Reaction processing device and processing method for preparing mineral fertilizer

By designing a reaction processing device for potassium fertilizer production, and using mechanical force chemical effects to treat low-grade phosphate ore and potassium feldspar, the problems of high energy consumption and high production costs in traditional potassium fertilizer production processes are solved, and low-cost and high-efficiency nitrogen, phosphorus and potassium mineral fertilizer production are achieved.

CN119971980APending Publication Date: 2025-05-13ANHUI DIYUANKANG AGRICULTURAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510326844.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-19
Publication Date
2025-05-13

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Abstract

The invention discloses a reaction processing device for mineral fertilizer preparation and a processing method, and relates to the technical field of reaction production equipment of mineral fertilizers, the reaction processing device comprises a feeding device, a reaction tank, a stirring device, an acid adding device, a neutralizing device, a pressure monitoring device, a temperature monitoring device, a safe exhaust device and a screening device; powder materials and water are fully premixed in the feeding mixer, the production time is shortened, and the overall production efficiency is improved. As the water content is low after the materials are mixed, ball milling is added to improve the mixing effect. The material mixing and grinding, the acidification mechanochemical ion exchange reaction and the ammonification neutralization ammonification reaction are integrally completed in the reaction tank, the technological process is simplified, the production efficiency is high, the reaction yield is high, the production cost of the mineral fertilizer is reduced, and the market competitiveness of the product is enhanced.
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Description

Technical Field

[0001] The invention relates to the technical field of reaction production equipment for mineral fertilizers, and in particular to a reaction processing device and a processing method for preparing mineral fertilizers. Background Art

[0002] my country's potassium resources are not abundant, and soluble potassium resources are seriously insufficient. The potash reserves in Qinghai are 116 million tons (measured in KCl), and the average KCl grade of potassium-rich brine ore layers is 1.29%; the potash reserves in Lop Nur, Xinjiang are 250 million tons (measured in KCl), and the average KCl grade of brine is 1.40%. my country's per capita soluble potassium salt reserves are only 1 / 14 of the world average; and the application of potassium fertilizer is the most important factor in improving crop quality, which has led to the import of a large amount of potassium fertilizer. At present, my country's dependence on foreign potassium fertilizers has reached more than 80%. Therefore, it is of great significance to improve my country's potassium fertilizer self-sufficiency rate.

[0003] my country's insoluble low-grade potash reserves exceed 5 billion tons of K2O (equivalent to 8 billion tons of KCl), and are widely distributed in agricultural production areas. Among them, potassium feldspar is the main source. The development of potassium feldspar to produce potassium fertilizer technology in my country began in the late 1950s. Due to the lack of mechanism research, the development of technology has been slow. At present, the more typical process routes are: (1) High-temperature volatilization method, which is to crush potassium feldspar, limestone, dolomite, fluorite and coke and then mix them into the furnace in proportion. The furnace temperature is as high as 1600℃, and the volatilized K2O reacts with the CO2 in the furnace to generate K2CO3. The disadvantages are high energy consumption, low potassium yield and no economic benefits. (2) High-temperature sintering method, which is to mix potassium feldspar and additives and grind them into fine powder, and then melt and roast them in a high-temperature furnace. The temperature is around 1000℃, and the economic benefits are still difficult to pass. There are also serious problems such as high-temperature corrosion and difficulty in handling the lower slag. (3) Fluorine decomposition method, which uses fluoride or fluorine-containing auxiliary agents in an inorganic acid medium to decompose potassium feldspar at a temperature below 200°C. Since the side reaction product potassium fluorosilicate is only soluble in hydrochloric acid solution and insoluble in water, the potassium extraction rate in the non-hydrochloric acid system will not be very high, and can only be around 80% at most. At the same time, the quality of fluorine corrosion prevention equipment is difficult to pass. (4) Microbial decomposition method, which uses auxiliary materials such as microbial bacteria to react with potassium feldspar in a biochemical reaction. The advantage of this method is that the process is short and there is no discharge of three wastes. However, the reproduction ability and vitality of the strains are weak, and it is difficult to survive under natural conditions. Genetic engineering is also needed to further screen and cultivate new strains. At the same time, the decomposition speed is slow, the time is long, and the conversion rate is low, which cannot be used for large-scale industrial production.

[0004] Invention patent CN200610156031 conducted basic research on potassium feldspar, thus gaining an in-depth understanding of its structure and properties. The aluminum and silicon in potassium feldspar form coordination tetrahedra with oxygen, forming a strong tetrahedral network structure. Its chemical properties are extremely stable and it cannot be decomposed by any acid or alkali except hydrofluoric acid at room temperature. However, there are obviously large gaps in the structure of potassium feldspar. Under certain conditions, Ca 2+ 、Na + etc. can replace the variable ion K in the potassium feldspar structure + . Thus, the reaction mechanism of extracting potassium from potassium feldspar by ion exchange was proposed.

[0005] The above invention selects the acid leaching process of phosphate ore and potassium feldspar. During the acid leaching process, the inorganic acid decomposes the phosphate ore, freeing the calcium therein, and then replacing the potassium of the potassium feldspar (i.e., ion exchange). This process is represented by the following chemical reaction formula:

[0006] Ca5(PO4)3F+H + →Ca 2+ +H2PO4 + +HF

[0007] Ca 2+ +2KAlSi3O8→CaAl2Si2O8+2K + +4SiO2↓

[0008] As can be seen from the above formula, the product of the acid leaching reaction contains active phosphorus (H2PO4 + ) and active potassium (K + ), and the solution is acidic, so it can be neutralized (also called ammoniation) with ammonia (gas or liquid), ammonia water or ammonium carbonate to introduce active nitrogen (i.e. ammonium nitrogen NH 4+ ), and then granulate to obtain mineral fertilizer containing nitrogen, phosphorus and potassium.

