CN220834197U - Crystallization separation device for producing potassium nitrate by ammonium nitrate double decomposition method - Google Patents
Crystallization separation device for producing potassium nitrate by ammonium nitrate double decomposition method Download PDFInfo
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 238000002425 crystallisation Methods 0.000 title claims abstract description 97
- 230000008025 crystallization Effects 0.000 title claims abstract description 97
- 235000010333 potassium nitrate Nutrition 0.000 title claims abstract description 68
- 239000004323 potassium nitrate Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 39
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 28
- 238000000926 separation method Methods 0.000 title claims abstract description 25
- 208000028659 discharge Diseases 0.000 claims abstract description 69
- 238000005188 flotation Methods 0.000 claims abstract description 30
- 239000002562 thickening agent Substances 0.000 claims abstract description 27
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 54
- 239000007788 liquid Substances 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 30
- 235000019270 ammonium chloride Nutrition 0.000 claims description 27
- 239000012452 mother liquor Substances 0.000 claims description 25
- 238000010992 reflux Methods 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 25
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 23
- 239000013078 crystal Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 13
- 238000001816 cooling Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 238000010924 continuous production Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 230000005484 gravity Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000001103 potassium chloride Substances 0.000 description 5
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- -1 ammonium ions Chemical class 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 229910001950 potassium oxide Inorganic materials 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to the field of chemical crystallization separation engineering, and provides a crystallization separation device for producing potassium nitrate by an ammonium nitrate double-decomposition method, which comprises a crystallization system, wherein the crystallization system comprises a primary crystallizer, a primary discharge pump, a secondary crystallizer, a secondary discharge pump, a tertiary crystallizer and a tertiary discharge pump, the primary crystallizer, the primary discharge pump, the secondary crystallizer, the secondary discharge pump, the tertiary crystallizer and the tertiary discharge pump are sequentially connected in series through pipelines, and the tertiary discharge pump is connected with a flotation thickener. The patent solves the problems of low crystallization efficiency, high energy consumption, lower purity of potassium nitrate and the like of the potassium nitrate production device at the present stage by designing three crystallizers and adjusting the production process.
Description
Technical Field
The utility model relates to the field of chemical crystallization separation engineering, in particular to a crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method.
Background
The main potassium nitrate production processes in China are an ammonium nitrate double decomposition process and a magnesium nitrate double decomposition process, wherein the two processes account for more than 95% of the total national yield, the potassium nitrate produced by the ammonium nitrate double decomposition production process accounts for more than 50% of the total national yield, and in recent 10 years, the ammonium nitrate double decomposition production process has larger evaporation capacity under the prior art condition, the process is more complex than the magnesium nitrate double decomposition process route, mainly the ammonium nitrate double decomposition process has smaller solubility at low temperature in the cooling crystallization process of the ammonium chloride during primary crystallization, a large amount of ammonium chloride is crystallized and separated out simultaneously, a large amount of mixed crystals are produced, and great difficulty is brought to separation and purification of the subsequent procedures.
Therefore, the crystallization separation device for producing the potassium nitrate by the ammonium nitrate double decomposition method is provided, the content of the potassium nitrate during primary crystallization separation is improved, and reliable guarantee is provided for subsequent high-quality potassium nitrate.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the utility model provides a crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method, which solves the technical problems of low crystallization efficiency, high energy consumption and lower purity of potassium nitrate of the device for producing potassium nitrate by the ammonium nitrate double decomposition method at the present stage.
Technical proposal
In order to achieve the above purpose, the utility model is realized by the following technical scheme:
The crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method comprises a crystallization system, wherein the crystallization system comprises a primary crystallizer, a primary discharge pump, a secondary crystallizer, a secondary discharge pump, a tertiary crystallizer and a tertiary discharge pump, the primary crystallizer, the primary discharge pump, the secondary crystallizer, the secondary discharge pump, the tertiary crystallizer and the tertiary discharge pump are sequentially connected in series through pipelines, and the tertiary discharge pump is connected with a flotation thickener;
The upper portion of flotation thickener connects the filter vat, the lower part of flotation thickener is connected and is promoted the hank cage, promote the filter vat in the upper portion of hank cage, promote the screw feeder in the lower part of hank cage connection, screw feeder connects centrifuge, mother liquor groove is connected on filter vat upper portion, makes ammonium chloride mother liquor flow to the mother liquor groove in collect.
