CN109928408A - The method and system of ammonia is recycled from potassium nitrate process by-product ammonium chloride - Google Patents
The method and system of ammonia is recycled from potassium nitrate process by-product ammonium chloride Download PDFInfo
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Abstract
The invention provides the method and system that ammonia is recycled from potassium nitrate process by-product ammonium chloride, the method of especially a kind of utilization process that ammonia is recycled from nitric acid, ammonia and potassium chloride process for preparing potassium nitrate by double decomposition process by-product ammonium chloride, the following steps are included: the wet ammonium chloride for being centrifugated generation in process for preparing potassium nitrate by double decomposition technique or ammonium chloride solution are passed through pretreatment by (1), certain density ammonium chloride solution is made；(2) pretreated ammonium chloride solution is sent into after heat-exchange system in ammonia steaming system and milk of lime, steam reaction；(3) ammonia-containing gas of ammonia steaming system production are sent into compressor after heat-exchange system cooling and water removal etc.；(4) ammonia after compressor compresses send to ammonium nitrate workshop section and nitric acid and prepares ammonium nitrate, raw material of the ammonium nitrate of generation as process for preparing potassium nitrate by double decomposition technique.Technique and system of the invention has the characteristics that continually and steadily to run, simple flow, reduces by-product ammonium chloride, reduces ammonia consumption.
Description
Technical field
The invention belongs to chemical technology field, more particularly to a kind of from the preparation of nitric acid, ammonia and potassium chloride double decomposition
The utilization process for recycling ammonia in potassium nitrate process by-product ammonium chloride product, preparing high-purity calcium chloride solution simultaneously.
Background technique
The production method of potassium nitrate is mainly by sodium nitrate-potassium chloride conversion method, ammonium nitrate-potassium chloride double decomposition, nitric acid
Ammonium-potassium chloride ions exchange process, nitric acid-potassium chloride solvent extraction etc., wherein ammonium nitrate-potassium chloride double decomposition exists former
Expect that convenient sources, process equipment are simple, low energy consumption, byproduct type is few and the advantages such as pollution-free, becomes domestic potassium nitrate at present
The main technique of production.
Ammonium nitrate-potassium chloride double decomposition main flow is: cold after potassium chloride and ammonium nitrate are dissolved by a certain percentage
But cool down, obtain product potassium nitrate using centrifuge separation；50~70 DEG C are cooled to after isolated mother liquid evaporation is concentrated, warp
It is centrifugally separating to obtain wet ammonium chloride, can further be dried to obtain dry ammonium chloride.
The ammonium chloride product of by-product can be used as fertilizer.But the high chlorinity of ammonium chloride it make fertilizer to be easy to cause soil
Earth salinization, while the main way of domestic production ammonium chloride is Hou's process for soda production, the price of ammonium chloride is generally relatively low.Therefore for
The ammonium chloride of potassium nitrate process by-product is sold not advantageous as fertilizer.Raw material ammonium nitrate mainly passes through nitric acid, ammonia neutralizes
The preparation of method technique.Therefore byproduct ammonium chloride is decomposed to the preparation for being prepared into ammonia and being used for raw material ammonium nitrate, to reach ammonia
Recycle.
Sol is tieed up in the technique of legal system soda ash, using the mother liquor of milk of lime and containing ammonium chloride, sodium chloride, ammonium carbonate etc. in vapour
It is reacted in stripper, recycles ammonia and carbon dioxide etc..But while recycling ammonia, 1 ton of soda ash of every preparation will generate about 10m3's
Evaporated waste ammonia liquid, calcium chloride concentration is lower in waste liquid, and there are impurity such as sodium chloride, affects the further benefit of calcium chloride in waste liquid
With.
It with highly acid ammonium salt is the side controlled brilliant agent and prepare large-grain magnesium hydroxide that patent CN101857248B, which is disclosed a kind of,
Method.Its technical process is that the magnesium chloride solution for having configured concentration is heated to 50~90 DEG C, then with a certain amount of highly acid ammonium
Salt (controlling brilliant agent), ammonium hydroxide reaction, generate magnesium hydroxide solid.The highly acid ammonium salt of the high concentration of generation with milk of lime by reacting
Recycle ammonia.The technical process does not carry out heat recovery, and certain magnesium chloride, purity are contained in the calcium salt soln finally generated
It is lower.
