CN110229024B - Industrial decomposing crystallizer for potassium salt - Google Patents
Industrial decomposing crystallizer for potassium salt Download PDFInfo
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- CN110229024B CN110229024B CN201910466770.8A CN201910466770A CN110229024B CN 110229024 B CN110229024 B CN 110229024B CN 201910466770 A CN201910466770 A CN 201910466770A CN 110229024 B CN110229024 B CN 110229024B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/10—Preparation of sulfates by double decomposition with sulfates of magnesium, calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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Abstract
The utility model provides an industrial decomposition crystallizer of sylvite, includes crystallizer body, outer draft tube, interior draft tube, feed baffle, scattered glassware, main agitating unit, cloth liquid device, mother liquor fluid infusion pipe, water conservancy diversion awl and row's material agitating unit, outer draft tube, interior draft tube, feed baffle and crystallizer body fixed connection, the (mixing) shaft and the paddle of main agitating unit are arranged in the draft tube, scattered glassware links to each other with interior draft tube or direct mount on the (mixing) shaft, and the crystallizer is originally internal to be located to the water conservancy diversion awl, is located outer draft tube below, and the crystallizer is originally internal to be located to the cloth liquid device, and mother liquor fluid infusion pipe is connected with the cloth liquid device, arranges the bottom in the crystallizer body that material agitating unit locates, and crystallizer body upper end is equipped with the mother liquor overflow mouth, and crystallizer body bottom is equipped with the bin outlet. The invention can improve the upper limit of the feeding granularity of the raw materials and the processing capacity of unit volume in the dissolving area, reduce the entrainment rate of the raw materials in the crystallized product and improve the granularity of the product.
Description
Technical Field
The invention relates to a decomposing crystallizer for potassium salt industry.
Background
China is a big agricultural country, and the demand on potassium fertilizer is large, but the industrial yield of potassium salt in China is far from meeting the agricultural demand, nearly 50% of potassium salt still needs to be imported from foreign countries, and the dependence on foreign countries is extremely high.
The decomposing crystallizer commonly used in the potassium salt industry is a variant form of DTB type crystallizer developed in the potassium salt industry, and is mainly used for preparing potassium chloride by dissolving and crystallizing low-sodium carnallite and preparing potassium sulfate by double decomposition of double salt containing magnesium sulfate and potassium chloride. In the existing decomposing crystallizer in the sylvite industry, raw materials, dissolved ore mother liquor and fresh water are added into an inner cylinder according to a set proportion and mixed with sucked circulating ore pulp in a dissolving region to be dissolved, then partial crystallization is completed in a crystallization region between the inner cylinder and an outer cylinder, the obtained mother liquor and partial fine crystals directly enter a crystallizer body, the produced mother liquor and partial fine crystals enter a mother liquor clarification region, and crystallized products enter a product discharge region. However, in actual production operation, part of the raw materials in the crystallized product are not fully dissolved and enter the slurry of the crystallizer body so as to be included in the product flow, and the entrainment of the raw materials influences the final quality of the product. When the potassium chloride is prepared by decomposing and crystallizing low-sodium carnallite, the entrainment rate of raw material carnallite in the potassium chloride product is sometimes as high as 20%. The reasons for this phenomenon are manifold: 1) the mechanical main stirring device in the inner cylinder sucks enough circulating ore pulp and simultaneously finishes stirring and mixing actions, the upward flow at the central axis of the inner cylinder is relatively weak, and the raw material is directly fed from the upper part and has a certain downward speed, so that part of the raw material cannot move according to the set flow direction of a decomposition area, a crystallization area and a product area, but directly flows out from the lower part of the inner cylinder and directly enters a product discharge area; 2) due to phase composition change or quality fluctuation of the fed raw materials, but the process ratio cannot be adjusted in time, partial raw materials are not fully dissolved in a dissolving region, so that the material flow is conformed to enter the product from a decomposition region, a crystallization region and a product region; 3) part of the large particles in the feed material was not sufficiently dissolved due to insufficient dissolution time.
CN103073030B discloses a crystallizer for hydrolyzing carnallite, but does not solve the relative separation problem of the crystallization raw material and the crystallization product in the crystallization production, nor the circulating crystallization problem of the large-particle raw material. CN105597363B discloses an industrial mechanical crystallizer for potassium salt, which is characterized in that a bowl-shaped baffle is arranged at the lower part of an inner cylinder to reduce the entrainment of raw materials in the product, but the baffle structure is easy to form a "dead zone" for material accumulation at the lower side of a stirring shaft, occupies the internal space of the crystallizer to form an inefficient area, and once the "dead zone" is formed, the bowl-shaped baffle can no longer achieve the purpose of prolonging the residence time of undissolved raw materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing the decomposing crystallizer for the potassium salt industry, which has strong adaptability to raw materials, reduces the fine crystal quantity in the product and reduces the entrainment rate of the raw materials in the crystallized product.