In a further embodiment, the primary crystallizer is a DBT crystallizer, the secondary crystallizer and the tertiary crystallizer are vacuum flash crystallization crystallizers, the secondary crystallizer and the tertiary crystallizer comprise crystallization hoppers, the crystallization hoppers are funnel-shaped, the crystallization hoppers are clear liquid areas, crystallization areas and supersaturation areas from top to bottom in sequence, the clear liquid areas are provided with vertical circulating pumps, the vertical circulating pumps are connected with upper circulating pipes, the upper circulating pipes are connected with a flash chamber, the lower ends of the flash chamber are connected with lower circulating pipes, and the lower circulating pipes extend into the bottoms of the crystallization hoppers and are not connected with the crystallization hoppers.
In a further embodiment, the upper parts of the primary crystallizer, the secondary crystallizer and the tertiary crystallizer are respectively connected with a condenser, the condensers are connected with a vacuum buffer tank, the upper part of the vacuum buffer tank is connected with a vacuum pump, and the lower end of the vacuum buffer tank is connected with a condensate tank.
In a further embodiment, the primary crystallizer is provided with four discharge ports and a clear liquid overflow port, the clear liquid overflow port is arranged on the upper portion of the primary crystallizer, the discharge ports are arranged on the middle portion and the lower portion of the primary crystallizer, the secondary crystallizer is provided with two discharge ports and a clear liquid overflow port, the discharge ports are arranged in the crystallization area, the clear liquid overflow port is arranged in the flash chamber, the tertiary crystallizer is provided with three discharge ports, and the discharge ports are arranged in the crystallization area and the clear liquid area.
In a further embodiment, the lower part of the primary crystallizer is connected with a feed pump, the discharge port of the primary crystallizer is connected with a primary discharge pump, the primary discharge pump is connected to the middle part of a lower circulation pipeline of the secondary crystallizer after converging with a clear liquid overflow port of the primary crystallizer, the discharge port of the secondary crystallizer is connected with a secondary discharge pump, the secondary discharge pump is connected to the middle part of a lower circulation pipeline of the tertiary crystallizer after converging with a clear liquid overflow port of the secondary crystallizer, the discharge port of the tertiary crystallizer is connected with a tertiary discharge pump, and the tertiary discharge pump is connected with the upper part of the flotation thickener.
In a further embodiment, the upper portion of the filter tank is provided with a mother liquor overflow port and a feed port, the bottom of the filter tank is provided with a reflux port, the lower portion of the filter tank is provided with a filter screen, the filter screen is lower than the mother liquor overflow port and the feed port, the reflux port is connected with a reflux pump, and the reflux pump is connected with a flotation thickener.
In a further embodiment, the flotation thickener is provided with a stirring motor, the stirring motor is connected with a stirring shaft, an upper stirring blade and a lower stirring blade are arranged on the stirring shaft, and the upper stirring blade is larger than the lower stirring blade.
In a further embodiment, the primary crystallizer, the primary discharge pump, the secondary crystallizer, the secondary discharge pump, the tertiary crystallizer, the tertiary discharge pump, the condenser, the feed pump, the flotation thickener, the reflux pump, the mother liquor tank, the vacuum pump buffer tank, the vacuum pump and the condensate tank are connected through pipelines, and valves are arranged at the joints.
Advantageous effects
The utility model provides a crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method. Compared with the prior art, the method has the following beneficial effects:
1. the device can reduce raw material consumption and steam consumption.
2. By adopting the device, the high-efficiency separation of two crystals of potassium nitrate and ammonium chloride is realized, and the content of the primary crystallized potassium nitrate is improved.
3. Can run for a long period, has less maintenance and simple maintenance.
Drawings
In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the utility model, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a process flow diagram of the present embodiment.
Fig. 2 is a schematic structural diagram of the secondary crystallizer according to this embodiment.
Fig. 3 is a schematic structural diagram of the flotation thickener according to this example.
