CN104118891A - Potassium nitrate production process by double decomposition-air cooling crystallization method - Google Patents
Potassium nitrate production process by double decomposition-air cooling crystallization method Download PDFInfo
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- CN104118891A CN104118891A CN201410310839.5A CN201410310839A CN104118891A CN 104118891 A CN104118891 A CN 104118891A CN 201410310839 A CN201410310839 A CN 201410310839A CN 104118891 A CN104118891 A CN 104118891A
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Abstract
A potassium nitrate production process by a double decomposition-air cooling crystallization method is disclosed. Ammonium nitrate and potassium chloride are adopted as raw materials. A double decomposition reaction is adopted to produce the potassium nitrate and ammonium chloride. In a process of producing the potassium nitrate and the ammonium chloride, an air cooling crystallization process is adopted, air is adopted as a cooling medium and is directly mixed with and in contact with a solution and convective heat transfer and diffusion heat transfer occur, thus achieving cooling crystallization of the potassium nitrate and the ammonium chloride. The potassium nitrate production process has characteristics of high raw material utilization rate, significant energy conservation and consumption reduction, good potassium nitrate product quality and good ammonium chloride product quality, and achieves large-scale continuous production.
Description
1, technical field
The present invention relates to a kind of production technique of producing saltpetre and ammonium chloride by ammonium nitrate and Repone K replacement(metathesis)reaction, particularly a kind of production technique that adopts air cooling crystallization technique in the technique of metathesis production saltpetre and ammonium chloride.
2, background technology
Saltpetre is a kind of important inorganic chemical product, according to its purposes, saltpetre is mainly divided into industrial potassium nitrate and agricultural saltpetre, saltpetre mainly adopts nitrate and Repone K conversion method to produce, typical production technique has SODIUMNITRATE and Repone K double decomposition, nitric acid and Repone K conversion method, ammonium nitrate and potassium chloride ions exchange process, and ammonium nitrate and Repone K double decomposition, due to ammonium nitrate and Repone K preparing potassium nitrate by means of double decomposition raw material sources wide, pay product ammonium chloride use value large, at present, domestic main employing ammonium nitrate and Repone K preparing potassium nitrate by means of double decomposition, and announced multinomial Chinese invention patent, as the method > > of Chinese invention patent 200910115890X < < preparing potassium nitrate by means of double decomposition, Chinese invention patent 200910044146.5 < < replacement(metathesis)reactions are produced the method > > of saltpetre and ammonium chloride, the method > > of a Chinese invention patent 200510094223.X < < process for preparing potassium nitrate by double decomposition.
Chinese invention patent 200910115890X and Chinese invention patent 200910044146.5 are produced in saltpetre process, there are two deficiencies: the one, gained work in-process saltpetre product needed is used clear water to rinse potassium nitrate crystals and is washed away to dissolve the ammonia chloride crystal of carrying secretly, simultaneously, also dissolve and washed away a part of potassium nitrate crystals, cause saltpetre that single loop is produced to yield poorly; The 2nd, gained ammonium chloride product is that ammonium chloride product is easily carried potassium nitrate crystals secretly at saltpetre and ammonium chloride crystallization in saturated solution altogether, and not only ammonium chloride product is of poor quality, also causes in saltpetre product the potassium rate of recovery low.Chinese invention patent 200510094223.X produces in saltpetre process, owing to adopting vacuum crystallizing equipment, need to adopt steam to be used for vacuum cyrsytalliser injection and vacuumize, and has the shortcoming that needs to consume a large amount of water coolants and steam, causes energy consumption high.
3, goal of the invention
The object of the invention is to overcome the deficiency of above-mentioned patent, provide a kind of and there is saltpetre and ammonium chloride product quality is good, the potassium rate of recovery is high, production cost is low and can realize the novel process of large-scale continuous production saltpetre.
3, summary of the invention
It is raw material that Repone K and ammonium nitrate are take in the present invention, by replacement(metathesis)reaction, produces saltpetre and ammonium chloride, and production process of the present invention is:
(1) Repone K and ammonium nitrate and water are mixed by a certain percentage and add in batching dissolving tank, pass into steam direct heating, stir, Repone K and ammonium nitrate are fully dissolved, control solution temperature is 70-100 ℃, in control solution, ammonium nitrate and Repone K mol ratio are (1.35-1.8): 1, and controlling solution Baume concentration is 35-44Be.
