672 B CN106766672 B CN 106766672B CN 201611001322 A CN201611001322 A CN 201611001322A CN 106766672 B CN106766672 B CN 106766672B
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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
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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
- 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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- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Sorption Type Refrigeration Machines (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention discloses a kind of device based on swell refrigeration purification ammonia and the methods for purifying ammonia with the device, device includes sequentially connected surge tank, primary adsorption system, Primary filter system, compressor, expansion refrigeration system, gasifier, depth adsorption system, depth-type filtration system, rectifying column, can also include low-temperature liquid filling pump, finished pot, water cooler, nitrogen purger and heater.The apparatus and method using swell refrigeration method Ammonia recovery high purity ammonia that the present invention develops, it is especially effective to LED factory 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 techniques, 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 technique
High-purity ammon acts in big sun energy industry and provides nitrogen source and IC manufacturing, compound for silicon nitride film
Semiconductor, liquid crystal display and clean process gas ammonia is preferably provided for cleaning silicon chip；High-purity ammon is as electronics row
The quality of the raw material of industry, product is most important, is directly related to the yield of final products, quality for raw material and at
The development of this and industry is all to have close relationship.Existing market mostly uses the ultrapure ammonia conduct that extensive process is produced
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) be largely used in LED production technology,
And a large amount of recycling exhaust gas are generated, it pollutes the environment if not being used and also results in the wasting of resources；Therefore it needs to provide newly
Method can especially purify recycling ammonia to purify ammonia.
Summary of the invention
Ammonia is purified the object of the present invention is to provide a kind of device based on swell refrigeration purification ammonia and with the device
Method, especially suitable recycling 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 that: it is a kind of based on swell refrigeration purification ammonia
Device, including sequentially connected surge tank, primary adsorption system, Primary filter system, compressor, expansion refrigeration system, gasification
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 expansion refrigeration system includes blower braking expanding machine, the heat exchange of the sequentially connected first order
Equipment, second level heat exchange equipment, third level heat exchange equipment；The depth adsorption system includes depth absorber；The depth mistake
Filter system includes deep filter；Described the top of the distillation column is equipped with condenser, bottom is equipped with tower reactor；The rectifying column is equipped with to essence
Evaporate ammonia feed mouth and high-purity ammonia discharge port；The first order heat exchange equipment is by First Heat Exchanger and the first gas-liquid separator group
At；The second level heat exchange equipment is made of the second heat exchanger and the second gas-liquid separator；The third level heat exchange equipment is by
Three heat exchangers and third gas-liquid separator form；The compressor is connect with First Heat Exchanger；The gasifier and the first heat exchange
Device connection；It is described to be located at below high-purity ammonia discharge port to rectifying ammonia feed mouth；It is described to rectifying ammonia feed mouth with it is high-purity
The distance of ammonia discharge port is the 20~30% of rectifying tower height degree；Distance of the high-purity ammonia discharge port apart from rectifying tower top be
The 10~20% of rectifying tower height degree；Blower braking expanding machine successively with third heat exchanger, the second heat exchanger, First Heat Exchanger
Connection.
In above-mentioned technical proposal, the connection refers to be connected between each equipment, is conveyed for gas or liquid, if gas
Body transmission is then tracheae connection, is liquid pipe connection if liquid transmission；The connection type of pipeline and each component is existing way,
It does not reveal；Some components connect multiple other components simultaneously in the present invention, reach and save the energy, reached most with minimal consumption
Good refining effect, those skilled in the art can understand with reference to the embodiment of the present invention.
