CN105217659B - Method for producing potassium nitrate and system for method - Google Patents

Method for producing potassium nitrate and system for method Download PDF

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Publication number
CN105217659B
CN105217659B CN201510709706.XA CN201510709706A CN105217659B CN 105217659 B CN105217659 B CN 105217659B CN 201510709706 A CN201510709706 A CN 201510709706A CN 105217659 B CN105217659 B CN 105217659B
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pipeline
ion exchange
exchange column
water
stage
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CN105217659A (en
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张春生
张太翔
苏卫
张忠
张文琴
吴慧敏
申晓丽
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Tianji Group potash Co.,Ltd.
Tianji Coal Chemical Industry Group Co Ltd
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Tianji Coal Chemical Industry Group Co Ltd
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Abstract

The invention discloses a method for producing potassium nitrate. The method comprises a potassium chloride feeding stage, a primary back-flushing stage, an ammonium chloride receiving stage, a secondary back-flushing stage, a conventional well-flushing stage, an ammonium nitrate feeding stage and a washing stage. The invention also discloses a system used for realizing the method; the system comprises a potassium chloride feeding pipeline, a primary back-flushing pipeline, an ammonium chloride receiving pipeline, a secondary back-flushing pipeline, a conventional well-flushing pipeline, an ammonium nitrate feeding pipeline and a washing pipeline. According to the method and the system disclosed by the invention, through refined control on the method and staged recycling, wastewater zero discharging is realized; the usage amount of fresh water is greatly reduced, and by-product yield is increased; the output ratio reaches a relatively stable equilibrium.

Description

A kind of method producing potassium nitrate and system thereof
Technical field
The invention belongs to field of fertilizer production, particularly relate to the system used by a kind of method producing potassium nitrate and the method production, the method is, by ion exchange, waste water is carried out Accurate Classification, it is achieved wastewater zero discharge.
Background technology
Potassium nitrate is the nitrogen composite fertilizer of potassium without chlorine of a kind of important raw material of industry and a kind of high-quality, agriculturally it is mainly used in Nicotiana tabacum L., flowers, vegetable, fruit tree and other industrial crops sensitive to chloride ion, can significantly improve the yield and quality, it is also possible to be used for doing the raw material of water soluble fertilizer.It is described as " third generation potash fertilizer " after potassium sulfate.China is a large agricultural country, and the whole nation there are about the soil potassium deficiency of 84%.At present, the production technology of potassium nitrate mainly has natural kentite ore deposit extraction method, double decomposition circulation process, ion exchange, U.S.'s ion exchange, Chile SQM nitre sodium conversion method, South West USA potash company law, Israel's M method etc., although production technology is of a great variety, but China's agricultural potassium nitrate is due to factor restriction slower developments such as production cost, large scale production method technology are immature, therefore, exploitation new technique, new method are the most urgent problems solved.
Ion exchange is as one of which production technology, its wastewater flow rate producing potassium nitrate water consumption and generation is the biggest, as a example by producing 10000 tons of potassium nitrate unit per year, potassium nitrate product per ton consumption fresh water about 40 tons, every h produces waste water about 35 tons, these waste water are original design is i.e. emitted into off-site through simple process, containing substantial amounts of NH in waste water4 +, more than 3000mg/L time the highest, the significantly larger than requirement of total nitrogen 15mg/L in state environmental emissioning standard, not only pollute environment, and a large amount of fresh water need to be consumed.Along with the reinforcement of Environmental protection, traditional ion exchange produces potassium nitrate technology and has been faced with crisis of survival.
Summary of the invention
In order to solve problems of the prior art, the invention discloses one and utilize ion exchange to produce potassium nitrate system and its apparatus, this system is that the waste water produced in production process is carried out classified utilization, it is achieved wastewater zero discharge, fresh water consumption are substantially reduced.