Patent CN103693701A discloses a kind of full ashes ammonia steaming device of ammonia-soda process mother liquid and technique.The technical process
It is: is entered after pre- hot mother liquor and pulverized limestone being configured in preliming tank well in stripping destilling tower to recycle ammonia.In the technique
Heat not yet in effect using tower top ammonia, the ammonia of generation contain a large amount of CO2, vapor etc..Meanwhile technique is to raw material lime
The granularity requirements of powder are higher, and Lime Pretreatment equipment investment is larger.
Patent CN102976355A discloses a kind of technique using ammonium chloride and carbide slag production ammonia and calcium chloride.It should
Technical process is that ammonium chloride and carbide slag slurry react in -5~110 DEG C of reactors, produces ammonia and crystallization of calcium chloride.Its
In, after ammonia water or weak aqua ammonia dilution, using distillation, the dry obtained anhydrous ammonia gas of calcium oxide.The Ammonia recovery process stream
Journey is cumbersome, energy consumption is larger, will need to consume a large amount of desiccant using calcium oxide drying.
Summary of the invention
In view of this, the invention is directed to a kind of method that ammonia is recycled from potassium nitrate process by-product ammonium chloride,
Especially one kind recycles ammonia, simultaneously from nitric acid, ammonia and potassium chloride process for preparing potassium nitrate by double decomposition process by-product ammonium chloride product
Prepare the utilization process of high-purity calcium chloride solution.
The system that the present invention also provides a kind of to recycle ammonia from potassium nitrate process by-product ammonium chloride, including heat-exchange system, steaming
Ammonia system and ammonia compression device, the ammonia steaming system include ammonia still, preliming tank and flash evaporation etc., they are sequentially connected.Institute
The one end for stating heat-exchange system is ammonium chloride solution entrance, and one end is connected with ammonia steaming system, and one end is connect with ammonia compression device,
And there are three channel, a channels to enter heat exchange system by ammonia steaming system for ammonia-containing gas for the connection of heat-exchange system and ammonia steaming system
The channel of system, a channel are the channel for entering ammonia steaming system containing ammonia solution condensed in heat-exchange system, and a channel is high temperature
Ammonium chloride solution enters the channel of ammonia steaming system from heat-exchange system.Ammonium chloride solution is sent into ammonia steaming system and pre- through heat-exchange system
Ash bucket, the milk of lime in ammonia still distilling period and through ammonia still tower reactor steam stripping, then ammonia-containing gas of ammonia steaming system production
It is sent into ammonia compression device after heat-exchange system cooling and water removal etc..
The ammonia still is divided into top preheating section and lower part distilling period two parts, and the ammonium chloride solution after preheating enters preheating
Further preheating, preheating section bottom go out liquid and enter preliming tank top, reacted with the milk of lime in preliming tank section, the pre- newborn bottom of ash
Portion goes out liquid and enters at the top of distilling period that the reaction was continued, and outlet enters in the middle part of preliming tank at the top of distilling period, and reaction generates in preliming tank
Ammonia, steam enter preheating section bottom gas-phase space；Live steam is added from distilling period bottom.Preferably, preliming tank stirs for band
The container of device is mixed, milk of lime is added from top；It is furthermore preferred that the waste liquid of distilling period bottom is discharged into level-one shwoot by head of liquid
Device, the secondary steam that level-one flash evaporation top generates return to preheating section bottom gas-phase space, and bottom goes out liquid and enters second level flash evaporation,
The secondary steam generated at the top of second level flash evaporation is sent into distilling period bottom after jet pump pressurizes.