The invention overcomes the defect that partial raw materials are not fully dissolved and enter a crystallized product due to the material flow short-circuit phenomenon in the conversion process of the raw materials, circulating ore pulp and the product in the existing equipment by optimizing the flow field distribution in the existing equipment and improving the crystallization growth environment of particles in a crystallizer.
The technical scheme adopted by the invention for solving the technical problems is as follows: a sylvite industrial decomposing crystallizer comprises a crystallizer body, an outer draft tube, an inner draft tube, a feeding baffle, a material scattering device, a main stirring device, a liquid distribution device, a mother liquid replenishing tube, a draft cone and a discharging stirring device, wherein the outer draft tube, the inner draft tube and the feeding baffle are fixedly connected with the crystallizer body through a support, the main stirring device is fixed on the crystallizer body through the support, a stirring shaft and blades of the main stirring device are positioned in the inner draft tube, the material scattering device is connected with the inner draft tube through the support or directly installed on the stirring shaft, the draft cone is arranged in the crystallizer body and is positioned below the outer draft tube and is fixedly connected with the crystallizer body through the support, the liquid distribution device is arranged in the crystallizer body and is positioned under the inner draft tube and the outer draft tube, the mother liquid replenishing tube is connected with the liquid distribution device, the discharging stirring device is arranged at the inner bottom of the crystallizer body, the crystallizer body upper end is equipped with the mother liquor overflow mouth, crystallizer body bottom is equipped with the bin outlet.
Further, the material scattering device is positioned right above the blades of the main stirring device; the bulk cargo ware can be in one of conical, hemisphere, multiaspect toper, preferably conical, and the equivalent diameter of its maximum cross-section is 0.15 ~ 0.40 times of interior draft tube diameter.
Further, the liquid distribution device is positioned right below the main stirring device, and the distance from the top of the liquid distribution device to the bottom of the inner guide cylinder is 0.8-1.2 times of the diameter of the inner guide cylinder; the liquid distribution device comprises a bottom plate and a liquid distribution plate, the bottom plate is connected with a mother liquid supplementing pipe, the bottom plate is in one or combination of an inverted cone shape, a multi-surface cone shape and a horn shape, the bottom plate is preferably in an inverted cone shape, the included angle between a bus line and the horizontal direction is 30-60 degrees, water distribution holes are distributed in the liquid distribution plate, and the diameter of each water distribution hole is 0.20-3.0 mm.
Further, the guide cone is in an inverted cone shape, and the central axis of the guide cone is the same as that of the crystallizer body; the top of the diversion cone is 0.1-1.0 time of the diameter of the bottom of the outer diversion cylinder higher than the bottom of the outer diversion cylinder, the bottom of the diversion cone is 0-0.2 time of the diameter of the top of the liquid distribution device lower than the top of the liquid distribution device, and the included angle between the generatrix of the diversion cone and the horizontal direction is 52-90 degrees.
The invention has the beneficial effects that:
the material scattering device is arranged in the inner guide cylinder, so that feeding is mainly fed along the side wall of the inner guide cylinder, the amount of raw materials in a low-efficiency dissolving area with low ascending flow velocity and small mass transfer effect, which directly enter the central axis of the inner guide cylinder, is reduced, the dissolving reaction efficiency of the raw materials in the dissolving area is improved, and the possibility that the raw materials have higher vertical speed and directly impact the central axis of the inner guide cylinder with small ascending flow velocity and are difficult to rise along with stirring ascending flow to enter a crystallization area and directly enter a product area is reduced;
the liquid distribution device is arranged at the lower part of the inner guide cylinder, active upwelling is introduced into the main stirring device in the inner guide cylinder, the phenomenon that the upwelling is small due to the fact that the linear velocity close to the center of the impeller is small below the stirring shaft of the main stirring device at the lower side of the inner guide cylinder is weakened, and meanwhile, the effect of the main stirring device on producing the upwelling is partially shared, so that the effect of the main stirring device is focused on ensuring the stirring homogenization and the reaction dissolution of ore pulp in the inner guide cylinder;
by arranging the liquid distribution device and the flow guide cone, the flow field distribution in the crystallizer body is optimized, active upwelling is introduced into the crystallizer body to promote particle stratification, and a particle stratification area is additionally arranged. The crystallized product entering the slurry in the crystallizer body has a greater density and average particle size than the entrained feed material, while the feed material continues to dissolve less and the product grows further with increasing residence time. In the particle layering area, the product particles with higher relative density and the raw material particles with lower density are layered by utilizing the difference of the particle sedimentation final speed in the ascending flow, so that the raw material which is not fully dissolved is separated from the product in the ascending flow, the retention time of the raw material with low density in the crystallizer is prolonged, the raw material with low density is further dissolved, reduced or even disappeared, meanwhile, the retention time of partial fine particles in the crystallized product can also be prolonged due to the fact that the fine particles and the coarse particles have different movement tracks in the flow field, the product particle size is further increased, and finally the crystals with larger particles enter the material discharging area.