(2) solution of preparation send strainer to filter after removal impurity, and it is 10-30 ℃ that filtrate send thick potassium crystallisation by cooling system to adopt air cooling crystallization to temperature, and a large amount of Temperatures of crystallization, separate out Temperature and contain certain ammonium chloride impurity; Temperature feed liquid is sent in thick potassium thickener and carried out thickening, Temperature feed liquid after thickening send thick potassium whizzer to carry out separating and dehydrating, in sepn process, to passing into washing water in thick potassium whizzer, Temperature is washed, control after washing chlorion Cl in Temperature product
-content is below 1.5%, obtains thick potassium mother liquor (containing washings) and Temperature after separation.
(3) separating obtained Temperature is added in saltpetre dissolving tank, add pure water and directly pass into steam heating, Temperature is fully dissolved, controlling potassium nitrate solution temperature is 90-115 ℃, and Baume concentration is 44-52 ° of Be.
(4) potassium nitrate solution in saltpetre dissolving tank is sent in smart potassium crystallisation by cooling system and adopts air cooling crystallization to 20-30 ℃, crystallization essence saltpetre; Smart saltpetre feed liquid is sent in smart potassium thickener and carried out thickening, smart saltpetre feed liquid after thickening send smart potassium whizzer to carry out separating and dehydrating again, in sepn process, in smart potassium whizzer, pass into pure water detergent saltpetre product, the washing water yield is the 15-30% of smart saltpetre amount, after separation smart potassium mother liquor (containing washing water) and smart saltpetre, washing water when smart potassium mother liquor returns in (2) as washing Temperature are used.
(5) in separating obtained smart saltpetre product, add appropriate salt of wormwood, salt of wormwood add-on is definite according to the ammonium ion content containing in smart saltpetre product, and then send drying machine dry, is industrial potassium nitrate product after saltpetre product drying.The salt of wormwood adding reacts with ammonium nitrate in saltpetre product and generates saltpetre, and emits CO
2with NH
3thereby, improve product purity.
(6) send preheater to be preheating to 80-100 ℃ in separating obtained thick potassium mother liquor in (2), the few part of thick potassium mother liquor after preheating is for (7) washing ammonium chloride product, and it is 37-43Bc to concentration that the thick potassium mother liquor of rest part send vapo(u)rization system to carry out evaporation concentration.
(7) concentrated solution is sent in ammonium chloride crystallisation by cooling system and adopt air cooling crystallization to 55-70 ℃, a large amount of ammonium chloride of crystallization, separates out ammonium chloride and contains certain saltpetre impurity; Ammonium chloride feed liquid is sent into and in ammonium chloride thickener, carried out thickening, ammonium chloride feed liquid after thickening is sent the centrifuge dehydration of ammonium chloride whizzer, in sepn process, to passing into the thick potassium mother liquor after preheating in (6) in ammonium chloride whizzer, wash, passing into thick potassium mother liquor amount of liquor is the 15-30% of ammonium chloride product amount, to wash away the saltpetre of carrying secretly in ammonium chloride product, after separation, obtain ammonium chloride product and ammonium mother liquor.
(8) ammonium mother liquor, water, Repone K and ammonium nitrate are prepared burden in dissolving tank by a certain percentage mixed adding, pass into steam direct heating, stir, Repone K and ammonium nitrate are fully dissolved, control solution temperature is 70-100 ℃, in control solution, ammonium nitrate and Repone K mol ratio are (1.35-1.8): 1, and controlling solution Baume concentration is 35-44Be.Press said sequence cyclical operation later.
In preparing potassium nitrate by means of double decomposition technique described above, its technical characterictic is, ammonium chloride carries out centrifugal separation processes, uses 80-100 ℃ of thick potassium mother liquor to wash ammonium chloride product, controls potassium ion K in ammonium chloride product
+content is below 0.8%, and thick potassium mother liquor is preheating to after 80-100 ℃, and it can dissolve more saltpetre, but the ammonium chloride amount that can dissolve is much smaller.