The invention it is a kind of from potassium nitrate process by-product ammonium chloride recycle ammonia method the following steps are included:
(1) it will be centrifugated the wet ammonium chloride of generation in process for preparing potassium nitrate by double decomposition technique, ammonium chloride solution is made；
(2) ammonium chloride solution is sent into after heat-exchange system in ammonia steaming system and milk of lime, steam reaction；
(3) ammonia-containing gas of ammonia steaming system production are sent into compressor after heat-exchange system cooling and water removal etc.；
(4) ammonia after compressor compresses send to ammonium nitrate workshop section and nitric acid and prepares ammonium nitrate, and the ammonium nitrate of generation is made
For the raw material of process for preparing potassium nitrate by double decomposition technique.
Wherein: ammonium chloride solution concentration concentration determination according to needed for generation calcium chloride in the step (1), but it is low
The ammonium chloride solution of concentration will consume the ammonium chloride concentration of more steam and low concentration.General concentration is 15~28wt%.
Further, the ammonium chloride solution in the step (2) is handled by heat-exchange system, is and ammonia still process column overhead outlet
It exchanges heat, recycles heat, reduce heat and cooling capacity consumption.Ammonium chloride solution temperature after heat exchange is according to the big of device location
Air pressure and ammonia still process column overhead temperatures determine；Preferable temperature is 50~80 DEG C.
Further, being sent into ammonia steaming system in heat exchange treated ammonium chloride solution in the step (2) and stone
Grey cream, steam reaction are ammonium chloride and milk of lime reaction generates calcium chloride and ammonia, at the same tower bottom be passed through steam carry out stripping and
Heat is provided.The low-pressure steam specification that steam can have according to existing factory, preferred steam pressure are 0.1~0.5MPaG.
Further, the milk of lime in the step (2) can be what lime generated after adding aquation ash to handle, activity
For CaO concentration between 140~200tt, the concentration of active CaO is higher, more saving lime, but milk of lime viscosity increases, and causes stone
The power consumption of grey cream delivery pump.
Further, the ammonia steaming system in the step (3) includes the equipment such as ammonia still, preliming tank, flash evaporation.Ammonia still
It can be sieve-plate tower or bubble column, be also possible to the destilling tower that sieve plate and bubble-cap have.Preliming tank is the appearance with agitating device
Device.
Further, the ammonia steaming system operating pressure in described can be positive pressure operation, can also be negative-pressure operation.Excessive positive pressure
Operation will consume a large amount of steam, and the solution temperature that tower bottom generates is higher, can not efficiently use, while be easy to causeing ammonia still
Fouling, the operation cycle for reducing ammonia still；Excessive negative-pressure operation, to the more demanding of equipment, investment increases.Preferred operation
Pressure is -0.01~0.01MPaG.The ammonia steaming system tower top operation temperature is determined according to the atmospheric pressure in device location；It is preferred that
Temperature is 60~85 DEG C.
Further, after the gas of the ammonia-containing gas in the step (3), water vapour and a small amount of fixed gas is by pretreatment
Ammonium chloride solution heat exchange, the heat exchange such as cooling water or refrigerant.Ammonia-containing gas temperature after the heat exchange is according to location
The requirement of cooling water, refrigerant temperature or specification and ammonia compressor to moisture content etc. determines that gas temperature can be 5~15
DEG C, so as to the removing moisture of maximum possible, reduce influence of the moisture to compressor performance；Preferred refrigerant is chilled water, gas
Temperature is 12~15 DEG C.Water removal in the step (3) also may include being removed by the way of desiccant or absorption
Water, but a large amount of desiccant will be consumed, operating cost is higher.
Further, the condensate liquid condensed from ammonia-containing gas due to cooling etc. in the step (2) is re-fed into steaming
Ammonia system, to recycle because of condensation absorbed ammonia.
Further, the gas after cooling water removal is sent into compressor compresses, and the compressor in the step (3) and (4) can
To be centrifugal compressor, it is also possible to screw compressor.
Further, the step (4) is that the pressure of compressed ammonia requires to determine according to technique prepared by ammonium nitrate.
