Homogeneous crystal reaction system for continuously preparing functional powder material and application of homogeneous crystal reaction system

Abstract

The invention discloses a homogeneous crystal reaction system for continuously preparing a functional powder material and application of the homogeneous crystal reaction system. A homogeneous crystal reaction system comprises a constant flow pump used for controlling the feed liquid conveying amount and monitoring pipeline pressure and used for conveying all reaction feed liquid; the micro-mixing reactor is used for powder material nucleation and homogeneous crystal mixing reaction; the micro-channel aging device is used for micro-nano material aging; the system further comprises a detection device used for detecting reaction parameters. The collecting, filtering and washing device is used for collecting reaction products; the invention further discloses an application method corresponding to the system, and the problem that a reactor is blocked during synthesis of nanometer and micrometer functional powder materials can be solved. And a process route that the microreactor and the pipeline reactor are connected in series is adopted, the microreactor realizes a rapid and uniform mixing nucleation process of a multi-phase reaction liquid, and the pipeline reactor is used for realizing growth, aging and crystallization of a continuous powder material and prolonging the retention time, so that the purpose of continuously and efficiently preparing nano and micron functional powder materials is achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of functional powder preparation, and in particular relates to a homogeneous crystal reaction system for continuously preparing functional powder materials and an application thereof. Background Art

[0002] Traditional metallurgical and chemical processes are all carried out in reactors. In the process of preparing micro-nano powder materials, there are problems such as large equipment footprint, poor stability of powder materials in different reactors or batches, poor consistency of product batches, the need for multiple batches of mixing and packaging, low degree of automation, many operators required, high work intensity, low efficiency, large steam consumption, and high energy consumption.

[0003] In addition, micro-reaction technology is currently recognized as a cutting-edge innovative technology in the international chemical industry. Its core is to use microchannel structures and their modular combinations to continuously cut macroscopic fluids, creating a new micron-scale, highly structured flow mixing state and a highly controllable, fast heat exchange constant temperature reaction environment. Compared with other equipment, the reaction interface volume ratio and heat and mass transfer efficiency of the micro-reaction system are about 2 to 3 orders of magnitude higher than those of traditional kettle reactors. The advantages of the micro-reaction system are: the system is fully enclosed, feeding and discharging at room temperature, efficient gas-liquid separation, and strong process control capabilities; micro-reaction is a reaction process that realizes the participation or release of toxic and harmful substances; it is a rapidly exothermic reaction process; it is an innovative way with inherent safety attributes; it provides an inherent guarantee for obtaining higher purity, yield, selectivity, and high-quality products. However, when traditional micro-reactors are used to process solid-containing liquids, the channels will be blocked, making it difficult to run smoothly and achieve production.

[0004] Therefore, in view of the above-mentioned technical problems and defects, it is urgent to design and develop a homogeneous crystal reaction system for continuously preparing functional powder materials and its application. Summary of the invention

[0005] In order to overcome the above-mentioned deficiencies and difficulties in the prior art, the first object of the present invention is to provide a homogeneous crystal reaction system for continuously preparing functional powder materials.

[0006] The second object of the present invention is to provide a method for continuously preparing a homogeneous crystal reaction system of functional powder materials.

[0007] The first object of the present invention is achieved as follows: the homogeneous crystal reaction system includes a constant flow pump for conveying each reaction raw material liquid for controlling the material liquid conveying amount and monitoring the pipeline pressure; and a micro-mixing reactor for powder material nucleation and homogeneous crystal mixing reaction and a micro-channel aging device for aging micro-nano materials; The system also includes a detection device for detecting reaction parameters; and a collection, filtering and washing device for collecting reaction products.

[0008] The second object of the present invention is achieved in that the method comprises the steps of: Step 1: preparing at least two reaction fluids for preparing powder functional materials, and adjusting the pH value of the reaction stock solution corresponding to the fluids with an acid or a base; Step 2: passing the fluid into a continuous flow homogeneous crystal mixing reactor to cut it into micron-sized droplets to achieve rapid contact, collision and reaction; Step 3: After the reaction is completed, the generated solid powder product is filtered and dried to obtain a functional material precursor.