The present invention is achieved through the following technical solutions:
A kind of method producing potassium nitrate, including upper potassium chloride stage, for the first time backwash stage, reception ammonium chloride stage, for the second time backwash stage, just washes stage, upper ammonium nitrate phase, water rinses, wherein:
In the upper potassium chloride stage, Klorvess Liquid was recycled to after ion exchange in deposit groove standby, and was controlled the addition of potassium chloride by flow meter;
Backwash stage for the first time, delivers to carry out backwash for the first time in ion exchange column by the water in deposit groove, and backwash water is recycled in wastewater trough standby;
Receive the ammonium chloride stage, the waste water in wastewater trough is formed after ion exchange ammonium chloride solution and discharges;
Backwash stage for the second time, delivers to carry out second time backwash in ion exchange column by the water in deposit groove, and backwash water is recycled in wastewater trough standby;
Just wash the stage, deliver to ion exchange column is just washed by the water in deposit groove, and the wash water is recycled in deposit groove standby;
Upper ammonium nitrate phase, first exchanges ammonium nitrate solution through ion, then is recycled in deposit groove standby by the solution after exchange;
Water rinses, is drained in ion exchange column wash by the water in deposit groove, is drained into by water lotion in deposit groove standby.
A kind of system for realizing said method, including ion exchange column, wastewater trough and deposit groove, its pipeline constituted includes potassium chloride pipeline, for the first time backwash pipeline, reception ammonium chloride pipeline, for the second time backwash pipeline, just washes pipeline, upper ammonium nitrate pipeline, washing pipeline, wherein:
Described upper potassium chloride pipeline is, potassium chloride import bottom ion exchange column connects with potassium chloride supply line, during Klorvess Liquid enters ion exchange, the waste water of the discharge upper potassium waste water discharge opening from ion exchange column top flows out, and is drained to by the road lay in groove;
Described first time backwash pipeline is, the first time backwash water import bottom the first time backwash water outlet of deposit groove and ion exchange column is connected with wastewater trough by pipeline by pipeline communication, the first time backwash water outlet on ion exchange column top;
Described reception ammonium chloride pipeline is, the liquid outlet of wastewater trough connects entrance ion exchange column by pipeline with the waste water inlet bottom ion exchange column, and the ammonium chloride through described ion exchange column top exports discharge ammonium chloride;
Described second time backwash pipeline is, the second time backwash water import bottom the second time backwash water outlet of deposit groove and ion exchange column is connected with wastewater trough by pipeline by pipeline communication, the second time backwash water outlet on ion exchange column top;
Described pipeline of just washing is, during the wash water outlet of deposit groove enters ion exchange column by the wash water inlet communication of pipeline with described ion exchange column top, the water discharged is discharged by the wash water outlet bottom ion exchange column, and in tuber drainage to described deposit groove;
Described upper ammonium nitrate pipeline is, the ammonium nitrate import of ion exchange column and ammonium nitrate pipeline communication, and the water that ammonium nitrate is discharged during entering ion exchange column upper ammonium wastewater outlet bottom ion exchange column is discharged into described deposit groove.
Described washing pipeline is, the washing outlet of deposit groove and the washing import on ion exchange column top are by pipeline communication, and the waste water that water-washing process produces water lotion outlet bottom ion exchange column is discharged, and is drained in deposit groove standby.
As a kind of preferred implementation, at described potassium chloride supply line, the pipeline between first time backwash water import bottom the first time backwash water outlet of described deposit groove and ion exchange column, the pipeline between second time backwash water import bottom the second time backwash water outlet of described deposit groove and ion exchange column, on the pipeline between waste water inlet bottom the liquid outlet of described wastewater trough and ion exchange column, the pipeline between the wash water outlet and deposit groove bottom described ion exchange column, the pipeline between the wash water outlet and deposit groove bottom described ion exchange column, it is respectively equipped with regulation valve on pipeline between upper potassium wastewater outlet and the deposit groove on described ion exchange column top;And the second time backwash water import bottom potassium chloride import bottom described ion exchange column, the first time backwash water import bottom described ion exchange column, described ion exchange column, the waste water inlet bottom described ion exchange column are same inlet;Ammonium liquid outlet bottom the wash water outlet bottom described ion exchange column, described ion exchange column, the upper potassium wastewater outlet of described ion exchange column upper bottom portion are same liquid outlet.