Further, the step (4) can be used as double decomposition preparation in the ammonium nitrate that nitric acid and ammonia reaction generate
The raw material of potassium nitrate.
The calcium chloride solution that ammonia steaming system tower reactor in the step (2) generates recycles after the flash distillation of second level flash evaporation
Steam reduces the consumption of live steam and the discharge temperature of calcium chloride solution, while improving the concentration of calcium chloride.
Further, the solution such as the calcium chloride of high-purity that the ammonia steaming system reaction in the step (2) generates can be through quiet
Set the calcium chloride product for being prepared into high-purity by the modes such as tedding or evaporating after clarification.
The invention has the advantage that
(1) process is simple, and ammonia is recycled by way of milk of lime and steam is simply added, and reduces nitric acid, ammonia and chlorination
Potassium prepares the consumption of ammonia in potassium nitrate technique；
(2) present invention recycles heat, if ammonium chloride solution and tower top ammonia-containing gas exchange heat, tower reactor solution
By flash distillation recovered steam and exclusion temperature is reduced, reduces the consumption of live steam and cooling capacity；
(3) present invention not only provides a kind of from nitric acid, ammonia and potassium chloride process for preparing potassium nitrate by double decomposition process by-product chlorination
Ammonia is recycled in ammonium product, reduces the consumption of ammonia, and the circulation technology method of high-purity calcium chloride solution can be prepared simultaneously.
Detailed description of the invention
Fig. 1 is that one kind is returned from from nitric acid, ammonia and potassium chloride process for preparing potassium nitrate by double decomposition process by-product ammonium chloride product
It receives ammonia, reduce ammonia consumption, while preparing the circulation technology flow chart of high-purity calcium chloride solution.
Wherein: 1- heat-exchange system, 2- ammonia steaming system, 3- ammonia compression device
Specific embodiment
In addition to being defined, technical term used in following embodiment has and the invention one of ordinary skill in the art
The identical meanings being commonly understood by.In order to be readily apparent from the technical means, creative features, achievable purpose and effectiveness of the invention
Understand, the present invention is further explained combined with specific embodiments below, without will limit the present invention.
A kind of system recycling ammonia from potassium nitrate process by-product ammonium chloride,
Including heat-exchange system, ammonia steaming system and ammonia compression device, the ammonia steaming system includes ammonia still, preliming tank and sudden strain of a muscle
Device etc. is sent out, they are sequentially connected.One end of the heat-exchange system is ammonium chloride solution entrance, and one end is connected with ammonia steaming system,
One end is connect with ammonia compression device, and the connection of heat-exchange system and ammonia steaming system, there are three channel, a channel is containing ammonia
Gas is entered the channel of heat-exchange system by ammonia steaming system, and a channel is that the ammonia solution that contains condensed in heat-exchange system enters ammonia still process system
The channel of system, a channel are the channel that high-temp chlorination ammonium salt solution enters ammonia steaming system from heat-exchange system.Ammonium chloride solution is through changing
Hot systems are sent into ammonia steaming system with the milk of lime in preliming tank, ammonia still distilling period and through ammonia still tower reactor steam stripping, so
The ammonia-containing gas of ammonia steaming system production are sent into ammonia compression device after heat-exchange system cooling and water removal etc. afterwards.
The ammonia still is divided into top preheating section and lower part distilling period two parts, and the ammonium chloride solution after preheating enters preheating
Further preheating, preheating section bottom go out liquid and enter preliming tank top, reacted with the milk of lime in preliming tank section, the pre- newborn bottom of ash
Portion goes out liquid and enters at the top of distilling period that the reaction was continued, and outlet enters in the middle part of preliming tank at the top of distilling period, and reaction generates in preliming tank
Ammonia, steam enter preheating section bottom gas-phase space；Preliming tank is the container of belt stirrer, and milk of lime is added from top；Distillation
The waste liquid of section bottom is discharged into level-one flash evaporation by head of liquid, and the secondary steam generated at the top of level-one flash evaporation returns to preheating section
Bottom gas-phase space, bottom go out liquid and enter second level flash evaporation, and the secondary steam generated at the top of second level flash evaporation adds by jet pump
Distilling period bottom is sent into after pressure.Live steam is added from distilling period bottom.