The decomposing crystallizer for potassium salt industry can be used for dissolving and crystallizing carnallite to prepare potassium chloride and can also be used for the crystal production of potassium sulfate by double decomposition of potassium chloride and double salt containing magnesium sulfate. The potassium chloride and the potassium sulfate are crystallized and produced by the invention, and the upper limit of the feeding granularity of the raw materials and the processing capacity of unit volume in the dissolving area can be improved due to the existence of the material scattering device and the liquid distribution device; a liquid distribution device and a flow guide cone are arranged on the basis of CFD and DEM technologies, active upwash is introduced to form a particle bed, so that the residence time of fine particle products and low-density raw materials in a crystallizer body is prolonged by utilizing the difference of motion paths of different particle densities and particle sizes in a fluid, the entrainment rate of the raw materials in crystallized products is reduced, the particle sizes of the products are increased, and a better crystallization effect is obtained.
Drawings
FIG. 1 is a schematic view of a decomposition crystallizer in accordance with embodiment 1 of the present invention;
in the figure: 1. the device comprises a crystallizer body, 2 mother liquor overflow ports, 3 feeding baffle plates, 4 bulk spreaders, 5 a main stirring device, 6 an inner guide cylinder, 7 an outer guide cylinder, 8 a guide cone, 9 a liquid distribution device, 10 a discharging stirring device, 11 a discharge port, 12 and a mother liquor replenishing pipe; a-dissolution zone, B-crystallization zone, C-particle stratification zone, D-mother liquor clarification zone, and E-product discharge zone.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Referring to fig. 1, this embodiment includes crystallizer body 1, feed baffle 3, balk cargo ware 4, main agitating unit 5, interior draft tube 6, outer draft tube 7, diversion cone 8, cloth liquid device 9, arranges material agitating unit 10 and mother liquor moisturizing pipe 12, feed baffle 3, interior draft tube 6, outer draft tube 7, diversion cone 8, cloth liquid device 9 pass through support and crystallizer body 1 welded connection, main agitating unit 5, row material agitating unit 10 pass through support and bearing and are connected with crystallizer body 1, crystallizer body 1 upper end is equipped with mother liquor overflow mouth 2, and the bottom is equipped with bin outlet 11, cloth liquid device 9 is located under interior draft tube 6, links to each other with mother liquor moisturizing pipe 12.
In the embodiment, the diameter phi of a cylinder at the upper end of the crystallizer body 1 is 12m, the height of the cylinder is 5.0m, and the included angle between the bevel edge of a cone at the lower end and the horizontal plane is 50 degrees and the height of the bevel edge of the cone is 6.2 m; the feeding baffle 3 is cylindrical, and has a diameter phi of 3.6m and a height phi of 0.96 m; the bottom edge of the mother liquor overflow hole 2 is 0.6m away from the upper end of the crystallizer body 1; the material scattering device 4 is conical, and the maximum section diameter is 0.4 m; the main stirring device 5 is a double-helix propelling type stirring device with 4 blades; the inner draft tube 6 is horn-shaped, the diameter of the upper end of the inner draft tube is phi 4.8m, the included angle between the inclined edge and the horizontal plane is 60 degrees and the height of the inclined edge is 2.1m, and the diameter of the lower end of the inner draft tube is phi 2.4m and the height of the lower end of the inner draft tube is 3.0 m; the outer guide cylinder 7 is horn-shaped, the diameter of the cylinder at the upper end is phi 9.6m and the height is 0.96m, the included angle between the inclined edge of the middle section and the horizontal plane is 45 degrees and the height is 2.4m, and the diameter of the cylinder at the lower end is 4.8m and the height is 1.7 m; the diversion cone 8 is in a reverse taper shape, the diameter phi of the upper end is 8.0m, the included angle between a bus and the horizontal is 55 degrees, the diameter of the bottom is 4.0m, the top of the diversion cone is 0.5m higher than the lowest part of the lower end of the outer diversion cylinder 7, and the bottom of the diversion cone is 0.3m lower than the top of the liquid distribution device 9; the liquid distribution device 9 consists of a bottom plate and a liquid distribution plate, the diameter of a water distribution hole on the liquid distribution plate is 0.8mm, the bottom plate is in a reverse taper shape, the diameter phi of the upper end of the bottom plate is 2.4m, the included angle between a bus and the horizontal line is 32 degrees, the diameter DN200 of the bottom of the liquid distribution plate, and the distance between the highest position of the top center and the lower end of the outer draft tube 7 is 2.0 m; the discharging and stirring device 10 is a straight 2-blade stirring device; the diameter DN150 of the discharge opening 11; the diameter of the mother liquor replenishing pipe 12 is DN 200.