As a kind of preferred implementation, the wash water at described deposit groove exports and is respectively equipped with valve on the pipeline washed between import on the pipeline between the wash water import on described ion exchange column top, described ammonium nitrate pipeline, the washing outlet of described deposit groove and described ion exchange column top;And the wash water import on described ion exchange column top, the ammonium nitrate import of described ion exchange column, the washing import on described ion exchange column top are same inlet.
As a kind of preferred implementation, the pipeline between the outlet of first time backwash water and the wastewater trough on described ion exchange column top, the second time backwash water on described ion exchange column top export and are respectively equipped with valve on the pipeline between the pipeline between wastewater trough, described ammonium chloride pipeline, the upper potassium wastewater outlet on described ion exchange column top and deposit groove;And the first time backwash water outlet on described ion exchange column top, the second time backwash water outlet on described ion exchange column top, the ammonium chloride outlet on described ion exchange column top, the upper potassium wastewater outlet on described ion exchange column top are same liquid outlet.
As a kind of preferred implementation, described first time backwash pipeline, reception ammonium chloride pipeline, washing pipeline add mother-in-law U.S. meter respectively, described second time backwash pipeline adds conductivity meter.
As a kind of preferred implementation, described deposit groove is additionally provided with fresh water import and/or process condensate import.
Its waste water is accepted as side-product ammonium chloride according to the difference of waste strength, washes and material water by the present invention, and the waste water of lower concentration directly replaces fresh water to use, and reclaims, by method refines control and segmentation, the Appropriate application realized waste water.Being recovered in wastewater trough standby by the backwash waste that first time backwash stage, for the second time backwash stage discharge, the waste water of recovery is mainly used in receiving the consumption during ammonium chloride stage;Upper potassium chloride, just wash, upper ammonium nitrate and washing four-stage row waste water reclamation lay in groove to exchange water, and when just washing stage and water rinses with water be by deposit groove in water supply, owing to deposit groove reclaims the most inadequate production and application of the water yield, therefore appropriate process condensate and/or fresh water (that is: one time water) can be supplemented in deposit groove.After realizing wastewater zero discharge, the usage amount of fresh water be substantially reduced and improve side-product yield, output ratio reaches a relatively stable equilibrium.
Accompanying drawing explanation
Fig. 1 is the process without drainage of waste water flow chart of embodiment of the present invention.
In figure: 1. ion exchange column, 2. deposit groove, 3. wastewater trough.
Detailed description of the invention
In order to be better understood from technical scheme, in conjunction with embodiment, the present invention is further explained explanation.