Process example 1
Case study on implementation location atmospheric pressure is 73KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 15wt%
The ammonia-containing gas that 80kg/h (net ammonia content about 3.81kg/h) is sent into heat-exchange system with the discharge of ammonia still process column overhead exchange heat, after heat exchange
Ammonium chloride solution is 73 DEG C, and tower top ammonia-containing gas are cooled to 57.3 DEG C from 78 DEG C.Ammonium chloride solution after heat exchange is sent into ammonia still
Tower top, while the milk of lime 29kg/h of 85 DEG C, the CaO of activity containing 200tt being added on preliming tank, ammonia still tower bottom is passed through 0.5MPaG
Fresh saturated vapor 13kg/h.Control tower top operating pressure 0MPaG.
Ammonia-containing gas and the heat exchange of 27 DEG C of recirculated water after exchanging heat with ammonium chloride solution are cooled to 32 DEG C, then pass through 7 DEG C
Chilled water is cooled to 12 DEG C, and moisture content is reduced to 1wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use screw rod
It is sent after compressor compresses ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation returns to nitric acid as raw material
In potassium technique.
103.3 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 93 DEG C after two-stage flash, and primary flash vapour is direct
It is passed through ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 13kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is 1214W.
Process implementing counter-example 1
Case study on implementation location atmospheric pressure is 73KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 15wt%
80kg/h (net ammonia content about 3.81kg/h) is sent into ammonia still process column overhead, while 85 DEG C, the CaO of activity containing 200tt being added on preliming tank
Milk of lime 29kg/h, ammonia still tower bottom is passed through the fresh saturated vapor 27kg/h of 0.5MPaG.Control tower top operating pressure
0MPaG。
The ammonia-containing gas and the heat exchange of 27 DEG C of recirculated water that 77.6 DEG C of tower top are cooled to 32 DEG C, then are dropped by 7 DEG C of chilled water
For temperature to 12 DEG C, moisture content is reduced to 1wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use helical-lobe compressor pressure
It is sent after contracting ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation returns to potassium nitrate technique as raw material
In.
103 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 93 DEG C after two-stage flash, and primary flash vapour is directly logical
Enter ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 27kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is
10510W.Compared with Example 1, implement counter-example 1 and consume 2 times that steam is embodiment 1, cooling capacity is 8.66 times of embodiment 1.It says
Bright tower top heat recovery facilitates energy-saving.
Process example 2
Case study on implementation location atmospheric pressure is 73KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 17wt%
The ammonia-containing gas that 50kg/h (net ammonia content about 2.70kg/h) is sent into heat-exchange system with the discharge of ammonia still process column overhead exchange heat, after heat exchange
Ammonium chloride solution is 50 DEG C, and tower top ammonia-containing gas are cooled to 62.3 DEG C from 71.3 DEG C.Ammonium chloride solution after heat exchange is sent into ammonia still process
Column overhead, while the milk of lime 24.8kg/h of 85 DEG C, the CaO of activity containing 160tt being added on preliming tank, ammonia still tower bottom is passed through
The fresh saturated vapor 10kg/h of 0.2MPaG.Control tower top operating pressure -0.01MPaG.
Ammonia-containing gas and the heat exchange of 32 DEG C of recirculated water after exchanging heat with ammonium chloride solution are cooled to 37 DEG C, then pass through 7 DEG C
Chilled water is cooled to 12 DEG C, and moisture content is reduced to 1.2wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use spiral shell
It is sent after the compression of bar compressor compresses ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation is returned as raw material
Into potassium nitrate technique.
100.5 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 89 DEG C after two-stage flash, and primary flash vapour is direct
It is passed through in the middle part of ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 10kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is 1584W.