In preparing potassium nitrate by means of double decomposition technique described above, its technical characterictic is: Temperature crystallisation by cooling, smart saltpetre crystallisation by cooling and ammonium chloride crystallisation by cooling all adopt air cooling cold crystallization technique, air cooling crystallization technique is to using air as direct mixed contact of heat-eliminating medium and solution, transmission of heat by convection occurs in mixing process to conduct heat with diffusion, solution is cooled and is taken away a part of moisture content by air, the cooling post crystallization crystallize out of solution.Air cooling crystallization technique is mainly comprised of cooling crystallization tower, gas blower, recycle pump, it is by the solution in cooling crystallization tower base channel, by recycle pump, pump to the jet apparatus arranging in tower, solution is sprayed from the bottom up, solution is upwards ejected into after certain altitude, is more freely scattered and falls into tower bottom groove; Simultaneously gas blower blasts air and upwards flows at the bottom of tower, and in the upper and lower process of solution, solution and freezing air are directly mixed, and transmission of heat by convection and diffusion heat transfer occur, the solution crystallization crystalline product that is cooled.The cooling approach of solution in air cooling crystallization tower mainly contains two: the first, utilize solution and enter the temperature head between air in tower, come cooling by thermal conduction; The second,, by entering moisture content in the absorption of air solution in tower, make the moisture evaporation in solution.
In Production of Potassium Nitrate by Double Decomposition-Circulation Method technique described above, its technical characterictic is, Temperature centrifugation adopts two-stage material-pushing centrifuge, the centrifugation of essence saltpetre adopts two-stage material-pushing centrifuge, ammonium chloride centrifugation adopts two-stage material-pushing centrifuge, two-stage material-pushing centrifuge has that separating power is large, good separating effect, and can realize continuous separate from, continuous washing operation.
4, advantage of the present invention
(1) the present invention adopts smart potassium mother liquor to wash Temperature, because saltpetre in smart potassium mother liquor is saturated, but ammonium chloride unsaturation, utilize smart potassium mother liquor to remove to wash ammonium chloride impurity in Temperature product, saltpetre in can dissolved product, washing effect is good, saves water and energy, and has overcome the deficiency that Chinese invention patent 200910115890X and Chinese invention patent 200910044146.5 adopt washing.
(2) the present invention has overcome Chinese invention patent 200910115890X and Chinese invention patent 200910044146.5 deficiencies, employing will go to wash the potassium nitrate crystals of carrying secretly in ammonium chloride product after the preheating of thick potassium mother liquor, potassium content in ammonium chloride product is significantly reduced, in ammonium chloride, the potassium of wash-out is finally converted into saltpetre by circulation, thereby raising feed stock conversion, has saved production cost.
(3) the present invention adds salt of wormwood with micro-ammonium ion in removing product in saltpetre product, thereby has improved product purity.
(4) the present invention adopts air cooling crystallization technique for Temperature and smart saltpetre and ammonium chloride crystallisation by cooling, owing to using air for medium and the direct mixed solution crystallisation by cooling that makes of solution, do not need water consumption consumption vapour, throughput is large, energy-saving effect is remarkable, has overcome in Chinese patent 200510094223.X and has adopted vacuum cooling crystallizer need consume the deficiency of large water gaging and steam.
5, accompanying drawing explanation
Accompanying drawing 1 is metathesis air cooling crystallization method production saltpetre technological process block-diagram of the present invention.
Accompanying drawing 2 is air cooling crystallization process flow diagram of the present invention.
6, embodiment
As shown in Figure 1 and Figure 2, metathesis air cooling crystallization method of the present invention is produced saltpetre technique, and it is that to take Repone K and ammonium nitrate be raw material, by replacement(metathesis)reaction and air cooling crystallization, produces saltpetre and ammonium chloride, and the present invention implements in the following manner:
(1), Repone K, ammonium nitrate and water are mixed by a certain percentage and add in batching dissolving tank, pass into steam direct heating, stir, Repone K and ammonium nitrate are dissolved, and being mixed with temperature and being 70-100 ℃, ammonium nitrate is (1.35-1.8) with Repone K mol ratio: the mixed solution that 1, Baume concentration is 35-44Be.