In above-mentioned technical proposal, sequentially connected first order heat exchange equipment, second level heat exchange equipment, third level heat exchange equipment
Multilevel heat exchanger is formed, the ammonia purity after series more high disposal is higher；Every grade of heat exchange equipment is all by heat exchanger and gas-liquid
Separator group is at heat exchanger includes entering and leaving for the cold source gas entrance of heat exchange, for isolated raw material entrance, liquid ammonia
Mouthful, gas-liquid separator includes feed(raw material)inlet, gas vent and liquid outlet；Raw material (gas-liquid mixture) after heat exchange enters 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 crucial composition, plays the effect of refrigerated separation, front end receives compression
Mixed gas afterwards, rear end export the ammonia after liquefaction separation, purify path according to ammonia, specific connection type 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, third heat exchanger feed(raw material)inlet, third gas-liquid separation
Device feed(raw material)inlet is sequentially connected；Third gas-liquid separator liquid outlet is connect with the second heat exchanger liquid ammonia entrance；Second gas-liquid
Separator liquid outlet is connect with the second heat exchanger liquid ammonia entrance；First gas-liquid separator liquid outlet and First Heat Exchanger liquid
The connection of body ammonia entrance；The outlet of second heat exchanger liquid ammonia is connect with First Heat Exchanger liquid ammonia entrance.Preferably, third gas-liquid point
It is connect again with the second heat exchanger liquid ammonia entrance after converging from device liquid outlet with the second gas-liquid separator liquid outlet；Second changes
Hot device liquid ammonia outlet is connect 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 connect with gasifier.To enter after re-heat by the liquid ammonia of gas-liquid separator separates at different levels
Gasifier, gasify laggard adsorption system, carries out depth absorption, ammonia purity is more than 99.1% at this time.
In preferred technical solution, each gas-liquid separator liquid outlet is connected to fluid pressure valve, for adjusting liquid
The pressure of ammonia is 0.25 MPa；It is handled conducive to depth absorption with depth-type filtration.
In above-mentioned technical proposal, it is that oil-free lubrication blower brakes expanding machine that blower, which brakes expanding machine, is provided for heat exchanger cold
Source, it is -70 ~ -75 DEG C that blower, which brakes the control of expander outlet temperature,.Preferably, blower braking expanding machine successively with third
Heat exchanger, the second heat exchanger, First Heat Exchanger formation are connected by circulation, and the cold source of depleted of energy can return to the promotion as blower
Gas；Third gas-liquid separator gas vent is sequentially connected with the second heat exchanger, blower braking expanding machine, third gas-liquid separator
Light component passes through the laggard expansion unit of the second heat exchanger re-heat, cryogenic gas after expansion successively step by step reflux heat exchanger make it is cold
Source is out recycling cold source after heat exchanger, while light component can also pass into expansion unit and do between centers protector；Blower braking expansion
Machine is connect with tower bottom of rectifying tower, and between centers protector can be used as tower reactor heat source；Cold source energy can be utmostly utilized, energy conservation subtracts
Row reduces energy consumption.
In above-mentioned technical proposal, primary adsorption system is concatenated more primary absorbers, and the absorption of primary absorber is deep
Degree is that oxycarbide is lower than 10ppm, moisture is lower than 10ppm, and in preferably primary absorber, bottom is aluminium oxide, and top is 5A points
Son sieve；Guarantee the precision of successive depths absorption.Depth adsorption system is two groups of depth absorbers in parallel, one group when one group of work
Regeneration treatment, it is ensured that propose that work is continuous, every group of depth absorber includes concatenated more depth adsorption columns, depth absorption
The adsorption deeply of column is that oxycarbide is lower than 1ppm, moisture is lower than 1ppm；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 meter；Nitrogen heater is connect with depth adsorption column, the nitrogen purging after heating
Depth adsorption column realizes regeneration treatment, and Efficient Cycle utilizes, energy-saving and emission-reduction, purged nitrogen discharge.
In above-mentioned technical proposal, it can be braked in blower and heater is set between expanding machine and tower bottom of rectifying tower, from blower
The between centers protection gas that braking expanding machine goes out enters tower reactor after can heating；Further, heating device ratio is equipped in tower reactor lateral wall
It is inadequate to prevent between centers protection temperature degree such as electric heater unit, play reinforcing effect.
In above-mentioned technical proposal, it is described based on swell refrigeration purification ammonia device further include low-temperature liquid filling pump, at
Product tank, water cooler, preferably water cooler include cold water storage cistern and water pump；Water cooler and the top of the distillation column connect equipped with condenser
It connects, rectifying tower top condenser cold source is provided by water cooler, and rectifier goes out product high-purity ammon gas, and the high-purity ammonia of product passes through
Low-temperature liquid filling pump is filled into finished pot, can be used for industrial production.
In above-mentioned technical proposal, surge tank is that recycling raw material ammonia plays buffer function；Primary filter system is by primary mistake
Filter composition enters oil-free lubricating piston compressor to gas progress compression processing, primary filter after filtering out solid impurity
Precision be 1 micron；Compressor is that middle pressure piston oil-free lubricates compressor, can be equipped with two groups, and one opens one for being used alternatingly.