The reference numerals in the figures are:
1. A primary crystallizer; 2. a primary discharge pump; 3. a secondary crystallizer; 4. a secondary discharge pump; 5. a third-stage crystallizer; 6. a three-stage discharging pump; 7. a condenser; 8. a feed pump; 9. a flotation thickener; 10. a reflux pump; 11. a mother liquor tank; 12. a vacuum buffer tank; 13. a vacuum pump; 14. a condensate tank; 15. lifting the stranding cage; 16. a screw feeder; 17. a centrifuge; 18. a crystallization hopper; 19. a clear liquid zone; 20. a crystallization zone; 21. a supersaturation zone; 22. a vertical circulation pump; 23. an upper circulation pipe; 24. a lower circulation pipe; 25. a discharge port; 26. a clear liquid overflow port; 27. a flash chamber; 28. a filter screen; 29. a filter tank; 30. a mother liquor overflow port; 31. a feed inlet; 32. a stirring motor; 33. a stirring shaft; 34. an upper stirring blade; 35. lower stirring blades.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present utility model more clear, the technical solutions in the embodiments of the present utility model are clearly and completely described, and it is obvious that the described embodiments are some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The embodiment of the application solves the technical problems of low crystallization efficiency, high energy consumption and lower potassium nitrate purity of the existing ammonium nitrate double-decomposition production device by providing the crystallization separation device for producing potassium nitrate by the ammonium nitrate double-decomposition method, and realizes the improvement of the content of primary crystallization potassium nitrate and the reduction of raw material consumption and steam consumption during use.
Comparative examples
Taking 2 ammonium nitrate double decomposition methods adopted at present in China as examples for effect comparison:
In the first crystallization, the current production enterprises use normal pressure cooling kettles and coil pipe circulating water cooling in a more mode, the specific gravity of the material before cooling crystallization is 1.37-1.38 g/m1, 5-5.2 m3 of reaction solution is needed for producing 1 ton of potassium nitrate, the end temperature of the material cooling is 32-35 ℃, the slurry volume of the crystallization mixture before separating crystals after crystallization is 4.9-5 m, the separation of ammonium chloride is carried out by a floatation method after crystallization, the mother liquor is separated by centrifugal dehydration, the ammonium chloride and the potassium nitrate form a mixed crystal primary product, the ammonium chloride content before washing is 7-10%, the potassium nitrate content in crystals after filtering overflow mother liquor is 40-45%, the crystals in the mother liquor are all dissolved during evaporation, the potassium nitrate primary product is washed by primary washing liquid (the mixture of the soaking liquid and the mother liquor and then evaporation), the primary recrystallization mother liquor is soaked (the dissolution of the potassium chloride after the reaction is removed), the primary washing is 2-3 times (wherein the lower layer material is washed once again), the primary potassium nitrate is produced, the ammonium chloride content after the primary potassium nitrate is washed by water is 0.900%, and the primary crystal potassium chloride content after the previous 1 ton is 0.0.0.0-0.4% is the primary standard product after the primary crystal is dehydrated, and the primary crystal is purified, the ammonium chloride content is 0.0.0.6% after the primary crystal is 0.6% is purified. The main consumption and production conditions are shown in Table I and Table II.
Table I, conventional batch production equipment industry product potassium nitrate production consumption table (per ton of finished product KNO 3)
Sequence number | Name of the name | Specification of specification | Unit (B) | Guarantee value |
1 | Potassium chloride (100% meter) | ≥95% | t | 0.812 |
2 | Ammonium nitrate (100% meter) | 92% | t | 0.855 |
3 | Low pressure steam | 0.8MPaG 158.4℃ | t | 2.70 |
4 | Electric power | 380V | kwh | 140 |
5 | Production personnel for every class | Human body | 27 |
Table two. Conventional batch production plant industry potassium nitrate production status table (in terms of KNO 3 per ton of finished product):
Sequence number | Name of the name | Specification of specification | Unit (B) | Guarantee value |
1 | Volume after primary crystallization | Primary crystallization of mixed material | m3 | 0.812 |
2 | Volume after secondary crystallization | Comprising primary crystallization and recrystallization | m3 | 1.5 |
3 | Evaporation capacity | t | 1.80 | |
4 | Chlorine ion amount before redissolution | % | 0.65 | |
5 | Ammonium ion amount before redissolution | % | 0.46 | |
6 | Potassium oxide content in ammonium chloride | % | 3.5 | |
7 | Product quality grade | National standard of industrial potassium nitrate | Primary product |
In the second example, the ammonium nitrate double decomposition method is used for producing agricultural first-grade potassium nitrate (the national standard potassium nitrate content is more than 44.5%, and the chloride ion is less than 1.2%), the annual output is 6 ten thousand tons of continuous production devices, the production enterprises currently use a continuous 3-grade vacuum flash crystallizer for the first crystallization, the material cooling crystallization end temperature is 23-25 ℃ (the third stage also adopts 5-7 ℃ frozen salt water as circulating cooling water), the specific gravity of the material before cooling crystallization is 1.32-1.34 g/ml, the reaction solution is required for producing 1 ton of potassium nitrate, the volume of the crystallization mixture slurry before separating crystals after crystallization is 4.7-4.8 m (the flash water yield of cooling crystallization water is 0.7-0.8 m), the ammonium chloride content in the primary potassium nitrate after centrifuging and separating mother liquor is 10-12%, the potassium nitrate content in the product is 44.8-45.1%, the chloride content in the product is 0.7-1.7 m after continuous 2-grade countercurrent washing and centrifugal dehydration of each ton of the product, the chloride content in the product is 0.8-0.7-0.0.7 m, and the consumption of the production conditions are shown in the three and four production states.