(2), the solution of preparation send strainer to filter and removes after impurity, filtrate is sent into thick potassium crystallisation by cooling system and is adopted air cooling crystallization technique to carry out crystallisation by cooling, air cooling crystallization technique is mainly by cooling crystallization tower, gas blower, recycle pump forms, it is by the solution in cooling crystallization tower base channel, by recycle pump, pump to the jet apparatus arranging in tower, solution is sprayed from the bottom up, solution is upwards ejected into after certain altitude, freely be scattered again, while gas blower blasts air upwards flows air at the bottom of tower, in the upper and lower process of solution, solution and freezing air are directly mixed, solution is cooled crystallization until temperature is 10-30 ℃, the a large amount of Temperatures of crystallization.Temperature feed liquid is sent in thick potassium thickener and carried out thickening, Temperature feed liquid after thickening is sent into thick potassium whizzer and is carried out separating and dehydrating, thick potassium whizzer adopts two-stage material-pushing centrifuge, in sepn process, to passing into smart potassium mother liquor in thick potassium whizzer, Temperature is washed, control after washing Cl in Temperature product
-content is below 1.5%, separated Temperature and the thick potassium mother liquor of obtaining.
(3), separating obtained Temperature is added to saltpetre dissolving tank, add pure water and directly pass into steam heating, saltpetre is fully dissolved, controlling potassium nitrate solution temperature is 90-115 ℃, and Baume concentration is 44-52 ° of Be.
(4) potassium nitrate solution in saltpetre dissolving tank is sent in smart potassium crystallisation by cooling system and adopted air cooling crystallization technique to carry out crystallisation by cooling, air cooling crystallization technique is mainly by cooling crystallization tower, gas blower, recycle pump forms, it is by the solution in cooling crystallization tower base channel, by recycle pump, pump to the jet apparatus arranging in tower, solution is sprayed from the bottom up, solution is upwards ejected into after certain altitude, freely be scattered again, while gas blower blasts air upwards flows air at the bottom of tower, in the upper and lower process of solution, solution and freezing air are directly mixed, solution is cooled crystallization until to 20-30 ℃, crystallization essence saltpetre, smart saltpetre feed liquid is sent in smart potassium thickener and carried out thickening, in essence potassium thickener, feed liquid send smart potassium whizzer to carry out separating and dehydrating, essence potassium whizzer adopts two-stage material-pushing centrifuge, in sepn process, to smart potassium whizzer, pass into pure water detergent saltpetre product, the washing water yield is the 15-30% of smart saltpetre amount, separated smart saltpetre and the smart potassium mother liquor of obtaining, and washing water when smart potassium mother liquor returns to (2) middle conduct washing Temperature are used.
(5) in separating obtained smart saltpetre product, add appropriate salt of wormwood, salt of wormwood add-on is definite according to the ammonium ion content containing in smart saltpetre product, and then send drying machine dry, is industrial potassium nitrate product after saltpetre product drying.The salt of wormwood adding reacts with ammonium nitrate in saltpetre product and generates saltpetre, and emits CO
2with NH
3thereby, improve product purity.Industrial potassium nitrate is containing KNO
3>=99.4%, Cl≤0.01%, moisture content≤0.1%.
(6) send preheater to be preheating to 80-100 ℃ in separating obtained thick potassium mother liquor in (2), the thick potassium mother liquor part after preheating is gone in (7) for washing ammonium chloride product, and another part send vapo(u)rization system to carry out evaporation concentration to 37-43Be.
(7) concentrated solution is sent in ammonium chloride crystallisation by cooling system and adopt air cooling crystallization technique to carry out crystallisation by cooling, air cooling crystallization technique is mainly by cooling crystallization tower, gas blower, recycle pump forms, it is by the solution in cooling crystallization tower base channel, by recycle pump, pump to the jet apparatus arranging in tower, solution is sprayed from the bottom up, solution is upwards ejected into after certain altitude, freely be scattered again, while gas blower blasts air upwards flows air at the bottom of tower, in the upper and lower process of solution, solution and freezing air are directly mixed, the solution crystallization that is cooled, until temperature is 55-70 ℃, the ammonia chloride crystal feed liquid of separating out is sent into and in ammonium chloride thickener, is carried out thickening, the ammonium chloride feed liquid of thickening is sent the centrifuge dehydration of ammonium chloride whizzer, ammonium chloride whizzer adopts two-stage material-pushing centrifuge, in sepn process, to passing into the thick potassium mother liquor after preheating in (6) in ammonium chloride whizzer, wash, wash away the saltpetre of carrying secretly in ammonium chloride product, passing into thick potassium mother liquor amount of liquor is the 15-30% of ammonium chloride product amount, after separation, obtain ammonium chloride product and ammonium mother liquor.Ammonium chloride product is containing N >=24.0%, K≤0.80%, moisture content≤3.0%.