Process implementing counter-example 2
Case study on implementation location atmospheric pressure is 73KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 17wt%
50kg/h (net ammonia content about 2.70kg/h) is sent into ammonia still process column overhead, while 85 DEG C, the CaO of activity containing 160tt being added on preliming tank
Milk of lime 24.8kg/h, ammonia still tower bottom is passed through the fresh saturated vapor 13kg/h of 0.2MPaG.Control tower top operating pressure-
0.01MPaG。
The ammonia-containing gas and the heat exchange of 27 DEG C of recirculated water that 71.1 DEG C of tower top are cooled to 32 DEG C, then are dropped by 7 DEG C of chilled water
For temperature to 12 DEG C, moisture content is reduced to 1.1wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use helical-lobe compressor
It is sent after compression ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation returns to potassium nitrate technique as raw material
In.
102 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 88 DEG C after two-stage flash, and primary flash vapour is directly logical
Enter ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 13kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is 3447W.
Compared with Example 2, implement counter-example 2 and consume 1.3 times that steam is embodiment 2, cooling capacity is 2.176 times of embodiment 2.Illustrate tower
Top heat recycling facilitates energy-saving.
Process example 3
Case study on implementation location atmospheric pressure is 73KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 17wt%
The ammonia-containing gas that 50kg/h (net ammonia content about 2.70kg/h) is sent into heat-exchange system with the discharge of ammonia still process column overhead exchange heat, after heat exchange
Ammonium chloride solution is 70 DEG C, and tower top ammonia-containing gas are cooled to 66.8 DEG C from 80.6 DEG C.Ammonium chloride solution after heat exchange is sent into ammonia still process
Column overhead, while the milk of lime 28.4kg/h of 85 DEG C, the CaO of activity containing 140tt being added on preliming tank, ammonia still tower bottom is passed through
The fresh saturated vapor 11kg/h of 0.1MPaG.Control tower top operating pressure 0.01MPaG.
Ammonia-containing gas and the heat exchange of 32 DEG C of recirculated water after exchanging heat with ammonium chloride solution are cooled to 37 DEG C, then pass through 7 DEG C
Chilled water is cooled to 12 DEG C, and moisture content is reduced to 0.8wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use spiral shell
It is sent after the compression of bar compressor compresses ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation is returned as raw material
Into potassium nitrate technique.
105.6 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 96 DEG C after two-stage flash, and primary flash vapour is direct
It is passed through in the middle part of ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 11kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is 2040W.
Process implementing counter-example 3
Case study on implementation location atmospheric pressure is 73KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 17wt%
50kg/h (net ammonia content about 2.70kg/h) is sent into ammonia still process column overhead, while 85 DEG C, the CaO of activity containing 140tt being added on preliming tank
Milk of lime 28.4kg/h, ammonia still tower bottom is passed through the fresh saturated vapor 17kg/h of 0.1MPaG.Control tower top operating pressure
0.01MPaG。
The ammonia-containing gas and the heat exchange of 27 DEG C of recirculated water that 80 DEG C of tower top are cooled to 32 DEG C, then are cooled down by 7 DEG C of chilled water
To 12 DEG C, moisture content is reduced to 0.8wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use helical-lobe compressor pressure
It is sent after contracting ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation returns to potassium nitrate technique as raw material
In.
106 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 97 DEG C after two-stage flash, and primary flash vapour is directly logical
Enter ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 17kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is 5913W.
Compared with Example 3, implement counter-example 3 and consume 1.545 times that steam is embodiment 3, cooling capacity is 2.898 times of embodiment 3.Explanation
Tower top heat recovery facilitates energy-saving.
Process example 4
Case study on implementation location atmospheric pressure is 100KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 28wt%
The ammonia-containing gas that 60kg/h (net ammonia content about 5.338kg/h) is sent into heat-exchange system with the discharge of ammonia still process column overhead exchange heat, heat exchange
Afterchlorinate ammonium salt solution is 80 DEG C, and tower top ammonia-containing gas are cooled to 78 DEG C from 85 DEG C.Ammonium chloride solution after heat exchange is sent into ammonia still
Tower top, while the milk of lime 40.2kg/h of 85 DEG C, the CaO of activity containing 200tt being added on preliming tank, ammonia still tower bottom is passed through
The fresh saturated vapor 20kg/h of 0.4MPaG.Control tower top operating pressure 0MPaG.