Preferred depth filtration system is made of concatenated more deep filters, and the precision of deep filter is 0.1 micron.
In above-mentioned technical proposal, limit to rectifying ammonia feed mouth at a distance from high-purity ammonia discharge port as rectifying tower height degree
20~30%；Distance of high-purity ammonia discharge port apart from rectifying tower top is the 10~20% of rectifying tower height degree, and rectifying column is middle pressure
Cryogenic rectification operation, tower is fed in, and upper tower discharging, middle part charging, liquid lower layer to tower reactor heats light by tower reactor
Component, which rises, carries out heat exchange with sinking heavy constituent liquid, and tower top light component removes tail gas absorbing system, can be most effective
Ammonia is purified, obtained high-purity ammonia is filled by low-temperature liquid filling pump into finished pot, can be used for industrial production.
Device based on swell refrigeration purification ammonia of the invention is directed to technical grade ammonia, especially LED enterprise and recycles ammonia
The pure high purity ammonia of air lift, therefore, the invention also discloses the above-mentioned devices based on swell refrigeration purification ammonia in purification ammonia
Application in gas.
The present invention further discloses the method using the above-mentioned device purification ammonia based on swell refrigeration purification ammonia, packets
Include following steps:
(1) unstrpped gas enters the primary primary adsorption treatment of adsorption system progress after surge tank；
(2) gas after primary adsorption treatment enters Primary filter system progress primary filter processing；
(3) the first gas-liquid separator is entered back into after entering First Heat Exchanger after the gas compression after primary filter；First gas
The gas of liquid/gas separator output enters back into the second gas-liquid separator after entering the second heat exchanger；The gas of second gas-liquid separator output
Body enters back into third gas-liquid separator after entering third heat exchanger；
The liquid of first gas-liquid separator output enters gasifier after entering First Heat Exchanger；The output of second gas-liquid separator
Liquid sequentially enter and enter gasifier after the second heat exchanger, First Heat Exchanger；The liquid of third gas-liquid separator output is successively
Enter gasifier after into the second heat exchanger, First Heat Exchanger；
(4) gas after gasifier gasification enters depth-type filtration after depth is adsorbed；
(5) gas after depth-type filtration waits for that rectifying ammonia feed mouth enters rectifying column and carries out rectification process from rectifying column；Most
Afterwards from the ammonia after the high-purity ammonia discharge port output purification of rectifying column.
In above-mentioned technical proposal, the unstrpped gas is LED production recycling ammonia；The unstrpped gas volume constituents are as follows:
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 the gas compression to 2.2MPa after primary filter；The pressure has
Conducive to expansion separation, most of impurity in unstrpped gas can be effectively removed, collaboration link is played to successive depths adsorption system
Effect.
In above-mentioned technical proposal, the temperature of third heat exchanger is -70 ~ -75 DEG C；The temperature of third heat exchanger is changed lower than second
The temperature of hot device；The temperature of second heat exchanger is lower than the temperature of First Heat Exchanger；The temperature being stepped up is conducive to different in ammonia
The separation of component.
In the present invention, absorber carries out adsorption treatment to unstrpped gas, adsorbs carbon dioxide and moisture in unstrpped gas, mistake
Filter filtering solid particles object；By volume, carbon oxides in gas is lower than 10ppm after primary adsorption treatment, and moisture is lower than
10ppm, after depth absorption, oxycarbide is lower than 1ppm lower than 1ppm, moisture；Solid particulate matter grain after primary filter in gas
Diameter is lower than 1 micron, and the solid particulate matter partial size after depth-type filtration in gas is lower than 0.1 micron.
In above-mentioned technical proposal, the first gas-liquid separator, the second gas-liquid separator, third gas-liquid separator output liquid
Pressure is all 0.25MPa, purity 99.1%.