[0009] The scheme of the present invention is a homogeneous crystal reaction system for continuously preparing functional powder materials, the homogeneous crystal reaction system includes a constant flow pump for conveying each reaction raw material liquid for controlling the liquid delivery amount and monitoring the pipeline pressure; and a micro-mixing reactor for powder material nucleation and homogeneous crystal mixing reaction and a micro-channel aging device for aging micro-nano materials; the system also includes a detection device for detecting reaction parameters; and a collection, filtration and washing device for collecting reaction products; and an application method corresponding to the system, which can solve the problem of clogging the reactor in the synthesis of nano- and micron-functional powder materials. And the process route of microreactor and pipeline reactor in series is adopted, the former realizes the process of rapid and uniform mixing and nucleation of multi-phase reaction liquid, and the latter is used to realize the growth, aging and crystallization of continuous powder materials, and the residence time, aiming at continuous and efficient preparation of nano- and micron-functional powder materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 This is a schematic diagram of the framework structure of a homogeneous crystal reaction system for continuously preparing functional powder materials according to the present invention; Figure 2 It is a schematic diagram of the structure of a conventional reactor of a homogeneous crystal reaction system for continuously preparing functional powder materials according to the present invention; Figure 3 It is a schematic diagram of a conventional intermittent reactor structure of a homogeneous crystal reaction system for continuously preparing functional powder materials according to the present invention; Figure 4 It is a schematic diagram of a structure of an intelligent continuous synthesis of a homogeneous crystal reaction system for continuously preparing functional powder materials according to the present invention; Figure 5 It is a schematic diagram of the second structure of the intelligent continuous synthesis of a homogeneous crystal reaction system for continuously preparing functional powder materials according to the present invention; Figure 6 It is a schematic diagram of the intelligent continuous synthesis (one-step method) of iron phosphate by ammonium method / sodium method in a homogeneous crystal reaction system for continuously preparing functional powder materials of the present invention; Figure 7It is a schematic diagram of the intelligent continuous synthesis (two-step method) of iron phosphate by ammonium method / sodium method in a homogeneous crystal reaction system for continuously preparing functional powder materials of the present invention; Figure 8 This is a schematic diagram of anhydrous ferric phosphate prepared in Example 1 of the present invention; Fig. 9 This is a schematic diagram of anhydrous ferric phosphate prepared in Example 2 of the present invention; Fig.10 This is a schematic diagram of anhydrous ferric phosphate prepared in Example 3 of the present invention; Fig.11 This is a schematic diagram of the SEM electron microscope of the anhydrous ferric phosphate prepared in Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0011] The present invention is further described below in conjunction with the accompanying drawings, but the present invention is not limited in any way. Any changes or substitutions made based on the teachings of the present invention belong to the protection scope of the present invention.

[0012] As attached Figure 1-Figure 11 As shown, the present invention provides a homogeneous crystal reaction system for continuously preparing functional powder materials, the homogeneous crystal reaction system includes a constant flow pump for conveying each reaction raw material liquid for controlling the material liquid conveying amount and monitoring the pipeline pressure; and a micro-mixing reactor for powder material nucleation and homogeneous crystal mixing reaction and a micro-channel aging device for aging micro-nano materials; the system also includes a detection device for detecting reaction parameters; and a collection, filtering and washing device for collecting reaction products.

[0013] The microchannel aging device is a microwave reactor or an ultrasonic reactor or a multi-layer stirring pipeline.

[0014] The reaction parameters detected by the detection device include temperature data, pressure data, pH value data, dielectric data, conductivity data and nano-morphology monitoring data.

[0015] The system also includes: a rapid heat exchange system and a temperature and pressure monitoring element.

[0016] The micro-mixing reactor is also provided with a tubular reactor or a time-delay pipeline.