[0009] It can also be seen from the above formula that there are by-products such as calcium feldspar and silica in the acid leaching reaction products. These by-products are inert and will not affect the stability of mineral fertilizers if left in them, and will not damage the soil if applied to the soil.

[0010] The above invention has remained in the experimental stage since the beginning of research, due to the lack of breakthroughs in production equipment. Recently, through the mechanical chemical effects of planetary ball mills, stirred mills, ordinary ball mills, etc., a breakthrough has been made in the production process equipment of this invention.

[0011] At present, nitrogen, phosphorus and potassium ternary compound fertilizer is mainly made by mixing and processing urea, general calcium or calcium magnesium phosphate fertilizer and potassium chloride. It is a mixture with high production cost.

[0012] The invention can produce nitrogen, phosphorus and potassium mineral fertilizers from low-grade phosphate rock (P2O5≤15%) and low-grade potassium feldspar ore (K2O≤10%), has low raw material cost, simple production process, no large amount of heating energy consumption, low production cost, can effectively utilize my country's low-grade potassium ore and phosphorus ore resources, improve my country's self-sufficiency rate of potassium fertilizers, improve soil structure, increase the yield and quality of crops, and make outstanding contributions to my country's agricultural development. Summary of the invention

[0013] The invention provides a reaction processing device and a processing method for preparing mineral fertilizers, which solve the technical problem of high production cost of traditional production process equipment.

[0014] In order to solve the above technical problems, the present invention provides a reaction processing device for preparing mineral fertilizers, comprising a feeding device, a reaction tank, a stirring device, an acid adding device, a neutralizing device, a pressure monitoring device, a temperature monitoring device, a safety exhaust device and a screening device;

[0015] The discharge port of the feeding device is connected to the reaction tank, the stirring device, the acid adding device, the neutralizing device, the pressure monitoring device, the temperature monitoring device, and the safety exhaust device are all installed on the reaction tank, and the screening device is arranged below the reaction tank.

[0016] In some embodiments, the feeding device includes a phosphate rock powder metering and feeding device, a potassium feldspar ore powder metering and feeding device, a water spraying device, a mixer, a feeding and mixing device and a storage tank; the phosphate rock powder metering and feeding device and the potassium feldspar ore powder metering and feeding device are respectively arranged on both sides of the mixer, the water spraying device is arranged above the mixer, the feeding and mixing device is arranged at the bottom of the mixer, the discharge port of the feeding and mixing device is connected to the feed port of the storage tank, and the discharge port of the storage tank is connected to the reaction tank.

[0017] In some embodiments, the reaction tank is installed at an angle, a heating device is provided on the surface of the reaction tank, and a feeding port, an agitator inlet, an acid adding port, an ammonia adding port, a pressure measuring port, a gas phase temperature measuring port, a material temperature measuring port, a safety exhaust port, a ball adding port and a discharge port are respectively opened on the surface of the reaction tank, the interior of the reaction tank is lined with a corrosion protection lining, and a stirring grinding ball is provided in the reaction tank.

[0018] In some embodiments, the stirring device includes at least two sets of independent agitators, which are connected to the agitator inlet of the reaction tank, driven by a motor and a reducer, and have a rotation speed of 10 to 200 r / min. The distance from the outer edge of the spiral belt of the agitator to the tank wall is 1.2 to 10 times the maximum grinding ball diameter. The agitator is a cone tower structure, and the agitator is completely immersed 10 to 500 mm below the material.

[0019] In some embodiments, the acid adding device includes an acid storage container, an acid pump, a first flow meter, an acid spray nozzle and a first valve, the acid storage container is connected to the acid pump, the output end of the acid pump is connected to the first flow meter, the first valve and the acid spray nozzle in sequence, and the acid spray nozzle is connected to the acid adding port of the reaction tank.

[0020] In some embodiments, the neutralization device includes an ammonia cylinder, an ammonia pressure reducing valve, a regulating valve, a second flow meter and a second valve. The output end of the ammonia cylinder is connected to the ammonia pressure reducing valve, the regulating valve, the second flow meter and the second valve in sequence, and the outlet end of the ammonia cylinder is connected to the ammonia adding port of the reaction tank.

[0021] In some embodiments, the pressure monitoring device includes an anti-corrosion pressure sensor, a pressure display and a pressure alarm. The anti-corrosion pressure sensor is connected to the pressure measuring port of the reaction tank, and the anti-corrosion pressure sensor is electrically connected to the pressure display and the pressure alarm.

[0022] In some embodiments, the safety exhaust device includes an adjustable safety valve, a control valve and a gas recovery device. One end of the adjustable safety valve is connected to the connecting pipeline between the anti-corrosion pressure sensor and the pressure measuring port of the reaction tank, and the other end of the adjustable safety valve is connected to the control valve and the gas recovery device in turn.