Production consumption meter of agricultural potassium nitrate production by continuous production device (calculated by KNO 3 per ton of finished product)
Sequence number | Name of the name | Specification of specification | Unit (B) | Guarantee value |
1 | Potassium chloride (100% meter) | ≥95% | t | 0.795 |
2 | Ammonium nitrate (100% meter) | 92% | t | 0.845 |
3 | Low pressure steam | 0.8MPaG 158.4℃ | t | 1.90 |
4 | Electric power | 380V | kwh | 160 |
5 | Production personnel for every class | Yield 6 ten thousand tons/year | Human body | 13 |
Table IV. Table of conditions of production of potassium nitrate for continuous production plant industry (per ton of finished KNO 3):
Sequence number | Name of the name | Specification of specification | Unit (B) | Guarantee value |
1 | Volume after primary crystallization | Primary crystallization of mixed material | m3 | 4.8 |
2 | Total washing water content of 1 crystallization | Comprising primary crystallization and recrystallization | m3 | 0.85 |
3 | Evaporation capacity | t | 1.60 | |
4 | Chloride ion content in the product | % | 0.85 | |
5 | Ammonium ion content in the product | % | 0.61 | |
6 | Potassium oxide content in ammonium chloride | % | 2.1 | |
7 | Product quality grade | National standard of agricultural potassium nitrate | Primary product |
In the third embodiment, the technology continuously produces industrial high-grade potassium nitrate (the main content of potassium nitrate is more than 99.7%, chloride ions are less than 0.01%, ammonium ions are less than 0.015%), a continuous production device with 6 ten thousand tons is produced in one year, the cooling crystallization end point temperature of the material is 23-25 ℃ (the third stage adopts 7-10 ℃ frozen saline water as circulating cooling water), the specific gravity of the material before cooling crystallization is 1.38-1.385 g/ml, 4.6-4.7 m < 3 > is needed for producing 1 ton of potassium nitrate, the slurry volume of a crystallization mixture before separating crystals after crystallization is 3.9-4.1 m (the flash water yield of cooling crystallization water is 0.6-0.7 m), the content of ammonium chloride in the primary product of potassium nitrate is 2-3% after separating ammonium chloride crystals by continuous floatation, the primary product of potassium nitrate is subjected to continuous 2-stage countercurrent washing by 0.3-0.4t of water, the primary product of potassium nitrate is subjected to centrifugal dehydration, the main content of the primary product of potassium nitrate is 97.5-98%, the content of chloride ions is 0.28%, and the content of ammonium ions is 0.26%. The production consumption and the production state are shown in Table five and Table six.
Table five. Production consumption table of agricultural potassium nitrate produced by continuous production device (calculated by KNO 3 per ton of finished product):
Sequence number | Name of the name | Specification of specification | Unit (B) | Guarantee value |
1 | Potassium chloride (100% meter) | ≥95% | t | 0.795 |
2 | Ammonium nitrate (100% meter) | 92% | t | 0.840 |
3 | Low pressure steam | 0.8MPaG 158.4℃ | t | 2.10 |
4 | Electric power | 380V | kwh | 180 |
5 | Production personnel for every class | Yield 6 ten thousand tons/year | Human body | 15 |
Table six. Continuous production plant industry potassium nitrate production status table (calculated per ton of finished KNO 3):
The production effect difference of the above 3 ammonium nitrate decomposition methods for producing potassium nitrate is quite large due to the difference of the different production effects of the primary crystallization separation device, which is enough to show the scientificity and advancement of the device, and is a good device for producing potassium nitrate which is worth popularizing greatly.