The crystallizer is adopted to carry out cold decomposition crystallization on carnallite, overflow mother liquor after fine grains are removed and supplemented mother liquor are used as liquor distribution of a liquor distribution device 9, when the maximum feeding granularity of raw ore is 6.4mm, the mass concentration of slurry in a circulation area reaches 28 percent, and the treatment capacity of the crystallizer is 72 kg/(h.m)3) And the crystal product of the underflow discharge contains 3 percent of carnallite and the granularity of potassium chloride crystal P50 is 0.42 mm.
Example 2
This example differs from example 1 in that:
1) the diameter DN300 of the mother liquor replenishing pipe 12;
2) discharge port 11 diameter DN 200;
3) the liquid distribution device 9 consists of a bottom plate and a liquid distribution plate, the diameter of a water distribution hole on the liquid distribution plate is 1.2mm, the bottom plate is in a reverse taper shape, the diameter phi of the upper end of the bottom plate is 1.8m, the included angle between a bus and the horizontal plane is 38 degrees, the diameter DN of the bottom of the top of the bottom of the outer draft tube 7, and the top of the bottom of the outer draft tube of the bottom;
4) the material scattering device 4 is conical, and the maximum section diameter is 0.5 m;
5) the diversion cone 8 is in a reverse taper shape, the diameter phi of the upper end is 8.0m, the included angle between a bus and the horizontal is 55 degrees, the diameter of the bottom is 4.0m, the top of the diversion cone is 0.5m higher than the lowest part of the lower end of the outer diversion cylinder 7, and the bottom of the diversion cone is 0.2m lower than the top of the liquid distribution device 9;
6) the main stirring device 5 is a double-layer three-narrow-blade paddle, and the space between the paddles is 2 m.
The crystallizer is adopted to carry out cold double decomposition and cold crystallization on picromerite and potassium chloride, the overflow mother liquor and the supplement mother liquor after removing fine crystals are also used as the liquor distribution of the liquor distribution device 9, and the treatment capacity of the crystallizer is 55 kg/(h.m)3) The content of potassium sulfate in the crystal product discharged from underflow is 98.8%, and the granularity of potassium sulfate crystal P50 is 0.38 mm.
Claims (9)
1. A decomposing crystallizer for potassium salt industry is characterized in that: the crystallizer comprises a crystallizer body, an outer guide cylinder, an inner guide cylinder, a feeding baffle, a material scattering device, a main stirring device, a liquid distribution device, a mother liquid supplementing pipe, a guide cone and a discharging stirring device, wherein the outer guide cylinder, the inner guide cylinder and the feeding baffle are fixedly connected with the crystallizer body through a support, the main stirring device is fixed on the crystallizer body through the support, a stirring shaft and blades of the main stirring device are positioned in the inner guide cylinder, the material scattering device is connected with the inner guide cylinder through the support or directly installed on the stirring shaft, the guide cone is in an inverted cone shape, the guide cone is arranged in the crystallizer body and positioned below the outer guide cylinder and fixedly connected with the crystallizer body through the support, the liquid distribution device is arranged in the crystallizer body and positioned under the inner guide cylinder and the outer guide cylinder, the mother liquid supplementing pipe is connected with the liquid distribution device, and the discharging stirring device is arranged at the inner bottom of the crystallizer body, the crystallizer body upper end is equipped with the mother liquor overflow mouth, crystallizer body bottom is equipped with the bin outlet.