[0023] In some embodiments, the temperature monitoring device includes a gas phase temperature monitoring device and a liquid phase temperature monitoring device; the gas phase temperature monitoring device includes a gas phase temperature sensor, a gas phase temperature display and a gas phase temperature alarm, the gas phase temperature sensor is connected to the gas phase temperature measuring port of the reaction tank, and the gas phase temperature sensor is electrically connected to the gas phase temperature display and the gas phase temperature alarm; the liquid phase temperature monitoring device includes a liquid phase temperature sensor, a liquid phase temperature display and a liquid phase temperature alarm, the liquid phase temperature sensor is connected to the material temperature measuring port of the reaction tank, and the liquid phase temperature sensor is electrically connected to the liquid phase temperature display and the liquid phase temperature alarm.

[0024] In some embodiments, the screening device includes a hopper, a vibrating screen, and a ball transmission system. The hopper is arranged below the discharge port of the reaction tank, the vibrating screen is arranged in the hopper, the ball transmission system is arranged on the side of the hopper, and the ball transmission system is connected to the ball adding port of the reaction tank.

[0025] The present invention also provides a processing method of a reaction processing device for preparing mineral fertilizers, which specifically comprises the following steps:

[0026] S1, mixing: mixing phosphate rock powder and potassium feldspar ore powder in proportion, and premixing with water to form a slurry;

[0027] S2, reaction: adding the slurry and grinding balls into the reaction tank, starting stirring and heating to the reaction temperature;

[0028] S3, acidification: adding acid solution into the reaction tank for acidification reaction, and controlling the reaction process by pressure monitoring;

[0029] S4, neutralization: after the acidification reaction is completed, ammonia is added to neutralize to neutrality;

[0030] S5, screening: After the reaction is completed, the material is screened and the grinding balls are recovered.

[0031] In some embodiments, in step S1, the mixing ratio of the phosphate rock powder and the potassium feldspar ore powder is controlled by a metering feeding device, and an appropriate amount of water is added.

[0032] In some embodiments, in step S2, the volume of the grinding balls accounts for 1 / 5 to 1 / 2 of the volume of the reaction tank, and the reaction temperature is controlled by a gas phase and liquid phase temperature monitoring device.

[0033] In some embodiments, in step S3, the amount of acid added to the acidification reaction is controlled by a flow meter, and when the reaction pressure exceeds a safety threshold, a safety exhaust device is activated, and the gas is recovered for treatment.

[0034] In some embodiments, in step S4, the endpoint of the neutralization reaction is a pH value of 6 to 7, and the addition rate of ammonia is controlled by a pressure reducing valve and a second flow meter.

[0035] In some embodiments, in step S5, the screening process separates the grinding balls through a vibrating screen, and the grinding balls are returned to the reaction tank through a transmission system for recycling.

[0036] Compared with the related art, the reaction processing device and processing method for preparing mineral fertilizer provided by the present invention have the following beneficial effects:

[0037] The present invention provides a reaction processing device and a processing method for preparing mineral fertilizers. The interior of the reaction tank, the stirrer, and the grinding balls are made of protective materials such as alumina, zirconium oxide, tetrafluoroethylene, and PAI, which can be effectively protected, ensuring that the equipment can work stably for a long time and reducing the cost of equipment maintenance and replacement.

[0038] The present invention provides a reaction processing device and a processing method for preparing mineral fertilizers. The powder material and water are fully premixed in a feed mixer, which shortens the production time and improves the overall production efficiency. Since the water content of the materials after mixing is low, ball milling is added to increase the mixing effect. The material mixing and grinding, acid addition, mechanochemical ion exchange reaction, and ammonia addition and neutralization amination reaction are integrated in the reaction tank, which simplifies the process. It not only has high production efficiency, but also high reaction yield, which can reach 99.5% of the feed amount. Multi-blade stirring reduces stirring power and energy consumption, improves stirring, mixing, and grinding effects, greatly improves the mechanochemical effect, further shortens the reaction time, and the stirring speed is adjustable, which is convenient for multi-stage speed control, continuously improves efficiency, and reduces energy consumption.

[0039] The present invention provides a reaction processing device and a processing method for preparing mineral fertilizers. The entire process is equipped with a dust collecting device, and there is no dust pollution. The discharged gas is fully absorbed and filtered, and there is no pollution to the air. All reactants are useful fertilizers without solid waste. The liquid after gas absorption is used as water to add to the reaction materials when adding materials next time, and there is no waste liquid discharge, thereby realizing green production.

[0040] The present invention provides a reaction processing device and a processing method for preparing mineral fertilizers, which have low comprehensive energy consumption and high production efficiency, thereby reducing the production cost of mineral fertilizers and enhancing the market competitiveness of products. The pressure is controllable, the work is safer, the smooth operation of the production process is guaranteed, and the safety risks are reduced. The reaction tank can be heated, the reaction temperature can be adjusted, and the precise material addition and monitoring device are used to make the reaction more accurate and ensure the stable product quality. The comprehensive energy consumption is low and the production efficiency is high, thereby reducing the production cost of mineral fertilizers and enhancing the market competitiveness of products. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0042] Figure 2 It is a schematic structural diagram of the acid adding device of the present invention;

[0043] Figure 3 It is a schematic structural diagram of the neutralization device of the present invention.