(8) Repone K, ammonium nitrate and water are mixed by a certain percentage and add in batching dissolving tank, pass into steam direct heating, stir, Repone K and ammonium nitrate are dissolved, and being mixed with temperature and being 70-100 ℃, ammonium nitrate is (1.35-1.8) with Repone K mol ratio: the mixed solution that 1, Baume concentration is 35-44Be.
Press said sequence cyclical operation later.
Claims (3)
1. ammonium nitrate and Repone K replacement(metathesis)reaction are produced a production technique for saltpetre and ammonium chloride, and its technical characterictic is:
(1) the ammonium mother liquor returning in Repone K, ammonium nitrate, water and (7) is mixed by a certain percentage and add in batching dissolving tank, pass into steam direct heating, stir, Repone K and ammonium nitrate are dissolved completely, control solution temperature is 70-100 ℃, in solution, ammonium nitrate and Repone K mol ratio are (1.35-1.8): 1, and solution Baume concentration is 35-44Be;
(2) solution of preparation send strainer to filter after removal impurity, it is 10-30 ℃ that filtrate send thick potassium crystallisation by cooling system to adopt air cooling crystallization to temperature, crystallization Temperature, Temperature feed liquid is sent in thick potassium thickener and carried out thickening, Temperature feed liquid after thickening send thick potassium whizzer to carry out separating and dehydrating, in sepn process, to passing into the smart potassium mother liquor returning in (4) in thick potassium whizzer, Temperature is washed, controlling chloride ion content in the rear Temperature product of washing is below 1.5%, obtains thick potassium mother liquor (containing washings) and Temperature after separation;
(3) separating obtained Temperature is added to saltpetre dissolving tank, add pure water and directly pass into steam heating, Temperature is fully dissolved, controlling potassium nitrate solution temperature is 90-115 ℃, and Baume concentration is 44-52 ° of Be;
(4) potassium nitrate solution in saltpetre dissolving tank is sent in smart potassium crystallisation by cooling system and adopts air cooling crystallization to 20-30 ℃, crystallization essence saltpetre, smart saltpetre feed liquid is sent in smart potassium thickener and carried out thickening, smart saltpetre feed liquid after thickening send smart potassium whizzer to carry out separating and dehydrating, in sepn process, in smart potassium whizzer, pass into pure water detergent saltpetre product, the washing water yield is the 15-30% of smart saltpetre amount, after separation, obtain smart potassium mother liquor (containing washing water) and smart saltpetre, smart potassium mother liquor returns in (2) for washing Temperature;
(5) according to ammonium ion content in separating obtained smart saltpetre product, in separating obtained smart saltpetre product, add appropriate salt of wormwood, and then sending drying machine dry, the salt of wormwood adding reacts with ammonium nitrate in saltpetre product and generates saltpetre, and emits CO
2with NH
3, after saltpetre product drying, be industrial potassium nitrate product;
(6) send preheater to be preheating to 80-100 ℃ in separating obtained thick potassium mother liquor in (2), the few part of thick potassium mother liquor after preheating is for (7) washing ammonium chloride product, and it is 37-43Be to Baume concentration that the thick potassium mother liquor of rest part send vapo(u)rization system to carry out evaporation concentration;
(7) concentrated solution is sent in ammonium chloride crystallisation by cooling system and adopt air cooling crystallization to 55-70 ℃, crystallization ammonium chloride, ammonium chloride feed liquid is sent and in ammonium chloride thickener, carried out thickening, ammonium chloride feed liquid after thickening is sent the centrifuge dehydration of ammonium chloride whizzer, in sepn process, to the thick potassium mother liquor passing into after preheating in ammonium chloride whizzer, wash, passing into thick potassium mother liquor amount of liquor is the 15-30% of ammonium chloride product amount, after separation ammonium chloride product and ammonium mother liquor.