As it is shown in figure 1, as a example by the potassium nitrate method of potassium nitrate yield 10,000 tons, there are seven stages in one the method cycle: potassium chloride on the first stage, potassium chloride liquid rate of flow of fluid is 2-2.3m3/ h, controls the addition of potassium chloride, used time about 2h, i.e. this stage draining 4-4.6 ton by flow meter, is recovered to exchange water deposit groove 2;Second stage backwash for the first time, the water in stand-by storage groove 2, flow velocity is 3-6m3/ h, controls the end time by the content of mother-in-law U.S. measurement ammonium chloride, and when mother-in-law U.S. angle value is more than 0, backwash for the first time terminates, general used time 2h, i.e. this stage draining 6-12 ton, and is recovered in wastewater trough 3, containing Cl in the waste water of the discharge in this stage-;Phase III receives ammonium chloride, and reception speed is 5-7m3/ h, controls the end time by the content of mother-in-law U.S. measurement ammonium chloride, accepts ammonium chloride when mother-in-law U.S. angle value is equal to 0 and terminate, general used time 4-5h, i.e. this stage water 21-28 ton in wastewater trough 3;Fourth stage second time backwash, the water in stand-by storage groove 2, flow velocity is 3-6m3/ h, surveys Cl by conductivity meter-Content control the end time, when electrical conductivity is less than 3 s/cm, second time backwash terminates, and general used time 1-2h, i.e. this stage draining 3-12 ton, and be recovered to wastewater trough 3, containing Cl in the waste water of the discharge in this stage-And NH4 +;5th stage was just washing, the water in stand-by storage groove 2, and flow velocity is 5-10m3/ h, general used time 0.5-1h terminate, i.e. this stage draining 5-10 ton, and are recovered to lay in groove 2;6th stage upper ammonium nitrate, ammonium nitrate flow velocity is 2.5-2.7m3/ h, is controlled the addition of ammonium nitrate solution, general used time 2h, i.e. this stage draining 5-5.4 ton, and is recovered to lay in groove 2 by flow meter;The washing of 7th stage, the water in stand-by storage groove 2, flow velocity is 5-10m3/ h, is controlled by the content of mother-in-law U.S. measurement potassium nitrate, receives potassium nitrate when mother-in-law U.S. angle value is more than 0 and start, and after 1.5-2h, when mother-in-law U.S. degree is equal to 0, washing terminates, the water 10-15 ton in stand-by storage groove 2.
For realizing the system of said method, including ion exchange column 1, wastewater trough 3 and deposit groove 2, its pipeline constituted includes, upper potassium chloride pipeline, for the first time backwash pipeline, receive ammonium chloride pipeline, for the second time backwash pipeline, just wash pipeline, upper ammonium nitrate pipeline, washing pipeline, wherein:
Described upper potassium chloride pipeline is, potassium chloride import bottom ion exchange column 1 connects with potassium chloride supply line, during Klorvess Liquid enters ion exchange, the waste water of the discharge upper potassium waste water discharge opening from ion exchange column top flows out, and is drained to by the road lay in groove 2;
Described first time backwash pipeline is, the first time backwash water import bottom the first time backwash water outlet of deposit groove 2 and ion exchange column 1 is connected with wastewater trough by pipeline by pipeline communication, the first time backwash water outlet through ion exchange column 1 top;
Described reception ammonium chloride pipeline is, the liquid outlet of wastewater trough 3 connects entrance ion exchange column by pipeline with the waste water inlet bottom ion exchange column 1, and the ammonium chloride through described ion exchange column 1 top exports discharge ammonium chloride;
Described second time backwash pipeline is, the second time backwash water import bottom the second time backwash water outlet of deposit groove 2 and ion exchange column 1 is connected with wastewater trough 3 by pipeline by pipeline communication, the second time backwash water outlet on ion exchange column 1 top;
Described pipeline of just washing is, the wash water outlet of the deposit groove 3 the wash water inlet communication by pipeline Yu described ion exchange column 1 top, the wash water after ion exchange, is exported by the wash water bottom ion exchange column 1 and discharges, and in tuber drainage to described deposit groove 2;
Described upper ammonium nitrate pipeline is, the ammonium nitrate import of ion exchange column 1 and ammonium nitrate pipeline communication, and after ion exchange, the ammonium liquid outlet bottom ion exchange column 1 is discharged into described deposit groove 2 ammonium nitrate.
Described washing pipeline is, the washing outlet of deposit groove 2 is passed through pipeline communication with the washing import on ion exchange column 1 top and entered ion exchange column, and the waste water of discharge is discharged by the wash water outlet bottom ion exchange column, and is drained in deposit groove 2 standby.