[0044] Numbers in the figure: 1. Phosphate rock powder metering and feeding device; 2. Water spraying device; 3. Potash feldspar ore powder metering and feeding device; 4. Feeding and mixing device; 5. Storage tank; 6. Reactor; 7. Gas phase temperature monitoring device; 8. Stirring device; 9. Ball adding device; 10. Screening device; 11. Liquid phase temperature monitoring device; 12. Gas recovery device; 13. Safety exhaust device; 14. Pressure monitoring device; 15. Acid adding device; 16. Neutralizing device; 17. Heating device; 151. Acid storage container; 152. Acid pump; 153. First flowmeter; 154. First valve; 155. Acid spray nozzle; 161. Ammonia cylinder; 162. Ammonia pressure reducing valve; 163. Regulating valve; 164. Second flowmeter; 165. Second valve. DETAILED DESCRIPTION

[0045] Embodiment 1

[0046] This embodiment provides a reaction processing device and a processing method for preparing mineral fertilizers, such as Figure 1 As shown, the present invention includes a feeding device, a reaction tank 6, a stirring device 8, an acid adding device 15, a neutralizing device 16, a pressure monitoring device 14, a temperature monitoring device, a safety exhaust device 13 and a screening device 10. The discharge port of the feeding device is connected to the reaction tank 6, the stirring device 8, the acid adding device 15, the neutralizing device 16, the pressure monitoring device 14, the temperature monitoring device, and the safety exhaust device 13 are all installed on the reaction tank, and the screening device 10 is arranged below the reaction tank 6.

[0047] In this embodiment, the discharge port of the feeding device is connected to the reaction tank 6 to ensure that the material can smoothly enter the reaction tank for subsequent processing. The stirring device 8, the acid adding device 15, the neutralizing device 16, the pressure monitoring device 14, the temperature monitoring device and the safety exhaust device 13 are all installed on the reaction tank to ensure the smooth progress of the reaction. The screening device 10 is arranged below the reaction tank 6 to screen the product after the reaction.

[0048] Embodiment 2

[0049] On the basis of Example 1, the feeding device of this embodiment includes a phosphate rock powder metering and feeding device 1, a potassium feldspar ore powder metering and feeding device 3, a water spraying device 2, a mixer, a feeding and mixing device 4 and a storage tank 5; the phosphate rock powder metering and feeding device 1 and the potassium feldspar ore powder metering and feeding device 3 are respectively arranged on both sides of the mixer, the water spraying device 2 is arranged above the mixer, the feeding and mixing device 4 is arranged at the bottom of the mixer, the discharge port of the feeding and mixing device 4 is connected to the feed port of the storage tank 5, and the discharge port of the storage tank 5 is connected to the reaction tank 6.

[0050] In this embodiment, the phosphate rock powder metering and feeding device 1 and the potassium feldspar powder metering and feeding device 3 are respectively and accurately arranged on both sides of the mixer, and the mineral powder can be delivered to the mixer according to the preset formula ratio. The water spraying device 2 is located above the mixer, and the measured water can be sprayed into the mixer according to the ratio. In the mixer, the two mineral powders are fully in contact with water to achieve premixing. Subsequently, the material enters the feeding and mixing device 4, which is a key device for premixing, dispersing and homogenizing the two mineral powders and water, and has the characteristics of accurate metering, uniform dispersion and stable feeding amount. Its main composition is as follows: each of the two mineral powders is equipped with a spiral metering feeder, and the material is fed into the hopper of the feeding and mixing device 4, and the water is metered and sprayed into the hopper, which can both reduce dust and evenly distribute the material. The mineral powder after water spraying is sent to the mixing section through a spiral propeller for high-speed shearing, stirring and mixing. The mixed material finally enters the storage tank 5, and the discharge port of the storage tank 5 is connected to the reaction tank 6 to continuously supply the reaction tank 6.

[0051] Embodiment 3

[0052] On the basis of Example 1, the reaction tank 6 of this embodiment is installed at an angle, and a heating device 17 is provided on the surface of the reaction tank 6. The surface of the reaction tank 6 is respectively provided with a feeding port, an agitator inlet, an acid adding port, an ammonia adding port, a pressure measuring port, a gas phase temperature measuring port, a material temperature measuring port, a safety exhaust port, a ball adding port and a discharge port. The interior of the reaction tank 6 is lined with a corrosion protection lining, and stirring and grinding balls are provided in the reaction tank 6. The volume of the stirring and grinding balls accounts for 1 / 5 to 1 / 2 of the volume of the reaction tank 6.

[0053] In this embodiment, the reaction tank 6 is installed at an angle as the core reaction equipment, and a heating device 17 is provided on the surface, which can accurately control the temperature according to the reaction requirements. The surface of the reaction tank 6 is respectively provided with a feed port, an agitator inlet, an acid addition port, an ammonia addition port, a pressure measuring port, a gas phase temperature measuring port, a material temperature measuring port, a safety exhaust port, a ball adding port and a discharge port to meet various material addition, monitoring and operation requirements. The interior of the reaction tank 6 is lined with a corrosion protection lining, which uses protective materials such as alumina, zirconium oxide, tetrafluoro, PAI, etc., to effectively resist corrosion during the reaction process and ensure long-term stable operation of the equipment. In addition, a stirring and grinding ball is provided in the reaction tank 6, and the volume of the stirring and grinding ball accounts for 1 / 5 to 1 / 2 of the volume of the reaction tank 6, which plays a key role in the material mixing and grinding process.