The technical scheme in the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
The crystallization temperature is controlled to 55-65 ℃, the crystallization temperature is controlled to 30-45 ℃, the crystallization temperature is controlled to 20-25 ℃, the ammonium chloride and the potassium nitrate of the secondary crystallizer and the tertiary crystallizer are crystallized and separated out simultaneously, the newly fed materials enter the bottom of the crystallizer through the circulating pipe under the action of the circulating pump, a supersaturated area, a crystallization area and a clear liquid area are formed in the crystallization hopper along with the rising of the materials and the specific gravity difference of the materials, a vertical circulating pump is arranged at the upper part of the crystallization hopper, the crystallized clear liquid is conveyed to a flash chamber through the vertical circulating pump, high vacuum flash is cooled, the cooled liquid flows into the supersaturated area at the bottom of the crystallization hopper under the action of gravity, the potassium nitrate and the ammonium chloride grow up in the respective crystallization areas, the discharge pumps are connected through pipelines through discharge ports at different positions, the ammonium chloride content in the crystal is about 20%, the ammonium chloride and the potassium nitrate are separated through the discharge pumps, the ammonium chloride enters a mother liquid tank through gravity floatation, and the potassium nitrate is dehydrated through centrifugation, so that a potassium nitrate primary product with the purity of 94-95% is obtained. The content of ammonium chloride is only 2-3%. The potassium nitrate can reach 97-98% after washing.
In order to better understand the above technical solutions, the following detailed description will refer to the accompanying drawings and specific embodiments.
Referring to fig. 1-3, a crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method comprises a crystallization system, wherein the crystallization system comprises a primary crystallizer 1, a primary discharge pump 2, a secondary crystallizer 3, a secondary discharge pump 4, a tertiary crystallizer 5 and a tertiary discharge pump 6, wherein the primary crystallizer 1, the primary discharge pump 2, the secondary crystallizer 3, the secondary discharge pump 4, the tertiary crystallizer 5 and the tertiary discharge pump 6 are sequentially connected in series through pipelines, and the tertiary discharge pump 6 is connected with a flotation thickener 9;
The upper portion of flotation thickener 9 connects filter tank 29, and the lower part of flotation thickener 9 connects and promotes hank cage 15, promotes the filter tank 29 in the upper portion of hank cage 15, promotes the lower part of hank cage 15 and connects screw feeder 16, and screw feeder 16 connects centrifuge 17, and mother liquor groove 11 is connected to filter tank 29, makes ammonium chloride mother liquor flow to mother liquor groove 11 in the collection.
The primary crystallizer 1 is a DBT crystallizer, the secondary crystallizer 3 and the tertiary crystallizer 5 are vacuum flash-shot crystallizers, the secondary crystallizer 3 and the tertiary crystallizer 5 comprise a crystallization hopper 18, the crystallization hopper 18 is funnel-shaped, the crystallization hopper 18 is sequentially provided with a clear liquid area 19, a crystallization area 20 and a supersaturation area 21 from top to bottom, the clear liquid area 19 is provided with a vertical circulating pump 22, the vertical circulating pump 22 is connected with an upper circulating pipeline 23, the upper circulating pipeline 23 is connected with a flash chamber 27, the lower end of the flash chamber 27 is connected with a lower circulating pipeline 24, and the lower circulating pipeline 24 extends into the bottom of the crystallization hopper 18 and is not connected with the crystallization hopper 18, and referring to fig. 1.
The secondary crystallizer 3 and the tertiary crystallizer 5 can be selected from the aus Lu Jiejing device, referring to fig. 2.
The upper parts of the primary crystallizer 1, the secondary crystallizer 3 and the tertiary crystallizer 5 are respectively connected with a condenser 7, the condenser 7 is connected with a vacuum buffer tank 12, the upper part of the vacuum buffer tank 12 is connected with a vacuum pump 13, and the lower end of the vacuum buffer tank 12 is connected with a condensate tank 14.
The matching selection requirements of the vacuum pump 13 and the condenser 7 are that the temperature difference between the discharging temperature of the crystallizer and the circulating cooling water is 13-15 ℃ (the discharging temperature of the secondary crystallizer 3 is about 15 ℃ in summer and winter with larger influence of the local season temperature), the three-stage crystallizer 5 adopts 5-7 ℃ chilled water to circulate and cool down, and the discharging temperature of the three-stage crystallizer 5 is ensured to be maintained at 24-25 ℃ all the year round.