In above-mentioned technical proposal, compressed gas enters the first gas-liquid separator, light component after entering First Heat Exchanger
Into the second heat exchanger, after the liquefied ammonia for dividing ammonia to get off that liquefies is decompressed to 0.25MPa by expenditure and pressure valve, with the second gas-liquid separation
After device liquid composition converges return first order heat exchanger re-heat, gasifier is removed；Gas is come out from the first gas-liquid separator gaseous component
Body enters the second gas-liquid separator after exchanging heat into second, and wherein light component is into third heat exchanger, and the liquefied ammonia to get off that liquefies is through celebrating a festival
Stream valve is decompressed to the liquid composition come out after 0.25MPa with third gas-liquid separator separates and converges, sequentially enter the second heat exchanger,
Enter gasifier after First Heat Exchanger；Into third heat exchanger gas after heat exchange, into third gas-liquid separator, wherein ammonia
0.25MPa is decompressed to by throttle valve after liquefaction divides ammonia, converges with the liquefied ammonia of the second gas-liquid separator and sequentially enters second
Enter gasifier after heat exchanger, First Heat Exchanger, light component passes through the laggard expansion unit of the second heat exchanger re-heat, low after expansion
Successively reflux heat exchanger makees cold source to wet body step by step, goes out heat exchanger after recycling cold source.
In above-mentioned technical proposal, from expanding machine come out gas temperature reach -70 ~ -75 DEG C, successively by third heat exchanger,
Second heat exchanger, First Heat Exchanger；Laggard expansion unit blower is come out as brake gas from First Heat Exchanger, then blowing machine
The bearing protection gas that is used as gone out with third gas-liquid separator separates all the way converge by light component, and expanding unit out can be used as rectifying tower
Kettle heat source uses.
In above-mentioned technical proposal, by the ammonia depth degree adsorption system of gasifier gasification, depth absorption is carried out.Absorption system
System is two groups of depth adsorbers parallel compositions, 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 object is to after 0.1 micron or less
In the middle part of into rectifying column.
In above-mentioned technical proposal, rectifying column is that distillation process is pressed in low temperature, middle part charging, liquid lower layer to tower reactor,
Rise by tower reactor heating light component and carry out heat exchange with sinking heavy constituent liquid, overhead condenser cold source is by water cooler
It provides, tower top light component removes tail gas absorbing system；Rectifier goes out product high-purity ammon, and conduct can be recycled in the remaining industrial ammonia of tower bottom
Industrial ammonia uses, and product high-purity ammon is filled by low-temperature liquid filling pump into finished pot.
In above-mentioned technical proposal, the exhaust gas composition in the process includes light component and heavy constituent, and wherein light component is oxygen
Gas, nitrogen, hydrogen, oxycarbide etc., recombination are divided into water, heavy metal substance etc..
Due to the above technical solutions, the present invention has the following advantages over the prior art:
1. the present invention develops a kind of device and method using swell refrigeration method Ammonia recovery high purity ammonia, wound
Combination multi-stage absorption, multistage filtering and the swell refrigeration high purity ammonia for the property made, enable energy to be fully utilized,
It is energy-saving and environment-friendly；
2. the present invention first uses preliminary adsorption treatment, then carries out depth absorption, the impurity composition in tail gas is enable to obtain
To effective control, there is accurately reliability, to obtain high purity ammonia gas；
3. the present invention can effectively recycle rectifying tower basic skill or training's industry ammonia, production cost is effectively controlled；
And the purification efficiency of purifying plant of the invention is high, and it is easily operated, cost is relatively low, be suitable for popularization and application.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of device of the embodiment one based on swell refrigeration purification ammonia.