[0054] Embodiment 4

[0055] On the basis of the third embodiment, the stirring device 8 of this embodiment includes at least two sets of independent stirrers, which are connected to the stirrer inlet of the reaction tank 6, and are driven by a motor and a reducer. The rotation speed of the stirrer is adjustable between 10 and 200 r / min, and the distance from the outer edge of the spiral belt of the stirrer to the tank wall is 1.2 to 10 times the maximum grinding ball diameter. The stirrer is a cone tower structure, and the stirrer is completely immersed in the material 10 to 500 mm.

[0056] In this embodiment, the stirring device 8 includes at least two sets of independent stirrers, which are connected to the stirrer inlet of the reaction tank 6 and driven by a motor and a reducer. The rotation speed is adjustable at 10 to 200 r / min, and the stirring speed can be flexibly adjusted according to different reaction stages, which is more conducive to multi-stage speed control, improving efficiency and reducing energy consumption. The distance from the outer edge of the spiral belt of the stirrer to the tank wall is 1.2 to 10 times the diameter of the maximum grinding ball, which effectively prevents the material from sticking to the wall. The stirrer is a cone tower structure, which is completely immersed 10 to 500 mm below the material. The upper stirrer is designed to be conical, and its paddle body is completely located 10 to 400 mm below the material, which can not only enhance the reaction effect and improve the reaction efficiency, but also reduce power consumption and prevent current fluctuations. Each stirrer uses a spiral belt plus blade type or a multi-blade type or a frame type or a propeller type, which can be of the same structure or a different structure, to increase the pushing and turning effect on the material. Multiple stirrers use one outlet, and each stirrer is provided with a moving channel. After moving to the outlet, it can be taken out, which is convenient for maintenance and replacement.

[0057] Embodiment 5

[0058] On the basis of Example 3, the acid adding device 15 of this embodiment includes an acid storage container 151, an acid pump 152, a first flow meter 153, an acid nozzle 155 and a first valve 154. The acid storage container 151 is connected to the acid pump 152, and the output end of the acid pump 152 is connected to the first flow meter 153, the first valve 154 and the acid nozzle 155 in sequence. The acid nozzle 155 is connected to the acid adding port of the reaction tank 6.

[0059] In this embodiment, the acid adding device 15 ensures that the acid solution can be accurately measured and stably delivered to the reaction tank 6 to achieve a mechanochemical acidification reaction.

[0060] Embodiment 6

[0061] On the basis of Example 3, the neutralization device 16 of this embodiment includes an ammonia cylinder 161, an ammonia pressure reducing valve 162, a regulating valve 163, a second flow meter 164 and a second valve 165. The output end of the ammonia cylinder 161 is connected to the ammonia pressure reducing valve 162, the regulating valve 163, the second flow meter 164 and the second valve 165 in sequence, and the outlet end of the ammonia cylinder 161 is connected to the ammonia adding port of the reaction tank 6.

[0062] In this embodiment, in the later stage of the reaction, ammonia gas can be accurately introduced into the reaction tank 6 as required to carry out a neutralization and amination reaction until the pH reaches 6-7, the ammonia addition is completed, and the second valve 165 is closed.

[0063] Embodiment 7

[0064] Based on the first embodiment, the pressure monitoring device 14 of this embodiment includes an anti-corrosion pressure sensor, a pressure display and a pressure alarm. The anti-corrosion pressure sensor is connected to the pressure measuring port of the reaction tank 6, and the anti-corrosion pressure sensor is electrically connected to the pressure display and the pressure alarm.

[0065] In this embodiment, the pressure monitoring device 14 includes an anti-corrosion pressure sensor, a pressure display and a pressure alarm. The anti-corrosion pressure sensor is connected to the pressure measuring port of the reaction tank 6, and is electrically connected to the pressure display and the pressure alarm to monitor the pressure inside the reaction tank 6 in real time. When the pressure reaches the upper limit of the safe pressure, it can promptly alarm and ensure production safety.

[0066] Embodiment 8

[0067] On the basis of Example 7, the safety exhaust device 13 of this embodiment includes an adjustable safety valve, a control valve and a gas recovery device 12. One end of the adjustable safety valve is connected to the connecting pipeline between the anti-corrosion pressure sensor and the pressure measuring port of the reaction tank 6, and the other end of the adjustable safety valve is connected to the control valve and the gas recovery device 12 in sequence.

[0068] In this embodiment, the safety exhaust device 13 includes an adjustable safety valve, a control valve and a gas recovery device 12. One end of the adjustable safety valve is connected to the connecting pipeline between the anti-corrosion pressure sensor and the pressure measuring port of the reaction tank 6, and the other end is connected to the control valve and the gas recovery device 12 in sequence. When the reaction pressure is too high, the exhaust is opened in time to discharge the gas into the gas recovery device 12 for absorption of harmful gases to avoid polluting the environment.

[0069] Embodiment 9

[0070] On the basis of Example 3, the temperature monitoring device of this embodiment includes a gas phase temperature monitoring device 7 and a liquid phase temperature monitoring device 11; the gas phase temperature monitoring device 7 includes a gas phase temperature sensor, a gas phase temperature display and a gas phase temperature alarm, the gas phase temperature sensor is connected to the gas phase temperature measuring port of the reaction tank 6, and the gas phase temperature sensor is electrically connected to the gas phase temperature display and the gas phase temperature alarm; the liquid phase temperature monitoring device 11 includes a liquid phase temperature sensor, a liquid phase temperature display and a liquid phase temperature alarm, the liquid phase temperature sensor is connected to the material temperature measuring port of the reaction tank 6, and the liquid phase temperature sensor is electrically connected to the liquid phase temperature display and the liquid phase temperature alarm.