2. Ju metathesis air cooling crystallization claimed in claim 1 method is produced saltpetre technique, its technical characterictic is: Temperature crystallisation by cooling and smart saltpetre crystallisation by cooling and ammonium chloride crystallisation by cooling all adopt air cooling crystallization technique, air cooling crystallization technique be using air as heat-eliminating medium and solution directly mixed contact carry out transmission of heat by convection and diffusion heat transfer, the solution post crystallization crystallize out that is cooled, air cooling crystallization technique is mainly by cooling crystallization tower, gas blower, recycle pump forms, it is by the solution in cooling crystallization tower base channel, by recycle pump, pump to the jet apparatus arranging in tower, solution is sprayed from the bottom up, solution is upwards ejected into after certain altitude, freely be scattered again and fall into tower bottom groove, the air that gas blower blasts simultaneously upwards flows at the bottom of tower, in the upper and lower process of solution, solution and freezing air be mixed heat exchange directly, the solution crystallization crystalline product that is cooled.
3. Ju metathesis air cooling crystallization claimed in claim 1 method is produced saltpetre technique, its technical characterictic is: Temperature centrifugation adopts two-stage material-pushing centrifuge, the centrifugation of essence saltpetre adopts two-stage material-pushing centrifuge, ammonium chloride centrifugation adopts two-stage material-pushing centrifuge, two-stage material-pushing centrifuge has that separating power is large, good separating effect, and can realize continuous separate from, continuous washing operation.
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Cited By (7)
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| CN104261438A (en) * | 2014-10-10 | 2015-01-07 | 山东诺贝丰化学有限公司 | Continuous system and method for producing potassium nitrate through double decomposition method |
| CN104787782A (en) * | 2015-04-16 | 2015-07-22 | 岳阳市钾盐科学研究所 | Process for preparing industrial potassium nitrate and calcium sulfate |
| CN105084396A (en) * | 2015-07-30 | 2015-11-25 | 湘潭大学 | Method for strengtheningly separating byproduct ammonium chloride from potassium nitrate produced through complex decomposition method |
| CN105110355A (en) * | 2015-08-25 | 2015-12-02 | 浏阳市金和化工有限公司 | Method for processing optical glass level high-purity potassium nitrate |
| CN105060317B (en) * | 2015-07-30 | 2016-08-24 | 湖南丹化农资有限公司 | A kind of method being produced high-quality potassium nitrate with ammonium nitrate double decomposition circulation process by potassium chloride |
| CN106698483A (en) * | 2017-01-19 | 2017-05-24 | 青海盐湖工业股份有限公司 | Method for producing molten salt-grade sodium nitrate |
| CN108059175A (en) * | 2018-01-19 | 2018-05-22 | 江西金利达钾业有限责任公司 | A kind of potassium nitrate purification system |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261438A (en) * | 2014-10-10 | 2015-01-07 | 山东诺贝丰化学有限公司 | Continuous system and method for producing potassium nitrate through double decomposition method |
| CN104787782A (en) * | 2015-04-16 | 2015-07-22 | 岳阳市钾盐科学研究所 | Process for preparing industrial potassium nitrate and calcium sulfate |
| CN104787782B (en) * | 2015-04-16 | 2016-09-28 | 岳阳市钾盐科学研究所 | Produce industrial potassium nitrate and calcium sulfate technique |
| CN105084396A (en) * | 2015-07-30 | 2015-11-25 | 湘潭大学 | Method for strengtheningly separating byproduct ammonium chloride from potassium nitrate produced through complex decomposition method |
| CN105060317B (en) * | 2015-07-30 | 2016-08-24 | 湖南丹化农资有限公司 | A kind of method being produced high-quality potassium nitrate with ammonium nitrate double decomposition circulation process by potassium chloride |
| CN105110355A (en) * | 2015-08-25 | 2015-12-02 | 浏阳市金和化工有限公司 | Method for processing optical glass level high-purity potassium nitrate |
| CN106698483A (en) * | 2017-01-19 | 2017-05-24 | 青海盐湖工业股份有限公司 | Method for producing molten salt-grade sodium nitrate |
| CN108059175A (en) * | 2018-01-19 | 2018-05-22 | 江西金利达钾业有限责任公司 | A kind of potassium nitrate purification system |
| CN108059175B (en) * | 2018-01-19 | 2023-08-11 | 江西金利达钾业有限责任公司 | Potassium nitrate purification system |
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