Ammonia-containing gas and the heat exchange of 27 DEG C of recirculated water after exchanging heat with ammonium chloride solution are cooled to 32 DEG C, then pass through 7 DEG C
Chilled water is cooled to 12 DEG C, and moisture content is reduced to 0.62wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally use spiral shell
It is sent after bar compressor compresses ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation returns to nitre as raw material
In sour potassium technique.
111 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 103.5 DEG C after two-stage flash, and primary flash vapour is direct
It is passed through ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 20kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is 5505W.
Process implementing counter-example 4
Case study on implementation location atmospheric pressure is 100KPaA.
After the wet chloride leach generated in potassium nitrate technique, 25 DEG C, the ammonium chloride solution of containing ammonium chloride 28wt%
60kg/h (net ammonia content about 5.338kg/h) is sent into ammonia still process column overhead, while 85 DEG C, the CaO of activity containing 200tt being added on preliming tank
Milk of lime 40.2kg/h, ammonia still tower bottom is passed through the fresh saturated vapor 40kg/h of 0.4MPaG.Control tower top operating pressure
0MPaG。
The ammonia-containing gas and the heat exchange of 27 DEG C of recirculated water that 85 DEG C of tower top are cooled to 32 DEG C, then are cooled down by 7 DEG C of chilled water
To 12 DEG C, moisture content is reduced to 1wt%；The ammonia still process column overhead of pumped back containing ammonia solution of condensation.Finally compressed using helical-lobe compressor
It is sent after ammonia-containing gas to ammonium nitrate preparation workshop and generates ammonium nitrate, the ammonium nitrate of generation returns in potassium nitrate technique as raw material.
103 DEG C of the waste liquid that ammonia still tower reactor generates is cooled to 93 DEG C after two-stage flash, and primary flash vapour is directly logical
Enter ammonia still, two-stage flash vapour is sent into ammonia still as heat source after injector pressure-raising.
The steam of the ammonia consumption 40kg/h of 99.9wt% is recycled, the cooling capacity for needing to consume recirculated water and chilled water is
18781W.Compared with Example 4, implement counter-example 4 and consume 2 times that steam is embodiment 1, cooling capacity is 3.41 times of embodiment 1.It says
Bright tower top heat recovery facilitates energy-saving.
Claims (10)
1. recycling the method for ammonia from potassium nitrate process by-product ammonium chloride, it is characterised in that: the described method comprises the following steps:
(1) it will be centrifugated the wet ammonium chloride of generation in process for preparing potassium nitrate by double decomposition technique, ammonium chloride solution is made；
(2) ammonium chloride solution is sent into after heat-exchange system in ammonia steaming system and milk of lime, steam reaction；
(3) ammonia-containing gas of ammonia steaming system production are sent into compressor after heat-exchange system cools down and removes water；
(4) ammonia after compressor compresses send to ammonium nitrate workshop section and nitric acid and prepares ammonium nitrate, and the ammonium nitrate of generation is as multiple
Decomposition method prepares the raw material of potassium nitrate technique.
2. according to the method described in claim 1, it is characterized by: the ammonium chloride solution in the step (2) is by heat exchange system
System processing, the ammonium chloride solution temperature after heat exchange are 50~80 DEG C.
3. according to the method described in claim 1, it is characterized by: tower bottom is passed through steaming in ammonia steaming system in the step (3)
Vapour, steam pressure are 0.1~0.5MPaG.
4. according to the method described in claim 1, it is characterized by: the milk of lime in the step (2) is lime by adding water
It is generated after ashing processing, active CaO concentration is between 140~200tt.
5. according to the method described in claim 1, it is characterized by: in step (2) in heat-exchange system due to cooling from contain ammonia
The condensate liquid condensed in gas is re-fed into ammonia steaming system, to recycle because of condensation absorbed ammonia.