The primary crystallizer 1 is provided with four discharge holes 25 and a clear liquid overflow hole 26, the clear liquid overflow hole 26 is arranged on the upper part of the primary crystallizer 1, the discharge holes 25 are arranged on the middle part and the lower part of the primary crystallizer 1, the secondary crystallizer 3 is provided with two discharge holes 25 and a clear liquid overflow hole 26, the discharge holes 25 are arranged in the crystallization area 20, the clear liquid overflow hole 26 is arranged in the flash chamber 27, the tertiary crystallizer 5 is provided with three discharge holes 25, and the discharge holes 25 are arranged in the crystallization area 20 and the clear liquid area 19.
The lower part of the primary crystallizer 1 is connected with a feed pump 8, a discharge port 25 of the primary crystallizer 1 is connected with a primary discharge pump 2, the primary discharge pump 2 is connected with a clear liquid overflow port 26 of the primary crystallizer 1 and then connected to the middle part of a lower circulation pipeline 24 of the secondary crystallizer 3, a discharge port 25 of the secondary crystallizer 3 is connected with a secondary discharge pump 4, the secondary discharge pump 4 is connected with the middle part of a lower circulation pipeline 24 of the tertiary crystallizer 5 after being connected with a clear liquid overflow port 26 of the secondary crystallizer 3, a discharge port 25 of the tertiary crystallizer 5 is connected with a tertiary discharge pump 6, and the tertiary discharge pump 6 is connected with the upper part of the flotation thickener 9.
The discharge pump selects proper circulation volume, so that a material forms a relatively obvious supersaturation zone 21, a crystallization zone 20 and a clear liquid zone 19 from bottom to top in the crystallization hopper 18, mixed crystals of potassium nitrate and ammonium chloride are avoided, the discharge valves of the secondary crystallizer 3 are reasonably regulated, and the distribution density of crystals is reasonably controlled by reasonably distributing two discharge valves and overflow proportion of supernatant liquid so as to control the granularity of the potassium nitrate and ammonium chloride crystals.
The upper portion of filter tank 29 sets up mother liquor overflow port 30 and feed inlet 31, and the bottom of filter tank 29 sets up the reflux mouth, and the lower part of filter tank 29 sets up filter screen 28, and filter screen 28 is less than mother liquor overflow port 30 and feed inlet 31, and reflux pump 10 is connected to the reflux inlet, and reflux pump 10 connects flotation thickener 9.
The filter tank 29 serves to separate a part of the supernatant liquid free of ammonium chloride crystals and pump it back into the flotation thickener 9, improving the flotation effect.
The flotation thickener 9 is provided with a stirring motor 32, the stirring motor 32 is connected with a stirring shaft 33, an upper stirring blade 34 and a lower stirring blade 35 are arranged on the stirring shaft 33, and the upper stirring blade 34 is larger than the lower stirring blade 35, and refer to fig. 3.
The potassium nitrate settled to the bottom of the flotation thickener 9 is ensured to be evenly, continuously and stably discharged, the stirring motor 32 and the reflux pump 10 are both provided with variable frequency, and the flotation thickener 9 is adjusted to the optimal effect by adjusting the stirring motor 32 and the reflux pump 10 (the amount of the potassium nitrate at the overflow port is very small, and the ammonium chloride crystal is almost completely discharged out of the flotation filter tank 29 together with the mother liquor through the overflow port).
In summary, compared with the prior art, the method has the following beneficial effects:
1. the device can reduce raw material consumption and steam consumption.
2. By adopting the device, the high-efficiency separation of two crystals of potassium nitrate and ammonium chloride is realized, and the content of the primary crystallized potassium nitrate is improved.
3. The device can run for a long period, has less maintenance and is simple to maintain.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present utility model, and are not limiting; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present utility model.