Wherein: 1, surge tank, 2, primary adsorption system, 3, Primary filter system, 4, compressor, 5, expansion refrigeration system,
6, 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 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, 19, third heat exchanger, 20, third 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 meter,
27, noise reduction venting device, 28, condenser, 29, tower reactor, 30, cold water storage cistern, 31, water pump, 32, to rectifying ammonia feed mouth, 33, high-purity
Ammonia discharge port, 34, heater, 35, gasifier.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments:
Embodiment one
It is shown in Figure 1, a kind of device based on swell refrigeration purification ammonia include surge tank 1, primary adsorption system 2,
Primary filter system 3, compressor 4, swell refrigeration system 5, depth adsorption system 6, depth-type filtration system 7, rectifying column 8, Low Temperature Liquid
Body filling pump 9, finished pot 10, water cooler 11, gasifier 35；
The primary adsorption system is concatenated two primary absorbers 12, adsorption deeply be oxycarbide lower than 10ppm,
Moisture is lower than 10ppm；Primary filter system is the primary filter 13 that precision is 1 micron；
The expansion refrigeration system includes blower braking expanding machine 14, sequentially connected first order heat exchange equipment, the second level
Heat exchange equipment, third level heat exchange equipment；First order heat exchange equipment is made of First Heat Exchanger 15 and the first gas-liquid separator 16；The
Secondary heat exchange equipment is made of the second heat exchanger 17 and the second gas-liquid separator 18；Third level heat exchange equipment is by third heat exchanger 19
It is formed with third gas-liquid separator 20；Heat exchanger includes cold source gas entrance, raw material entrance, liquid ammonia entrance；Gas-liquid
Separator 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, second are changed
Hot device feed(raw material)inlet, the second gas-liquid separator feed(raw material)inlet, the second gas-liquid separator gas vent, third heat exchanger raw material enter
Mouth, third gas-liquid separator feed(raw material)inlet are sequentially connected；Third gas-liquid separator liquid outlet enters with the second heat exchanger liquid ammonia
Mouth connection；Second gas-liquid separator liquid outlet is connect with the second heat exchanger liquid ammonia entrance；First gas-liquid separator liquid discharge
Mouth is connect with First Heat Exchanger liquid ammonia entrance；The outlet of second heat exchanger liquid ammonia is connect 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 concatenated two
Depth adsorption column, the adsorption deeply of depth adsorption column are that oxycarbide is lower than 1ppm, moisture is lower than 1ppm, are gated by conventional valve
Working group processed and regeneration group；Depth-type filtration system is the deep filter 23 that concatenated three precision are 0.1 micron；It further include nitrogen
Gas purger is used for the regeneration treatment of adsorption column, is made of nitrogen heater 24, noise reduction venting device 25, nitrogen stream meter 26,
Purged nitrogen is emptied by noise reduction venting device 27；
The compressor is connect with First Heat Exchanger；The gasifier is connect with First Heat Exchanger；The top of the distillation column is equipped with
Condenser 28, bottom are equipped with tower reactor 29, and water cooler includes cold water storage cistern 30 and water pump 31, and water cooler is cold with the top of the distillation column
Condenser connection, rectifying tower top condenser cold source are provided by water cooler；Rectifying column be equipped with to rectifying ammonia feed mouth 32 with it is high-purity
Ammonia discharge port 33；It is located at below high-purity ammonia discharge port to rectifying ammonia feed mouth；To rectifying ammonia feed mouth and high-purity ammon
The distance of gas discharge port is the 22% of rectifying tower height degree；Distance of high-purity ammonia discharge port apart from rectifying tower top is rectifying tower height degree
18%；
The blower braking expanding machine is successively connected by circulation with third heat exchanger, the second heat exchanger, First Heat Exchanger；Third
Gas-liquid separator gas vent is sequentially connected with the second heat exchanger, blower braking expanding machine；Blower brakes expanding machine and rectifying column
Tower reactor connection；Blower, which is braked, is arranged heater 34 between expanding machine and tower bottom of rectifying tower, the between centers gone out from blower braking expanding machine
Protection gas enters tower reactor after can heating, heater is equipped with evacuation port.
In attached drawing, single arrow indicates that ammonia purifies direction；Double-head arrow indicates cold source loop direction；Three arrows indicate third gas
Liquid/gas separator light component direction is supplied as cold source all the way, protects gas as between centers all the way；Four arrows indicate between centers protect gas into
Tower reactor direction；In order to which attached drawing understands, purging nitrogen direction does not indicate that tail gas direction does not indicate, condenser water (flow) direction does not have
There is expression, and at same parts mark one, some traditional valve connectors are not marked, and do not influence invention effect.