2. The potassium salt industrial decomposition crystallizer according to claim 1, characterized in that: the material scattering device is positioned right above the blades of the main stirring device.
3. The potassium salt industrial decomposition crystallizer according to claim 2, characterized in that: the shape of the material scattering device is one of conical shape, hemispherical shape and multi-surface conical shape.
4. The potassium salt industrial decomposition crystallizer according to claim 3, characterized in that: the material scattering device is conical, and the equivalent diameter of the largest cross section of the material scattering device is 0.15-0.40 times of the diameter of the inner guide cylinder.
5. The potassium salt industrial decomposition crystallizer according to claim 1, characterized in that: the liquid distribution device is located under the main stirring device, and the distance from the top of the liquid distribution device to the bottom of the inner guide cylinder is 0.8-1.2 times of the diameter of the inner guide cylinder.
6. The potassium salt industrial decomposition crystallizer according to claim 5, characterized in that: the liquid distribution device is composed of a bottom plate and a liquid distribution plate, the bottom plate is connected with a mother liquid supplementing pipe, the bottom plate is one or combination of an inverted cone, a multi-face cone and a horn, water distribution holes are distributed in the liquid distribution plate, and the diameter of each water distribution hole is 0.20-3.0 mm.
7. The potassium salt industrial decomposition crystallizer according to claim 6, characterized in that: the bottom plate is in an inverted conical shape, and the included angle between a generatrix of the bottom plate and the horizontal direction is 30-60 degrees.
8. The potassium salt industrial decomposition crystallizer according to claim 1, characterized in that: the central axis of the flow guide cone is the same as that of the crystallizer body.
9. The potassium salt industrial decomposition crystallizer according to claim 8, characterized in that: the top of the diversion cone is 0.1-1.0 time of the diameter of the bottom of the outer diversion cylinder higher than the bottom of the outer diversion cylinder, the bottom of the diversion cone is 0-0.2 time of the diameter of the top of the liquid distribution device lower than the top of the liquid distribution device, and the included angle between the generatrix of the diversion cone and the horizontal direction is 52-90 degrees.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111643924B (en) * | 2020-05-29 | 2022-05-03 | 中蓝长化工程科技有限公司 | Circulating fluidized bed decomposition crystallization device and decomposition crystallization method |
| CN115159547A (en) * | 2022-08-12 | 2022-10-11 | 成都泰利创富锂业科技有限公司 | Method for improving recovery rate of potassium chloride prepared from raw ore carnallite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2634665B1 (en) * | 1988-07-29 | 1991-12-13 | Solvay | PROCESS AND PLANT FOR CRYSTALLIZATION OF A MINERAL SUBSTANCE AND CRYSTALS OF SODIUM CHLORIDE |
| WO2006047717A2 (en) * | 2004-10-25 | 2006-05-04 | The Doe Run Resources Corporation | A process for making high purity sodium sulfate |
| CN201139964Y (en) * | 2007-12-28 | 2008-10-29 | 化工部长沙设计研究院 | Enhancement type crystallizer |
| US8282898B2 (en) * | 2009-11-23 | 2012-10-09 | Karnalyte Resources Inc. | Process for the formulation of potassium chloride from a carnallite source |
| CN201857276U (en) * | 2010-10-19 | 2011-06-08 | 四川蓝光伟业高新技术有限公司 | Crystallizing device for producing large-particle sodium chloride |
| US9309576B2 (en) * | 2013-03-13 | 2016-04-12 | Rockwell Automation Technologies, Inc. | Sugar crystallization control system and method |
| CN105597362B (en) * | 2016-03-17 | 2017-08-25 | 化工部长沙设计研究院 | A kind of Potash Industry machinery crystallizer |
| CN207085390U (en) * | 2017-07-31 | 2018-03-13 | 南京圆点环境清洁技术有限公司 | A kind of titanium dioxide vacuum crystallization device |
| CN107638711B (en) * | 2017-09-22 | 2020-07-14 | 南通联源机电科技股份有限公司 | High-strength sylvite industrial crystallizer simply supported |
| CN107803047A (en) * | 2017-12-12 | 2018-03-16 | 天津大学 | A kind of continuous decomposition crystallizer for carnallite thermal decomposition preparing potassium chloride |
| CN109794176B (en) * | 2019-03-25 | 2021-11-26 | 中蓝长化工程科技有限公司 | Fine crystal dissolving device of carnallite cold decomposition crystallizer |
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