Wherein: at described potassium chloride supply line, the pipeline between first time backwash water import bottom the first time backwash water outlet of described deposit groove 2 and ion exchange column 1, the pipeline between second time backwash water import bottom the second time backwash water outlet of described deposit groove 2 and ion exchange column 1, on the pipeline between waste water inlet bottom the liquid outlet of described wastewater trough 3 and ion exchange column 1, the pipeline between the wash water outlet and deposit groove 2 bottom described ion exchange column 1, pipeline between wastewater outlet and deposit groove 2 that upper ammonium process bottom described ion exchange column 1 is discharged, it is respectively equipped with regulation valve on the pipeline between water lotion outlet and deposit groove 2 bottom described ion exchange column 1;And the waste water inlet bottom potassium chloride import bottom described ion exchange column 1, the first time backwash water import bottom described ion exchange column 1, the second time backwash water import bottom described ion exchange column 1, described ion exchange column 1 is same inlet;Water lotion outlet bottom the wash water outlet bottom described ion exchange column 1, the wastewater outlet of upper ammonium process discharge bottom described ion exchange column 1, described ion exchange column 1 is same liquid outlet.
The wash water at described deposit groove 2 exports and is respectively equipped with regulation valve on the pipeline washed between import on the pipeline between the wash water import on described ion exchange column 1 top, described ammonium nitrate pipeline, the washing outlet of described deposit groove 2 and described ion exchange column 1 top;And the wash water import on described ion exchange column 1 top, the ammonium nitrate import of described ion exchange column 1, the washing import on described ion exchange column 1 top are same inlet.
The pipeline between the outlet of first time backwash water and wastewater trough 3 on described ion exchange column 1 top, the second time backwash water on described ion exchange column 1 top export and are respectively equipped with regulation valve on the pipeline between wastewater outlet and the deposit groove 2 of the upper potassium process discharge on the pipeline between wastewater trough 3, described ammonium chloride pipeline, described ion exchange column 1 top;And the wastewater outlet that the first time backwash water outlet on described ion exchange column 1 top, the second time backwash water outlet on described ion exchange column 1 top, the ammonium chloride outlet on described ion exchange column 1 top, the upper potassium process on described ion exchange column 1 top are discharged is same liquid outlet.
Before implementing this new method, annual waste discharge amount is 227991.75 tons, and fresh water consumption 260562 tons adds up to expense about 1000000 yuan;After using the method for the implementation case, annual waste discharge amount is 0 ton, fresh water consumption is less than 12611 tons, total expense about 40000 yuan, only saves one cost that may be reduced by nearly 1000000 yuan of fresh water, and realizes wastewater zero discharge and have prior realistic meaning.

Claims (4)

1. one kind utilizes the method that waste water produces potassium nitrate, it is characterised in that including: goes up potassium chloride stage, for the first time backwash stage, reception ammonium chloride stage, for the second time backwash stage, just wash stage, upper ammonium nitrate phase, water rinses, wherein:
The upper potassium chloride stage, standby in the Water Sproading that Klorvess Liquid adverse current is discharged during entering ion exchange column to deposit groove;
Backwash stage for the first time, sends into the water in deposit groove bottom ion exchange column, carries out the most reverse backwash, and backwash water is recycled in wastewater trough standby;
Receive the ammonium chloride stage, the waste water in wastewater trough is formed after retrograde ion exchanges ammonium chloride solution and discharges;
Backwash stage for the second time, the water in deposit groove adverse current entrance ion exchange column, carries out the reverse backwash of second time, and backwash water is recycled in wastewater trough standby bottom ion exchange column;
Just wash the stage, deliver to ion exchange column is just washed by the water in deposit groove, and the wash water is recycled in deposit groove standby;
Upper ammonium nitrate phase, standby the Water Sproading that ammonium nitrate solution is discharged during ion exchange column top is sent into deposit groove;
Water rinses, is drained in ion exchange column wash by the water in deposit groove, is drained into by initial stage water in deposit groove standby, and monitor stops draining when showing concentration.