[0017] In order to achieve the object of the present invention, a method for continuously preparing a homogeneous crystal reaction system of a functional powder material is also provided, characterized in that the method comprises the following steps: Step 1: preparing at least two reaction fluids for preparing powder functional materials, and adjusting the pH value of the reaction stock solution corresponding to the fluids with an acid or a base; Step 2: passing the fluid into a continuous flow homogeneous crystal mixing reactor to cut it into micron-sized droplets to achieve rapid contact, collision and reaction; Step 3: After the reaction is completed, the generated solid powder product is filtered and dried to obtain a functional material precursor.

[0018] The reaction fluid contains one or more metal salt solutions, alkaline solutions or reagents that can precipitate the reaction fluid, and undergoes a co-precipitation reaction in a micro-mixing reactor, followed by filtration and washing, and then pumped into a tubular reactor for aging or crystallization.

[0019] The reagent that can precipitate the reaction fluid is one or more combinations of ammonium sulfide, ammonia water, sodium hydroxide, and ammonium carbonate. The reaction fluid is gas-liquid or oil-water or liquid suspension.

[0020] Specifically, in a specific embodiment of the scheme of the present invention, the purpose of the present invention is to provide a continuous intelligent micro-reaction metallurgical equipment for preparing functional powder materials; the equipment includes the following parts: a micro-mixing reactor with intelligent temperature control for nucleation of powder materials; a pipeline continuous flow reactor with intelligent temperature control for aging of micro-nano materials; a digital pump system for conveying raw material liquids of each reaction that can intelligently control the liquid delivery rate and monitor the pipeline pressure; a detection system for intelligently detecting parameters such as reaction pressure, temperature, pH value or dielectric constant of the reaction liquid at the target point; and a product collection system, etc.

[0021] Also provided is an application method of a micro-reaction intelligent device for continuously preparing functional powder materials, the method comprising the following steps: Two or more reaction fluids are configured to prepare powder functional materials, and the pH value of the reaction stock solution is adjusted by using an acid or a base; The fluid is passed into a continuous flow micro-mixing reactor to be fully cut into micron-sized droplets to achieve rapid contact, collision and reaction; After the reaction is completed, the generated solid powder product is filtered and dried to obtain a functional material precursor. The microreactor system includes a rapid heat exchange system and a temperature and pressure monitoring element.

[0022] The micro-mixing reactor is equipped with a tubular reactor or a time-delay pipeline to extend the reaction time. The multiple streams of fluids contain one or more metal salt solutions, alkaline solutions or other reagents that can precipitate them, and undergo a co-precipitation reaction in the micro-mixing reactor, followed by filtration and washing, and then pumped to the tubular reactor for aging or crystallization.

[0023] The multiple fluids contain one or more metal salt solutions, alkaline solutions or other reagents that can cause precipitation, such as one or more of ammonium sulfide, ammonia water, sodium hydroxide, ammonium carbonate, etc., and undergo a co-precipitation reaction in a micro-mixing reactor, and then directly enter a tubular reactor for aging or crystallization.

[0024] The microreactor system includes an ultrasonic reactor to promote precipitation reaction or crystallization aging process. Multiple fluids including one or more metal salt solutions and alkaline solutions are co-precipitated in a micro-mixing reactor and then directly enter a tubular reactor for aging or crystallization. Microwave energy or ultrasonic energy is input during the aging and crystallization process.

[0025] The micro-mixing reactor in the system can be a static mixer, or composed of two moving disks or moving barrels, or composed of a fixed disk or fixed barrel and a moving disk or moving barrel; the multiple fluids therein can also be gas-liquid, oil-water, liquid and suspension, or any combination of the above three.

[0026] The present invention has the following technical effects: The microchannel structure or the moving disk, the moving barrel and the guide groove therein in the mixing chamber of the microreactor of the present invention can cut the fluid material into extremely small droplets, so that the specific surface area of ​​the fluid material is sharply increased, thereby greatly enhancing the mass transfer rate, playing a role in homogenizing the flow field and the nucleation environment, thereby ensuring the consistency of nucleation before crystallization and the uniformity of the concentrations of the precipitant and the target metal ion at various locations; the present invention can not only use the microreactor to deal with the continuous nucleation problem of liquid-liquid reaction, but also can continuously deal with the growth process of the solution after nucleation in the microreactor or pipeline reactor, and has the advantage of a wide range of applications in the synthesis of micro-nano powder functional materials; the present invention can be used for the microreactor nucleation process.