Claims (7)
1. The crystallization separation device for producing potassium nitrate by an ammonium nitrate double-decomposition method is characterized by comprising a crystallization system, wherein the crystallization system comprises a primary crystallizer (1), a primary discharge pump (2), a secondary crystallizer (3), a secondary discharge pump (4), a tertiary crystallizer (5) and a tertiary discharge pump (6), the primary crystallizer (1), the primary discharge pump (2), the secondary crystallizer (3), the secondary discharge pump (4), the tertiary crystallizer (5) and the tertiary discharge pump (6) are sequentially connected in series through pipelines, and the tertiary discharge pump (6) is connected with a flotation thickener (9);
The utility model discloses a flotation thickener, including flotation thickener, filter tank (29) are connected on the upper portion of flotation thickener (9), the lower part of flotation thickener (9) is connected and is promoted hank cage (15), the filter tank (29) are connected on the upper portion of promotion hank cage (15), screw feeder (16) are connected on the lower part of promotion hank cage (15), centrifuge (17) are connected to screw feeder (16), mother liquor groove (11) are connected on filter tank (29) upper portion, make flotation play ammonium chloride mother liquor flow to mother liquor groove (11) in collect.
2. The crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method according to claim 1, wherein the primary crystallizer (1) is a DBT crystallizer, the secondary crystallizer (3) and the tertiary crystallizer (5) are vacuum flash crystallization crystallizers, the secondary crystallizer (3) and the tertiary crystallizer (5) comprise crystallization hoppers (18), the crystallization hoppers (18) are funnel-shaped, the crystallization hoppers (18) are a clear liquid area (19), a crystallization area (20) and a supersaturation area (21) from top to bottom in sequence, the clear liquid area (19) is provided with a vertical circulating pump (22), the vertical circulating pump (22) is connected with an upper circulating pipeline (23), the upper circulating pipeline (23) is connected with a flash chamber (27), the lower end of the flash chamber (27) is connected with a lower circulating pipeline (24), and the lower circulating pipeline (24) stretches into the bottom of the crystallization hoppers (18) and is not connected with the crystallization hoppers (18).
3. The crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method according to claim 1, wherein the upper parts of the primary crystallizer (1), the secondary crystallizer (3) and the tertiary crystallizer (5) are respectively connected with a condenser (7), the condenser (7) is connected with a vacuum buffer tank (12), the upper part of the vacuum buffer tank (12) is connected with a vacuum pump (13), and the lower end of the vacuum buffer tank (12) is connected with a condensate tank (14).
4. The crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method according to claim 2, wherein the primary crystallizer (1) is provided with four discharge ports (25) and a clear liquid overflow port (26), the clear liquid overflow port (26) is arranged at the upper part of the primary crystallizer (1), the discharge ports (25) are arranged at the middle part and the lower part of the primary crystallizer (1), the secondary crystallizer (3) is provided with two discharge ports (25) and a clear liquid overflow port (26), the discharge ports (25) are arranged in a crystallization area (20), the clear liquid overflow port (26) is arranged in a flash chamber (27), the tertiary crystallizer (5) is provided with three discharge ports (25), and the discharge ports (25) are arranged in the crystallization area (20) and the clear liquid area (19).
5. The crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method according to claim 4, wherein the lower part of the primary crystallizer (1) is connected with a feed pump (8), a discharge port (25) of the primary crystallizer (1) is connected with a primary discharge pump (2), the primary discharge pump (2) is connected with the middle part of a lower circulation pipeline (24) of the secondary crystallizer (3) after being converged with a clear liquid overflow port (26) of the primary crystallizer (1), the discharge port (25) of the secondary crystallizer (3) is connected with a secondary discharge pump (4), the secondary discharge pump (4) is connected with the middle part of a lower circulation pipeline (24) of the secondary crystallizer (3) after being converged with a clear liquid overflow port (26) of the secondary crystallizer (3), the discharge port (25) of the tertiary crystallizer (5) is connected with a tertiary discharge pump (6), and the tertiary discharge pump (6) is connected with the upper part of a flotation thickener (9).
6. The crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method according to claim 1, wherein a mother liquor overflow port (30) and a feed port (31) are arranged at the upper part of the filter tank (29), a reflux port is arranged at the bottom of the filter tank (29), a filter screen (28) is arranged at the lower part of the filter tank (29), the filter screen (28) is lower than the mother liquor overflow port (30) and the feed port (31), the reflux port is connected with a reflux pump (10), and the reflux pump (10) is connected with a flotation thickener (9).
7. A crystallization separation device for producing potassium nitrate by an ammonium nitrate double decomposition method according to claim 1, wherein a stirring motor (32) is arranged on the flotation thickener (9), the stirring motor (32) is connected with a stirring shaft (33), an upper stirring blade (34) and a lower stirring blade (35) are arranged on the stirring shaft (33), and the upper stirring blade (34) is larger than the lower stirring blade (35).
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