Utilize the method for the above-mentioned device purification ammonia based on swell refrigeration purification ammonia, comprising the following steps:
(1) LED factory emission enters the primary primary suction of adsorption system progress as unstrpped gas after surge tank pressure stabilizing
Attached processing, absorber bottoms are that aluminium oxide top is 5A molecular sieve, by into primary absorber, oxycarbide in tail gas and water
Divide and is adsorbed to 10ppm；
(2) gas after primary adsorption treatment enters Primary filter system progress primary filter processing, filters out by inhaling
Enter oil-free lubricating piston compressor after the solid impurity of adnexa and compression processing is carried out to gas；
(3) enter the first gas-liquid separator after entering First Heat Exchanger after the gas compression to 2.2MPa after primary filter,
Light component enters the second heat exchanger, after the liquefied ammonia for dividing ammonia to get off that liquefies is decompressed to 0.25MPa by expenditure and pressure valve, with the second gas
After liquid/gas separator liquid composition converges return first order heat exchanger re-heat, gasifier is removed；From the first gas-liquid separator gaseous component
Enter the second gas-liquid separator after gas exchanges heat into second out, wherein light component is into third heat exchanger, and liquefy the liquefied ammonia to get off
The liquid composition come out after throttle valve is decompressed to 0.25MPa with third gas-liquid separator separates is converged, and sequentially enters second
Enter gasifier after heat exchanger, First Heat Exchanger；Into third heat exchanger gas after heat exchange, into third gas-liquid separator,
Wherein ammonia is decompressed to 0.25MPa by throttle valve after liquefaction divides ammonia, converges successively with the liquefied ammonia of the second gas-liquid separator
Enter gasifier after into the second heat exchanger, First Heat Exchanger, light component passes through the laggard expansion unit of the second heat exchanger re-heat, swollen
Successively reflux heat exchanger makees cold source to cryogenic gas after swollen step by step；The temperature of third heat exchanger is -70 ~ -75 DEG C；Second heat exchanger
Temperature, the temperature of First Heat Exchanger successively increases；
The gas temperature come out from expanding machine reaches -70 ~ -75 DEG C, successively passes through third heat exchanger, the second heat exchanger, first
Heat exchanger；Laggard expansion unit blower is come out as brake gas, then blowing machine and third gas-liquid separation from First Heat Exchanger
The conduct bearing protection gas that device is isolated all the way converge by light component, and expanding unit out can be used as the use of tower bottom of rectifying tower heat source, must
It can be heated by heater when wanting；
(4) the ammonia depth degree adsorption system for passing through gasifier gasification, carries out depth absorption.Adsorption system is two groups of depth
Adsorbers parallel composition, wherein one group of work, one group of regeneration, regeneration gas is high pure nitrogen, and oxycarbide to be adsorbed and moisture are extremely
1ppm and it is following after, by thtee-stage shiplock deep filter, filtering solid particles object is to entering in rectifying column after 0.1 micron or less
Portion；
(5) gas after depth-type filtration waits for that rectifying ammonia feed mouth enters rectifying column and carries out rectification process from rectifying column；Most
Afterwards from the ammonia after the high-purity ammonia discharge port output purification of rectifying column, rectifying column is that distillation process is pressed in low temperature, middle part charging, liquid
State substance lower layer rises by tower reactor heating light component to tower reactor and carries out heat exchange with sinking heavy constituent liquid, tower top is cold
Condenser cold source is provided by water cooler, and tower top light component removes tail gas absorbing system；It is pure that rectifier goes out product high-purity ammon volume
Degree is more than 99.9995%, no metal residual, and the remaining industrial ammonia of tower bottom is recyclable to be used as industrial ammonia, and product high-purity ammon is through too low
Geothermal liquid filling pump is filled into finished pot.
Embodiment two
Consistent with one structure composition of embodiment, a kind of device based on swell refrigeration purification ammonia includes sequentially connected slow
Rush tank, primary adsorption system, Primary filter system, compressor, swell refrigeration system, gasifier, depth adsorption system, depth-type filtration
System, rectifying column, low-temperature liquid filling pump, finished pot, water cooler etc., the top of the distillation column is equipped with condenser, bottom is equipped with tower
Kettle；The difference lies in that electric heating cover is arranged in tower reactor lateral wall, to supply heat.Using above-mentioned apparatus, according to embodiment one
Method of purification, it is more than 99.9995% that rectifier, which goes out product high-purity ammon bulk purity, no metal residual, the remaining industrial ammonia of tower bottom
Recyclable to use as industrial ammonia, product high-purity ammon is filled by low-temperature liquid filling pump into finished pot.
Embodiment three
Consistent with one structure composition of embodiment, a kind of device based on swell refrigeration purification ammonia includes sequentially connected slow
Rush tank, primary adsorption system, Primary filter system, compressor, swell refrigeration system, gasifier, depth adsorption system, depth-type filtration
System, rectifying column, low-temperature liquid filling pump, finished pot, water cooler etc., the top of the distillation column is equipped with condenser, bottom is equipped with tower
Kettle is additionally provided with to rectifying ammonia feed mouth and high-purity ammonia discharge port；The difference lies in that rectifying ammonia feed mouth and high-purity ammon
The distance of gas discharge port is the 28% of rectifying tower height degree；Distance of high-purity ammonia discharge port apart from rectifying tower top is rectifying tower height degree
13%.Using above-mentioned apparatus, according to the method for purification of embodiment one, rectifier goes out product high-purity ammon bulk purity and is more than
99.9995%, no metal residual, the remaining industrial ammonia of tower bottom is recyclable to be used as industrial ammonia, and product high-purity ammon passes through cryogenic liquid
Filling pump is filled into finished pot.