[0027] The details are shown in the following table: Traditional reactor: products and concentrations are constantly changing, and the conditions for nucleus formation are unstable; material concentration is unevenly distributed, resulting in different particle sizes; reaction packages are agglomerated, hard, and have large gaps; trace amounts of raw materials will be encapsulated, resulting in difficult post-processing and a large amount of washing water; intelligent continuous synthesis: material concentration and temperature distribution are uniform, the raw materials are gradually consumed, forming crystals with uniform particle size, small particle size, large surface energy, adsorption agglomeration, adsorption agglomeration: post-processing is easy, and impurities can be controlled.

[0028] Intermittent reactor type: ① Temperature distribution: The specific surface area of ​​the reactor is small, the heat transfer efficiency is low, the temperature gradient is large, the heating rate is slow, and the energy consumption is high. ② Difficult temperature control: The desorption of ions on the surface of iron phosphate particles needs to be carried out in different temperature zones, and different ions require different desorption times. It is difficult to achieve temperature control in the reactor, the process is cumbersome, and the energy consumption is high. ③ Product quality: The product obtained by the reactor is not completely decrystallized, and some impurity ions are still adsorbed on the surface of the crystals.

[0029] Intelligent continuous synthesis: ① Temperature distribution: large specific surface area, high heat transfer efficiency, small temperature gradient, fast reaction temperature rise, and low energy consumption; ② Precise segmented temperature control: According to the different desorption temperatures and desorption times required by different ions, the microchannel can accurately control the reaction temperature and the desorption residence time in different temperature zones, which is easy to operate and has low energy consumption.

[0030] ③ Product quality: The products prepared by microchannel are more completely decrystallized, and there is basically no ion adsorption on the crystal surface.

[0031] A continuous preparation method for high-quality iron phosphate comprises the following steps: Step (1): adding ferrous sulfate heptahydrate produced as a byproduct of titanium dioxide to pure water and stirring to dissolve, maintaining the temperature at 80-85° C., then slowly adding ammonia water or liquid alkali to adjust the pH to 4.0-4.8, and after precipitation and filtration, taking the filtrate and adding dilute acid to adjust the pH to 1.4-2.5 to obtain an iron source solution; Step (2): diluting hydrogen peroxide with pure water to obtain a hydrogen peroxide solution; Step (3): premixing ammonia water and monoammonium phosphate solution or premixing phosphoric acid and liquid caustic soda, and then adding pure water to dilute the premixed mixture to obtain a phosphorus source solution; Step (4): respectively inputting the iron source solution, the hydrogen peroxide solution and the phosphorus source solution into the continuous micro-dynamic reactor by means of a constant flow pump, controlling the reaction temperature at 40 to 60° C., the reaction time at 0.5 to 3 min, and the pH of the reaction solution at 2.1 to 2.5, to synthesize an amorphous iron phosphate slurry; Step (5): rinsing the amorphous ferric phosphate slurry with pure water until the first conductivity is reached; Step (6): adding pure water and phosphoric acid to the rinsed amorphous iron phosphate, stirring and slurrying, controlling the pH of the slurry to 1.3-1.8 and the solid content to 8-25%, and then using a constant flow pump to transport the slurry to a continuous micro-dynamic reactor for aging, controlling the aging temperature to 80-95° C., aging for 1.5-2 hours, to obtain a crystalline iron phosphate slurry; Step (7): rinsing the crystalline ferric phosphate slurry with pure water until the second conductivity is reached; Step (8): drying the rinsed crystalline ferric phosphate at a temperature of 120 to 150° C. for 2 to 4 hours to remove adsorbed water to obtain a dried material; Step (9): calcining the dried material at a temperature of 550-650° C. for 4-6 hours to dehydrate the dried material, thereby obtaining anhydrous ferric phosphate; Step (10): The anhydrous ferric phosphate powder is crushed to obtain high-quality ferric phosphate.