[0071] In this embodiment, the gas phase temperature monitoring device 7 and the liquid phase temperature monitoring device 11 work together to accurately monitor the temperature of the gas phase and the liquid phase in the reaction tank 6, and through linkage with the heating device 17, accurate control of the reaction temperature is achieved.

[0072] Embodiment 10

[0073] Based on Example 3, the screening device 10 of this embodiment includes a hopper, a vibrating screen, and a ball transmission system. The hopper is arranged below the discharge port of the reaction tank 6, the vibrating screen is arranged in the hopper, the ball transmission system is arranged on the side of the hopper, and the ball transmission system is connected to the ball adding port of the reaction tank 6.

[0074] In this embodiment, the hopper is arranged below the discharge port of the reaction tank 6 to receive the reacted materials and grinding balls. The vibrating screen is arranged in the hopper to screen the materials and separate qualified mineral fertilizer products. The ball transmission system is arranged on the side of the hopper and connected to the ball feeding port of the reaction tank 6 to return the screened grinding balls to the reaction tank 6 to realize the recycling of the grinding balls.

[0075] Embodiment 11

[0076] This embodiment also provides a production method of a reaction processing device and a processing method for preparing a mineral fertilizer, which specifically includes the following steps:

[0077] (1) Two kinds of mineral powders are taken, and are fed into a feeding and mixing device 4 according to a formula ratio through a phosphate rock powder metering and feeding device 1 and a potassium feldspar ore powder metering and feeding device 3. After water is metered, it is sprayed into the feeding and mixing device 4 according to a ratio through a water spraying device 2. In the mixer, the two kinds of mineral powders are fully premixed with water, and then mixed and fed into a storage tank 5.

[0078] (2) The mixed materials enter the reaction tank 6 through the discharge port of the storage tank 5.

[0079] (3) Grinding balls are also added to the reaction tank 6 through the ball adding device 9 in proportion to the material.

[0080] (4) After all the materials and balls are added, close the valves of the ball adding port and the loading port; start the stirring device 8, and monitor and control the heating device 17 through the gas phase temperature monitoring device 7 and the liquid phase temperature monitoring device 11 to heat the reaction tank 6 and the materials in the tank.

[0081] (5) When the required temperature for the reaction is reached, the first valve 154 of the acid adding device 15 is opened while continuing to stir, and acid is added in a metered manner to carry out a mechanochemical acidification reaction. The reaction pressure is controlled by the pressure monitoring device 14. When the upper limit of the safety pressure is reached, the safety exhaust device 13 is opened, and the gas is discharged into the gas recovery device 12 for absorption of harmful gases. After the acid addition is completed, the first valve 154 is closed.

[0082] (6) Mix, grind and react under stirring conditions to fully activate the effective ingredients in the phosphate and potassium ore.

[0083] (7) After the reaction is completed, the second valve 165 of the neutralization device 16 is opened under stirring conditions, and ammonia is added in a metered manner to neutralize the amination reaction until the pH is 6-7. When the ammonia addition is completed, the second valve 165 is closed.

[0084] (8) Start the screening device 10, open the discharge valve, discharge and screen the grinding balls, and the grinding balls enter the ball adding device 9.

[0085] (9) When all the materials are discharged, turn off the stirring device 8; when the ball screening is completed, turn off the screening device 10; close the discharge valve and prepare for the next batch of production.

[0086] Example 12: Specific implementation method 1 of the production method of Example 11

[0087] (1) Take 28 kg of phosphate rock powder, 28 kg of potassium feldspar powder, and 14.6 kg of water and premix them thoroughly.

[0088] (2) Add the mixed materials into the 200L reaction tank 6.

[0089] (3) 80 L of grinding balls are added to the reaction tank 6 through the ball adding device 9.

[0090] (4) After all the materials and balls are added, close the tank cover; start the stirring device 8, adjust the speed to 80r / min for mixing and heating, and monitor and control the heating device 17 through the gas phase temperature monitoring device 7 and the liquid phase temperature monitoring device 11 to heat the reaction tank 6 and the materials to 100°C.

[0091] (5) When the temperature reaches 100°C, the first valve 154 of the acid adding device 15 is opened while continuing the stirring at 80 r / min, 23 kg of 98% sulfuric acid is added, and the stirring speed is increased to 110 r / min to carry out a mechanochemical acidification reaction. The reaction pressure is controlled below 0.6 MPa by the pressure monitoring device 14. When the pressure exceeds 0.6 MPa, the safety exhaust device 13 is opened, and the gas is discharged into the gas recovery device 12 for harmful gas absorption. After the acid addition is completed, the first valve 154 is closed.

[0092] (6) Mix, grind and react for 30 minutes at 110 r / min to fully activate the effective components in the phosphate and potassium ore.

[0093] (7) After the reaction is completed, under the stirring condition of 110 r / min, the second valve 165 of the neutralization device 16 is opened, ammonia is added to neutralize and ammonify to pH 6-7, and the second valve 165 is closed.

[0094] (8) The pressure in the reaction tank 6 is released to 0, and the tank cover is opened to discharge the materials. The grinding balls and the finished materials are separated by the screening device 10 to obtain 93 kg of nitrogen, phosphorus and potassium mineral fertilizer, with a phosphorus activation rate of 92%, a potassium release rate of 83%, and a comprehensive energy consumption of 380 kW·h / t.