Example IV
Consistent with one structure composition of embodiment, a kind of device based on swell refrigeration purification ammonia includes sequentially connected slow
Rush tank, primary adsorption system, Primary filter system, compressor, swell refrigeration system, gasifier, depth adsorption system, depth-type filtration
System, rectifying column, low-temperature liquid filling pump, finished pot, water cooler etc., the top of the distillation column is equipped with condenser, bottom is equipped with tower
Kettle；The difference lies in that being not provided with heater between blower braking expanding machine and tower bottom of rectifying tower, go out from blower braking expanding machine
Between centers protection gas is directly entered tower reactor.Using above-mentioned apparatus, according to the method for purification of embodiment one, rectifier goes out product height
Pure ammonia bulk purity is more than 99.9995%, no metal residual, and the remaining industrial ammonia of tower bottom is recyclable to be used as industrial ammonia, and product is high
Pure ammonia is filled by low-temperature liquid filling pump into finished pot.
Claims (10)
1. a kind of device based on swell refrigeration purification ammonia, it is characterised in that: the dress based on swell refrigeration purification ammonia
Set including 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 includes that blower brakes expanding machine, the heat exchange of the sequentially connected first order is set
Standby, second level heat exchange equipment, third level heat exchange equipment；The depth adsorption system includes depth absorber；The depth-type filtration
System includes deep filter；Described the top of the distillation column is equipped with condenser, bottom is equipped with tower reactor；The rectifying column is equipped with to rectifying
Ammonia feed mouth and high-purity ammonia discharge port；The first order heat exchange equipment is by First Heat Exchanger and the first gas-liquid separator group
At；The second level heat exchange equipment is made of the second heat exchanger and the second gas-liquid separator；The third level heat exchange equipment is by
Three heat exchangers and third gas-liquid separator form；The compressor is connect with First Heat Exchanger；The gasifier and the first heat exchange
Device connection；It is described to be located at below high-purity ammonia discharge port to rectifying ammonia feed mouth；It is described to rectifying ammonia feed mouth with it is high-purity
The distance of ammonia discharge port is the 20~30% of rectifying tower height degree；Distance of the high-purity ammonia discharge port apart from rectifying tower top be
The 10~20% of rectifying tower height degree；Blower braking expanding machine successively with third heat exchanger, the second heat exchanger, First Heat Exchanger
Connection；
Wherein, enter the first gas-liquid separator after First Heat Exchanger is entered after the gas compression to 2.2MPa after primary filter, gently
Component enters the second heat exchanger, after the liquefied ammonia for dividing ammonia to get off that liquefies is decompressed to 0.25MPa by expenditure and pressure valve, with the second gas-liquid
After separator liquid composition converges return first order heat exchanger re-heat, gasifier is removed；Go out from the first gas-liquid separator gaseous component
To enter the second gas-liquid separator after gas exchanges heat into second, wherein light component is into third heat exchanger, and liquefy the liquefied ammonia warp to get off
It crosses after throttle valve is decompressed to 0.25MPa and converges with the liquid composition of third gas-liquid separator separates out, sequentially enter second and change
Enter gasifier after hot device, First Heat Exchanger；Into third heat exchanger gas after heat exchange, into third gas-liquid separator,
Middle ammonia is decompressed to 0.25MPa by throttle valve after liquefaction divides ammonia, with the liquefied ammonia of the second gas-liquid separator converge successively into
Enter gasifier after entering the second heat exchanger, First Heat Exchanger, light component passes through the laggard expansion unit of the second heat exchanger re-heat, expansion
Successively reflux heat exchanger makees cold source to cryogenic gas afterwards step by step；The temperature of third heat exchanger is -70 ~ -75 DEG C；Second heat exchanger
Temperature, the temperature of First Heat Exchanger successively increase.
2. the device according to claim 1 based on swell refrigeration purification ammonia, it is characterised in that: the heat exchanger includes cold
Source gas entrance, raw material entrance, liquid ammonia entrance；The gas-liquid separator include feed(raw material)inlet, gas vent and
Liquid outlet.