[0032] In step (1), the dilute acid is at least one of sulfuric acid and phosphoric acid.

[0033] In step (1), the iron content in the ferrous sulfate solution is 0.9 to 1.6 mol / L.

[0034] In step (2), the concentration of the hydrogen peroxide solution is 10 to 27.5%.

[0035] In step (3), the concentration of the aqueous ammonia is 10-25%, and the concentration of the monoammonium phosphate solution is 1.5-2.5 mol / L.

[0036] In step (3), the concentration of phosphoric acid is 10-80%, and the concentration of liquid alkali is 5-20%.

[0037] In step (3), the molar ratio of the aqueous ammonia to monoammonium phosphate is 0.3-0.4:1.

[0038] In step (3), the molar ratio of phosphoric acid to liquid alkali is 0.5-0.6:1.

[0039] In step (3), the phosphorus content in the phosphorus source solution is 1.0 to 2.2 mol / L.

[0040] In step (4), the molar ratio of the iron source solution, the hydrogen peroxide solution and the phosphorus source solution is 1:0.55-0.6:0.995-1.05.

[0041] In step (4) and step (6), the continuous micro-dynamic reactor has a special structure inside, as described in the authorized patent CN216573100U.

[0042] In step (5), the first conductivity is <5 mS / cm; in step (7), the second conductivity is <0.3 mS / cm.

[0043] Beneficial effects: The invention has a simple process, fewer steps, small equipment footprint, and low energy consumption, that is, it eliminates the Fe2+ pre-oxidation step, saves sulfuric acid and alkali, avoids the problem of colloid deterioration generated by pre-oxidation during storage, and does not require a special pre-oxidation mixer or storage tank. The invention realizes the synthesis of iron phosphate by three-phase feed control, and completes the oxidation of Fe2+ to Fe in one step. 3+ , Fe 3+ and PO4 3- Combined with the process of generating FePO4•2H2O precipitation, the ferric phosphate has high crystallinity and low water content after aging, which greatly saves the investment in flash evaporation equipment and energy consumption.

[0044] The iron phosphate produced by the present invention has a small particle size and meets industry standards. By controlling the feed ratio of the iron source solution, the hydrogen peroxide solution and the phosphorus source solution, the reaction temperature, the reaction time and the fluid mechanics conditions of the reaction solution, it is avoided that Fe3+ is hydrolyzed to generate Fe(OH)3 colloid due to excessively high temperature, thereby causing agglomeration, and further avoids the problem that the generated iron phosphate stays in the reaction solution for too long, resulting in an increase in particle size and uneven particle size distribution.

[0045] The continuous micro-dynamic reactor uses CN216573100U equipment, which has a specially designed stirring blade inside. It can well control the fluid in a fluid mechanics method similar to plug flow, greatly reducing the back mixing that leads to large iron phosphate particle size and irregular morphology.

[0046] The present invention realizes continuous production of synthesis and aging processes, saves overall production time, has low energy consumption, and has controllable product quality. Rapid production of various types of iron phosphate can be achieved by adjusting process parameters.