6. according to the method described in claim 1, it is characterized by: the operation pressure of ammonia steaming system described in the step (3)
Power is -0.01~0.01MPaG；Operation temperature is 60~85 DEG C.
7. according to the method described in claim 1, it is characterized by: the production of ammonia steaming system described in the step (3) contains
Ammonia gas cools down by heat-exchange system, and the ammonia temperature after cooling is determined according to the temperature of refrigerant, and temperature is 5~15 DEG C；It is excellent
Choosing makees refrigerant using chilled water, and the ammonia temperature after cooling is preferably 12~15 DEG C.
8. according to the method described in claim 1, it is characterized by: what the ammonia steaming system tower reactor in the step (2) generated
Calcium chloride solution recovered steam after the flash distillation of second level flash evaporation；Preferably, the ammonia steaming system in the step (2), which reacts, produces
The calcium chloride solution of raw high-purity is after standing clarification by tedding or evaporation mode is prepared into the calcium chloride product of high-purity.
9. the system for recycling ammonia from potassium nitrate process by-product ammonium chloride, including heat-exchange system, ammonia steaming system and ammonia compression
Device, the ammonia steaming system include ammonia still, preliming tank and flash evaporation, they are sequentially connected；One end of the heat-exchange system is
Ammonium chloride solution entrance, one end are connected with ammonia steaming system, and one end is connect with ammonia compression device, and heat-exchange system and ammonia still process
There are three channel, a channel is the channel that ammonia-containing gas are entered heat-exchange system by ammonia steaming system, a channel for the connection of system
For the channel for entering ammonia steaming system containing ammonia solution condensed in heat-exchange system, a channel is from heat exchange for high-temp chlorination ammonium salt solution
System enters the channel of ammonia steaming system；Ammonium chloride solution is sent into ammonia steaming system and preliming tank, ammonia still distilling period through heat-exchange system
Interior milk of lime and through ammonia still tower reactor steam stripping, then the ammonia-containing gas of ammonia steaming system production by heat-exchange system cooling and
It is sent into ammonia compression device after water removal.
10. system according to claim 9, ammonia still is divided into top preheating section and lower part distilling period in the ammonia steaming system
Two parts, the ammonium chloride solution after preheating enter preheating section and further preheat, and preheating section bottom goes out liquid and enters preliming tank top, with
Milk of lime in preliming tank is reacted, and the pre- newborn bottom of ash goes out liquid and enters at the top of distilling period that the reaction was continued, outlet at the top of distilling period
In the middle part of into preliming tank, ammonia, the steam of reaction generation enter preheating section bottom gas-phase space in preliming tank；Live steam is from steaming
Section bottom is evaporated to be added；Preferably, preliming tank is the container of belt stirrer, and milk of lime is added from top；It is furthermore preferred that distilling period bottom
The waste liquid in portion is discharged into level-one flash evaporation by head of liquid, and the secondary steam generated at the top of level-one flash evaporation returns to preheating section bottom
Gas-phase space, bottom go out liquid and enter second level flash evaporation, and the secondary steam generated at the top of second level flash evaporation is after jet pump pressurizes
It is sent into distilling period bottom.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240185A (en) * | 2019-07-02 | 2019-09-17 | 天津渤化工程有限公司 | The production method of high purity magnesium hydroxide |
| CN111099639A (en) * | 2020-01-08 | 2020-05-05 | 广东南方碱业股份有限公司 | Ammonia supply system and method for preparing sodium carbonate |
| CN111268694A (en) * | 2020-03-10 | 2020-06-12 | 邓守国 | Double-solid ammonia distillation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240185A (en) * | 2019-07-02 | 2019-09-17 | 天津渤化工程有限公司 | The production method of high purity magnesium hydroxide |
| CN111099639A (en) * | 2020-01-08 | 2020-05-05 | 广东南方碱业股份有限公司 | Ammonia supply system and method for preparing sodium carbonate |
| CN111268694A (en) * | 2020-03-10 | 2020-06-12 | 邓守国 | Double-solid ammonia distillation method |
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