[0095] Example 13: Specific implementation method 2 of the production method of Example 11

[0096] (1) 1050 kg of phosphate rock powder is fed into the feeding and mixing device 4 in proportion through the phosphate rock powder metering and feeding device 1 and 1050 kg of potassium feldspar powder is fed into the feeding and mixing device 4 through the potassium feldspar powder metering and feeding device 3; 547 kg of water is sprayed into the feeding and mixing device 4 through the water spraying device 2 for pre-mixing, and the mixed materials enter the storage tank 5.

[0097] (2) The mixed material is transported to the reaction tank 6 (7500L) through the discharge port of the storage tank 5.

[0098] (3) 3000 L of grinding balls are added to the reaction tank 6 through the ball adding device 9.

[0099] (4) Close the valves of the ball adding port and the charging port; start the stirring device 8, adjust the speed to 100 r / min, and control the heating device 17 through the gas phase temperature monitoring device 7 and the liquid phase temperature monitoring device 11 to heat the reaction tank 6 and the materials to 100°C.

[0100] (5) When the temperature reaches 100°C, the speed of the stirring device 8 is adjusted to 120 r / min, the first valve 154 of the acid adding device 15 is opened, and 862 kg of acid is added for acidification reaction. The pressure monitoring device 14 controls the pressure to ≤ 0.4 MPa. If the pressure exceeds the limit, the gas is discharged into the gas recovery device 12 through the safety exhaust device 13. After the acid addition is completed, the first valve 154 is closed.

[0101] (6) Under the stirring condition of 120 r / min, the mixing and grinding reaction is carried out for 50 minutes, and the phosphorus utilization rate in the phosphate rock powder is ≥90%, and the potassium utilization rate in the potassium feldspar powder is ≥80%.

[0102] (7) Open the second valve 165 of the neutralization device 16, add ammonia to neutralize to pH 6-7, and close the second valve 165.

[0103] (8) Open the screening device 10 to discharge and separate the grinding balls to the ball adding device 9 for recycling.

[0104] (9) After the materials are completely discharged, the stirring device 8 and the screening device 10 are closed to obtain 3500 kg of finished nitrogen, phosphorus and potassium mineral fertilizer.

[0105] The following are the advantages compared with traditional processes:

[0106] 1. Reaction efficiency

[0107] Traditional reaction time (8h): The traditional process requires multi-stage reaction and drying, and has low efficiency; the new equipment shortens it to 3h through process integration.

[0108] Phosphorus / potassium activation rate: Due to insufficient reaction, the phosphorus activation rate (>70%) and potassium release rate (>60%) of the traditional process are significantly lower than those of the new equipment (>90%, >80%).

[0109] 2. Raw material requirements and costs

[0110] Phosphate ore: Traditional processes require high-grade phosphate ore (>30% P), while new equipment can process low-grade ore (>15% P) through activation technology, reducing costs from RMB 1,200 / t to RMB 180 / t.

[0111] Potash ore: Traditional processes rely on high-grade potash ore (>20% K), while new equipment is compatible with low-grade ore (>10% K) through slow-release technology, reducing costs from 1,000 yuan / t to 180 yuan / t.

[0112] 3. Economic advantages

[0113] Through process optimization and raw material adaptability, the comprehensive cost of the new equipment is only 26.6% of the traditional process (930 yuan / t vs. 3,500 yuan / t).

[0114] Working principle: The present invention uses a stirring reaction tank 6 as the main equipment, and through the stirring and grinding mechanochemical effect of the equipment, and uniformly spraying acid, the phosphate rock is acidified, the phosphorus element in the phosphate rock is activated, and active calcium is obtained. Then, through the mechanochemical effect, the active calcium completes ion exchange with the potash ore. Finally, ammonia is introduced to neutralize and ammine the active phosphorus and potash binary fertilizers after the reaction, introduce active nitrogen elements, and realize the production of mineral nitrogen, phosphorus and potassium mineral fertilizers. Through mechanochemical activation and segmented speed control, the efficient release of phosphorus and potassium in the mineral is realized, and the nitrogen element is introduced through neutralization reaction. The final product is a highly active nitrogen, phosphorus and potassium mineral fertilizer, which is suitable for large-scale continuous production.

Claims

1. A reaction processing device for preparing mineral fertilizers, characterized in that: It includes a feeding device, a reaction tank, a stirring device, an acid adding device, a neutralizing device, a pressure monitoring device, a temperature monitoring device, a safety exhaust device and a screening device; The discharge port of the feeding device is connected to the reaction tank, the stirring device, the acid adding device, the neutralizing device, the pressure monitoring device, the temperature monitoring device, and the safety exhaust device are all installed on the reaction tank, and the screening device is arranged below the reaction tank; The feeding device includes a phosphate rock metering and feeding device, a potassium feldspar ore metering and feeding device, a water spraying device, a mixer, a feeding and mixing device and a storage tank; the phosphate rock metering and feeding device and the potassium feldspar ore metering and feeding device are respectively arranged on both sides of the mixer, the water spraying device is arranged above the mixer, the feeding and mixing device is arranged at the bottom of the mixer, the discharge port of the feeding and mixing device is connected to the feed port of the storage tank, and the discharge port of the storage tank is connected to the reaction tank; The reaction tank is installed at an angle, a heating device is provided on the surface of the reaction tank, a feeding port, an agitator inlet, an acid adding port, an ammonia adding port, a pressure measuring port, a gas phase temperature measuring port, a material temperature measuring port, a safety exhaust port, a ball adding port and a discharge port are respectively opened on the surface of the reaction tank, the interior of the reaction tank is lined with a corrosion protection lining, and a stirring and grinding ball is arranged in the reaction tank.