3. the device according to claim 2 based on swell refrigeration purification ammonia, 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 further include low-temperature liquid filling pump, at
Product tank, water cooler.
4. the device according to claim 2 based on swell refrigeration purification ammonia, 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, third heat exchanger feed(raw material)inlet, third gas-liquid separator raw material enter
Mouth is sequentially connected；Third gas-liquid separator liquid outlet is connect with the second heat exchanger liquid ammonia entrance；Second gas-liquid separator liquid
Body outlet is connect 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 connect with First Heat Exchanger liquid ammonia entrance.
5. the device according to claim 2 based on swell refrigeration purification ammonia, it is characterised in that: the blower braking expansion
Machine is successively connected by circulation with third heat exchanger, the second heat exchanger, First Heat Exchanger formation；Third gas-liquid separator gas vent with
Second heat exchanger, blower braking expanding machine are sequentially connected；Blower braking expanding machine is connect with tower bottom of rectifying tower.
6. the device according to claim 1 based on swell refrigeration purification ammonia, it is characterised in that: the primary adsorption system
For concatenated more primary absorbers, the adsorption deeply of the primary absorber is that oxycarbide is lower than lower than 10ppm, moisture
10ppm；The depth adsorption system is two groups of depth absorbers in parallel, and every group of depth absorber includes concatenated more depth
Adsorption column, the adsorption deeply of the depth adsorption column are that oxycarbide is lower than 1ppm, moisture is lower than 1ppm；The primary filter system
System is made of primary filter, and the precision of the primary filter is 1 micron；The depth-type filtration system is by concatenated more depths
Filter composition is spent, the precision of the deep filter is 0.1 micron.
7. application of the device in purification ammonia based on swell refrigeration purification ammonia described in claim 1.
8. utilizing the method for the device purification ammonia described in claim 1 based on swell refrigeration purification ammonia, which is characterized in that packet
Include following steps:
(1) unstrpped gas enters the primary primary adsorption treatment of adsorption system progress after surge tank；
(2) gas after primary adsorption treatment enters Primary filter system progress primary filter processing；
(3) the first gas-liquid separator is entered back into after entering First Heat Exchanger after the gas compression after primary filter；First gas-liquid point
Gas from device output enters back into the second gas-liquid separator after entering the second heat exchanger；Second gas-liquid separator output gas into
Third gas-liquid separator is entered back into after entering third heat exchanger；
The liquid of first gas-liquid separator output enters gasifier after entering First Heat Exchanger；The liquid of second gas-liquid separator output
Body enters gasifier after sequentially entering the second heat exchanger, First Heat Exchanger；The liquid of third gas-liquid separator output sequentially enters
Enter gasifier after second heat exchanger, First Heat Exchanger；
(4) gas after gasifier gasification enters depth-type filtration after depth is adsorbed；
(5) gas after depth-type filtration waits for that rectifying ammonia feed mouth enters rectifying column and carries out rectification process from rectifying column；Finally from
Ammonia after the high-purity ammonia discharge port output purification of rectifying column.
9. according to the method described in claim 8, it is characterized by: entering the after gas compression to 2.2MPa after primary filter
One heat exchanger；The temperature of the third heat exchanger is -70 ~ -75 DEG C；The temperature of the third heat exchanger is lower than the second heat exchanger
Temperature；The temperature of second heat exchanger is lower than the temperature of First Heat Exchanger.
10. according to the method described in claim 8, it is characterized by: by volume, oxidation of coal in gas after primary adsorption treatment
Object is lower than 10ppm, and moisture is lower than 10ppm, and after depth absorption, oxycarbide is lower than 1ppm lower than 1ppm, moisture；After primary filter
Solid particulate matter partial size in gas is lower than 1 micron, and the solid particulate matter partial size after depth-type filtration in gas is lower than 0.1 micron；
The fluid pressure that first gas-liquid separator, the second gas-liquid separator, third gas-liquid separator export all is 0.25MPa.
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| US4549890A (en) * | 1982-12-23 | 1985-10-29 | Air Products And Chemicals, Inc. | Process and plant for removing methane and argon from crude ammonia synthesis gas |
| GB2192703A (en) * | 1986-07-17 | 1988-01-20 | Boc Group Plc | Gas treatment method and apparatus |
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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. |