[0047] Example 1 A continuous preparation method for high-quality iron phosphate comprises the following steps: Step (1): adding ferrous sulfate produced as a byproduct of titanium dioxide into pure water and stirring to dissolve, maintaining the temperature at 80° C., then slowly adding ammonia water to adjust the pH to 4.2, after precipitation and filtration, adding dilute sulfuric acid to the filtrate to adjust the pH to 2.5, and adding pure water to dilute, to obtain a ferrous sulfate solution with an iron content of 1.5 mol / L; Step (2): preparing a 27.5% hydrogen peroxide solution; Step (3): neutralize 20% ammonia water and 2.5 mol / L monoammonium phosphate at a molar ratio of NH3•H2O:NH4H2PO4=0.35:1, and add pure water to dilute to obtain a phosphorus source solution with a phosphorus content of 2.2 mol / L; Step (4): inputting ferrous sulfate solution, hydrogen peroxide and phosphorus source solution into a continuous micro-dynamic reactor in a molar ratio of 1:0.55:1.02 by a constant flow pump for reaction, and controlling the reaction temperature to 50° C., the reaction time to 2 min, the pH value to 2.2 and kept constant, and obtaining amorphous iron phosphate slurry; Step (5): rinsing the amorphous iron phosphate slurry with pure water until the conductivity is 3.4 mS / cm; Step (6): adding pure water and an appropriate amount of phosphoric acid to the rinsed amorphous iron phosphate, stirring and slurrying, dispersing the slurry to a pH of 1.7 and a solid content of 12%, and then transporting the slurry to a continuous micro-dynamic reactor for aging using a constant flow pump, controlling the aging temperature to 92±1°C and the aging time to 2h, to obtain a crystalline iron phosphate slurry; Step (7): rinsing the crystalline iron phosphate slurry with pure water until the conductivity is 250 μs / cm; Step (8): drying the rinsed crystalline ferric phosphate at 120° C. for 4 h to obtain a dried material; Step (9): placing the dried material in a rotary kiln and calcining it at 550° C. for 5 h to obtain anhydrous ferric phosphate.

[0048] Example 2 Based on Example 1, the difference from Example 1 is that the ammonia water in step (1) is replaced with liquid alkali, and the preparation of the phosphorus source solution in step (3) is changed to neutralizing 10% liquid alkali and 20% phosphoric acid in a molar ratio of H3PO4:NaOH=0.55:1.

[0049] Example 3 Based on Example 1, the difference from Example 1 is that the ratio of NH3•H2O:NH4H2PO4 in step (3) is adjusted to 0.32:1.

[0050] Example 4 Based on Example 1, the difference from Example 1 is that the iron source solution in step (4) is first oxidized with hydrogen peroxide Fe2+:H2O2 at a ratio of 1:0.55 to generate iron sulfate and phosphorus source solution, which are then input into the continuous micro-dynamic reactor for reaction using a constant flow pump at a Fe3+:P molar ratio of 1:1.02.

[0051] Example 5 Based on Example 1, the difference from Example 1 is that the amount of phosphoric acid in step (6) is adjusted so that the pH of the slurry is adjusted to 1.5.

[0052] Example 6 Based on Example 1, the difference from Example 1 is that the aging time is 1.5 hours.

[0053] Comparative Example 1 On the basis of Example 1, the difference from Example 1 is that: the iron source solution, hydrogen peroxide and phosphorus source solution in step (4) are input into a reactor with a stirring speed of 200 r / min in a molar ratio of 1:0.56:1.02 by a constant flow pump for reaction, the reaction temperature is controlled at 50±2°C, and after the addition of the materials, the mixture is kept warm and stirred for 30 minutes; in step (6), an aging kettle is used for aging.

[0054] Comparative Example 2 Based on Example 1, the difference from Example 1 is that: the iron source solution in step (4) is first oxidized with hydrogen peroxide Fe2+:H2O2 at a ratio of 1:0.56, and then the phosphorus source solution is transported to the reactor at a Fe3+:P molar ratio of 1:1.02 by a constant flow pump for reaction; and in step (6), an aging kettle is used for aging.

[0055] Comparative Example 3 Based on Example 1, the difference from Example 1 is that the continuous micro-dynamic reactor in step (6) is replaced by an aging kettle for aging.

[0056] Experimental example: Product effect test The morphology of the anhydrous ferric phosphate prepared in Examples 1-3 and Comparative Example 1 was observed using a scanning electron microscope. Figure 1 , 2 , 3 are SEM images of anhydrous ferric phosphate prepared in Example 1, Example 2, and Example 3, respectively; Figure 4 This is the SEM electron microscope image of the anhydrous ferric phosphate prepared in Comparative Example 1.