2. A reaction processing device for preparing mineral fertilizer according to claim 1, characterized in that: The stirring device includes at least two sets of independent stirrers, which are connected to the stirrer inlet of the reaction tank, driven by a motor and a reducer, with a rotation speed of 10 to 200 r / min, a distance from the outer edge of the spiral belt of the stirrer to the tank wall of 1.2 to 10 times the maximum grinding ball diameter, a cone tower structure, and a stirrer completely immersed 10 to 500 mm below the material.

3. A reaction processing device for preparing mineral fertilizer according to claim 1, characterized in that: The acid adding device comprises an acid storage container, an acid pump, a first flow meter, an acid spray nozzle and a first valve. The acid storage container is connected to the acid pump, and the output end of the acid pump is connected to the first flow meter, the first valve and the acid spray nozzle in sequence. The acid spray nozzle is connected to the acid adding port of the reaction tank.

4. The reaction processing device for preparing mineral fertilizer according to claim 1, characterized in that: The neutralization device includes an ammonia cylinder, an ammonia pressure reducing valve, a regulating valve, a second flow meter and a second valve. The output end of the ammonia cylinder is connected to the ammonia pressure reducing valve, the regulating valve, the second flow meter and the second valve in sequence, and the outlet end of the ammonia cylinder is connected to the ammonia adding port of the reaction tank.

5. The reaction processing device for preparing mineral fertilizer according to claim 1, characterized in that: The pressure monitoring device comprises an anti-corrosion pressure sensor, a pressure display and a pressure alarm. The anti-corrosion pressure sensor is connected to the pressure measuring port of the reaction tank, and the anti-corrosion pressure sensor is electrically connected to the pressure display and the pressure alarm.

6. A reaction processing device for preparing mineral fertilizer according to claim 5, characterized in that: The safety exhaust device includes an adjustable safety valve, a control valve and a gas recovery device. One end of the adjustable safety valve is connected to the connecting pipeline between the anti-corrosion pressure sensor and the pressure measuring port of the reaction tank, and the other end of the adjustable safety valve is connected to the control valve and the gas recovery device in sequence.

7. A reaction processing device for preparing mineral fertilizer according to claim 1, characterized in that: The screening device includes a hopper, a vibrating screen, and a ball transmission system. The hopper is arranged below the discharge port of the reaction tank, the vibrating screen is arranged in the hopper, the ball transmission system is arranged on the side of the hopper, and the ball transmission system is connected to the ball adding port of the reaction tank.

8. The reaction processing device for preparing mineral fertilizer according to claim 1, characterized in that: The temperature monitoring device includes a gas phase temperature monitoring device and a liquid phase temperature monitoring device; the gas phase temperature monitoring device includes a gas phase temperature sensor, a gas phase temperature display and a gas phase temperature alarm, the gas phase temperature sensor is connected to the gas phase temperature measuring port of the reaction tank, and the gas phase temperature sensor is electrically connected to the gas phase temperature display and the gas phase temperature alarm; The liquid phase temperature monitoring device includes a liquid phase temperature sensor, a liquid phase temperature display and a liquid phase temperature alarm. The liquid phase temperature sensor is connected to the material temperature measuring port of the reaction tank, and the liquid phase temperature sensor is electrically connected to the liquid phase temperature display and the liquid phase temperature alarm.

9. A processing method using the reaction processing device for preparing mineral fertilizers according to any one of claims 1 to 8, characterized in that: The specific steps include: S1, mixing: mixing phosphate rock powder and potassium feldspar ore powder in proportion, and premixing with water to form a slurry; S2, reaction: adding the slurry and grinding balls into the reaction tank, starting stirring and heating to the reaction temperature; S3, acidification: adding acid solution into the reaction tank for acidification reaction, and controlling the reaction process by pressure monitoring; S4, neutralization: after the acidification reaction is completed, ammonia is added to neutralize to neutrality; S5, screening: After the reaction is completed, the material is screened and the grinding balls are recovered.

10. The processing method of a reaction processing device for preparing mineral fertilizer according to claim 9, characterized in that: In step S1, the mixing ratio of the phosphate rock powder and the potassium feldspar ore powder is controlled by a metering feeding device, and an appropriate amount of water is added; in step S2, the volume of the grinding balls accounts for 1 / 5 to 1 / 2 of the volume of the reaction tank, and the reaction temperature is controlled by a gas phase and liquid phase temperature monitoring device; in step S3, the amount of acid added in the acidification reaction is controlled by a flow meter, and when the reaction pressure exceeds the safety threshold, the safety exhaust device is started, and the gas is recovered for treatment; in step S4, the end point of the neutralization reaction is a pH value of 6 to 7, and the addition rate of ammonia is controlled by a pressure reducing valve and a second flow meter; in step S5, the screening process separates the grinding balls by a vibrating screen, and the grinding balls are returned to the reaction tank for recycling through a transmission system.

Citation Information

Patent Citations

  • Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar

    CN100999423A