2. one kind utilizes the system that waste water produces potassium nitrate, including ion exchange column, wastewater trough, deposit groove, it is characterized in that: be provided with import and export in the bottom of described ion exchange column, the sidewall of described ion exchange column is respectively equipped with inlet and liquid outlet, the pipeline that described ion exchange column, wastewater trough and deposit groove are constituted includes: goes up potassium chloride pipeline, for the first time backwash pipeline, reception ammonium chloride pipeline, for the second time backwash pipeline, just wash pipeline, upper ammonium nitrate pipeline, washing pipeline, wherein:
Described upper potassium chloride pipeline is that potassium chloride supply line connects with the import and export bottom ion exchange column, the waste water that Klorvess Liquid is discharged during entering ion exchange, and the liquid outlet on ion exchange column sidewall is drained to lay in groove;
Described first time backwash pipeline is, the import and export bottom the liquid outlet of deposit groove and ion exchange column are by pipeline communication, and the liquid outlet on ion exchange column sidewall of the water after backwash flows out, and is connected with wastewater trough by pipeline;
Described reception ammonium chloride pipeline is, the liquid outlet of wastewater trough is connected with the import and export bottom ion exchange column by pipeline, and after waste water inversely flows through ion exchange column, the liquid outlet on ion exchange column sidewall is discharged, and is drained to ammonium chloride pipeline;
Described second time backwash pipeline is, the import and export bottom the liquid outlet of deposit groove and ion exchange column are by pipeline communication, and the liquid outlet on ion exchange column sidewall of the water after backwash flows out, and is connected with wastewater trough by pipeline;
Described pipeline of just washing is, the liquid outlet of deposit groove is connected with the inlet on described ion exchange column sidewall by pipeline, and the wash water is after ion exchange column, and the import and export bottom ion exchange column are discharged, and in tuber drainage to described deposit groove;
Described upper ammonium nitrate pipeline is, the inlet on the sidewall of ion exchange column and ammonium nitrate pipeline communication, and ammonium nitrate after ion exchange, discharge, and is drained to by the road in described deposit groove by the import and export bottom ion exchange column;
Described washing pipeline is, the liquid outlet of deposit groove and the inlet on ion exchange column sidewall are by pipeline communication, and after washing, the import and export bottom ion exchange column are discharged, and are drained to by initial stage water in deposit groove standby;
Described deposit groove is additionally provided with fresh water import and/or process condensate import.
Utilize the most as claimed in claim 2 waste water produce potassium nitrate system, it is characterised in that: on described potassium chloride pipeline, for the first time backwash pipeline, receive ammonium chloride pipeline, for the second time backwash pipeline, just wash pipeline, on ammonium nitrate pipeline, washing pipeline on be respectively equipped with regulation valve.
Waste water is utilized to produce the system of potassium nitrate the most as claimed in claim 2, it is characterised in that: on described first time backwash pipeline, reception ammonium chloride pipeline, washing pipeline, add mother-in-law U.S. meter respectively, described second time backwash pipeline adds conductivity meter.
CN201510709706.XA 2015-10-28 2015-10-28 Method for producing potassium nitrate and system for method Active CN105217659B (en)

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JP5293005B2 (en) * 2008-08-29 2013-09-18 住友大阪セメント株式会社 Method and apparatus for recovering thallium and potassium nitrate
CN201458761U (en) * 2009-08-18 2010-05-12 湖南丹化农资有限公司 Vacuum cooling crystallizer for producing potassium nitrate
CN104261438B (en) * 2014-10-10 2016-05-04 诺贝丰(中国)化学有限公司 A kind of system and method for continous way preparing potassium nitrate by means of double decomposition

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Address after: 047500 Zhonghua East Street, Lucheng City, Changzhi City, Shanxi Province

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Patentee before: TIANJI COAL CHEMICAL INDUSTRY GROUP Co.,Ltd.