[0057] The physical and chemical properties test results of the anhydrous ferric phosphate products obtained in Examples 1 to 6 and Comparative Examples 1 to 3, such as specific surface area and impurity content, are shown in Table 2: It can be seen from Table 2 that in Example 2, the iron source preparation is changed to liquid alkali for impurity removal, and the phosphorus source preparation is changed to phosphoric acid and liquid alkali for neutralization, and the particle size will increase; in Example 3, the ratio of ammonia water to monoammonium phosphate is reduced, which will also lead to an increase in particle size; in Example 4, ferrous sulfate is oxidized before hydrogen peroxide and then reacts with the premixed liquid, and the impurity Mn content is significantly increased; in Example 5, the pH of the aged slurry is reduced, which can shorten the aging time. In Comparative Examples 1 and 2, the intermittent kettle reaction is adopted, the particle size is significantly increased, and the impurities are also significantly increased; in Comparative Example 3, the aging process is changed to aging in an aging kettle, and the specific table is significantly increased.

[0058] The anhydrous iron phosphate powders prepared in the above Examples 1 to 3 and Comparative Example 1 were used to prepare lithium iron phosphate under the same conditions. The compaction density and electrical properties of the prepared lithium iron phosphate were tested. The results are shown in Table 3 below: It can be seen from Table 3 that the compaction density and electrical properties of lithium iron phosphate synthesized by using iron phosphate prepared by Examples 1 to 3 of the present invention are excellent, and are better than the traditional autoclave process of Comparative Example 1, which shows that the iron phosphate prepared by the scheme of the present invention has good application prospects in the field of lithium battery preparation.

Claims

1. A homogeneous crystal reaction system for continuously preparing functional powder materials, characterized in that: The homogeneous crystal reaction system includes a constant flow pump for conveying each reaction raw material liquid for controlling the material liquid conveying amount and monitoring the pipeline pressure; a micro-mixing reactor for powder material nucleation and homogeneous crystal mixing reaction and a micro-channel aging device for aging micro-nano materials; The system also includes a detection device for detecting reaction parameters; and a collection, filtering and washing device for collecting reaction products.

2. A homogeneous crystal reaction system for continuously preparing functional powder materials according to claim 1, characterized in that: The microchannel aging device is a microwave reactor or an ultrasonic reactor or a multi-layer stirring pipeline.

3. The homogeneous crystal reaction system for continuously preparing functional powder materials according to claim 1, characterized in that: The reaction parameters detected by the detection device include temperature data, pressure data, pH value data, dielectric data, conductivity data and nano-morphology monitoring data.

4. A homogeneous crystal reaction system for continuously preparing functional powder materials according to claim 1, 2 or 3, characterized in that: The system also includes: a rapid heat exchange system and a temperature and pressure monitoring element.

5. A homogeneous crystal reaction system for continuously preparing functional powder materials according to claim 4, characterized in that: The micro-mixing reactor is also provided with a tubular reactor or a time-delay pipeline.

6. A method for continuously preparing a homogeneous crystal reaction system of functional powder materials, characterized in that: The method comprises the following steps: Step 1: preparing at least two reaction fluids for preparing powder functional materials, and adjusting the pH value of the reaction stock solution corresponding to the fluids with an acid or a base; Step 2: passing the fluid into a continuous flow homogeneous crystal mixing reactor to cut it into micron-sized droplets to achieve rapid contact, collision and reaction; Step 3: After the reaction is completed, the generated solid powder product is filtered and dried to obtain a functional material precursor.

7. The method for continuously preparing a homogeneous crystal reaction system of functional powder materials according to claim 6, characterized in that: The reaction fluid contains one or more metal salt solutions, alkaline solutions or reagents that can precipitate the reaction fluid, and undergoes a co-precipitation reaction in a micro-mixing reactor, followed by filtration and washing, and then pumped into a tubular reactor for aging or crystallization.

8. The method for continuously preparing a homogeneous crystal reaction system of functional powder materials according to claim 7, characterized in that: The reagent capable of precipitating the reaction fluid is one or more combinations of ammonium sulfide, ammonia water, sodium hydroxide and ammonium carbonate.

9. The method for continuously preparing a homogeneous crystal reaction system of functional powder materials according to claim 6, characterized in that: The reaction fluid is gas-liquid or oil-water or liquid suspension.

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