Preparation method of titanium dioxide for lithium battery
By using new environmentally friendly solvents, innovative additives, step-by-step reaction technology and dynamic reaction monitoring system in the preparation method for lithium batteries, the problems of high production costs, operation complexity and product quality fluctuations in the existing technology are solved, and high-quality and low-cost titanium dioxide preparation is achieved.
Patent Information
- Application Number
- CN202411691094.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-25
- Publication Date
- 2025-03-11
AI Technical Summary
The existing titanium dioxide preparation method for lithium batteries has problems of high production costs, operational complexity and product quality fluctuations, especially during large-scale production.
A solvent system with a new environmentally friendly solvent mixed with aqueous phase, innovative additives, step-by-step reaction technology and dynamic reaction monitoring system, modified titanium source and efficient addition method, efficient cleaning and low-temperature freeze-drying technology, and process standardization process.
The crystal quality and purity of titanium dioxide are improved, the reaction conditions are optimized, the production costs are reduced, the product consistency and high quality are ensured, and it is suitable for industrial production.
Smart Images

Figure FDA0005150971060000011 
Figure FDA0005150971060000012 
Figure FDA0005150971060000021
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of lithium battery production, and in particular to a method for preparing titanium dioxide for lithium batteries. Background Art
[0002] In modern lithium battery technology, titanium dioxide (TiO2) is an important electrode material and is widely used in lithium-ion batteries. Titanium dioxide has excellent chemical stability, high theoretical capacity, high operating voltage (about 1.7V to Li / Li+) and long cycle life, making it an ideal negative electrode material for lithium batteries. At the same time, titanium dioxide can be used as a coating on the surface of the positive electrode material to improve the structural stability and cycle performance of the positive electrode material, and can be used as a template or additive to synthesize high-performance lithium battery positive electrode materials. In order to further improve the performance of titanium dioxide in batteries, researchers are committed to improving its preparation method to obtain higher quality and purer titanium dioxide.
[0003] After searching, application number CN202311256690.2 discloses a method for preparing titanium dioxide for lithium batteries, and the steps are as follows: add deionized water to a beaker containing an organic solvent, and then add a mixture of lysine and urea under stirring conditions, and add a titanium source dropwise and continue stirring. After 30-60 minutes, transfer it to a reactor for hydrothermal reaction, take it out after 5-8 hours and naturally cool it to room temperature, filter it, and wash it with anhydrous ethanol and deionized water for 2-3 times respectively, and dry it at 70°C for 10 hours to obtain titanium dioxide; the titanium dioxide prepared by the method of the present invention is a three-dimensional flower ball structure, which has a large specific surface area and a stable porous structure. It can not only effectively maintain the structural integrity of the material during the insertion and extraction of lithium ions, but also effectively improve its ion conductivity and electrical conductivity. After it is made into a lithium battery electrode, it has high charge and discharge efficiency and cycle stability, and the battery capacity is also significantly improved.
[0004] However, the inventors have discovered that the prior art still has the following defects:
[0005] The organic solvents, lysine, urea and other materials used in the method and the complex hydrothermal reaction steps increase the production cost and operational complexity, especially in large-scale production, the economic burden is heavy. The temperature and time in the hydrothermal reaction have a significant impact on the product quality, but the prior art does not provide optimized reaction parameters, which may lead to fluctuations in product quality and difficulty in control during the production process.
[0006] To this end, we propose a method for preparing titanium dioxide for lithium batteries. Summary of the invention
[0007] The present invention mainly solves the technical problems existing in the above-mentioned prior art and provides a method for preparing titanium dioxide for lithium batteries.
[0008] In order to achieve the above object, the present invention adopts the following technical scheme, a method for preparing titanium dioxide for lithium battery, comprising the following steps:
[0009] Step 1: using a solvent system in which a new environmentally friendly solvent is mixed with water in the reaction system;
[0010] Step 2: Introducing innovative additives into the reaction to improve the crystal quality of titanium dioxide;
[0011] Step 3: Use step-by-step reaction technology and dynamic reaction monitoring system to precisely control reaction conditions;
[0012] Step 4: Use modified titanium source and efficient addition method;
[0013] Step 5: Implement high-efficiency cleaning and low-temperature freeze-drying technology;
[0014] Step 6: Develop standardized process flow and conduct large-scale verification.
[0015] Preferably, the ratio of the novel environmentally friendly solvent to water is 1:(10-20), and comprises a combination of a green organic solvent and water;
[0016] The specific solvent selection and ratio are as follows: select a solvent system that is a mixture of green organic solvent and water, and set the volume of the environmentally friendly solvent to V s (Unit: ml), the volume of water is V w (Unit: ml), the volume ratio of the two is 1:(10 to 20), the set ratio is R, where the value range of R is 10 to 20, and the ratio relationship is as follows: Combined with the value range of ratio R, we get:
[0017] Preferably, the mixing process mixes the environmentally friendly solvent and water according to a calculated ratio to ensure sufficient mixing to form a uniform solvent system. The mixing process includes the following steps:
[0018] Use a stirrer or ultrasonic mixer for mixing, and use linear regression or polynomial regression method to analyze the effect of different ratios R on the quality of titanium dioxide. The formula is as follows: Y=β0+β1R+ò, where Y is the quality index of titanium dioxide, β0 and β1 are regression coefficients, and ò is the error term. Select the ratio R with the best performance in the regression analysis and apply it in production. After determining the optimal ratio, conduct verification experiments to ensure the stability and repeatability of the production process, and adjust the production parameters to maintain the stability of the selected ratio.
[0019] Preferably, the innovative auxiliary agent is a functionalized polymer material or a nano-scale catalyst, the polymer material is specifically polyethyleneimine (PEI) or polyvinyl alcohol (PVA), and its functionalized form can enhance the stability of the titanium source and improve the crystallization quality of titanium dioxide, and the nano-scale catalyst is specifically nano-molybdenum sulfide (MoS2) or nano-alumina (Al2O3), which can improve the reaction rate and the purity of titanium dioxide;
[0020] The amount of functional polymer material added is calculated as follows:
[0021] Set the concentration of functionalized polymer material to C f (Unit: grams per liter), the amount added to the reaction system is V f (Unit: ml), in the reaction system, the total mass of the functionalized polymer material is: M f =C f ×V f ;
[0022] The amount of nano-scale catalyst added is calculated as follows:
[0023] Set the concentration of nanocatalyst to C c (Unit: grams per liter), the amount added to the reaction system is V c (Unit: ml), the total mass of the nanocatalyst is: M c =C c ×V c .
[0024] Preferably, the stepwise reaction technique comprises a low-temperature pre-reaction and a high-temperature main reaction;
[0025] The low-temperature pre-reaction is specifically: pre-reaction is carried out under low-temperature conditions to promote the initial reaction of the reactants. The temperature of the low-temperature pre-reaction is set to T1 (unit: °C), the reaction time is t1 (unit: hour), and the reaction rate r1 is expressed by the following formula: Among them, k r1 is the reaction rate constant at low temperature, C s is the concentration of reactants, n is the reaction order;
[0026] The high-temperature main reaction is specifically as follows: after the pre-reaction, the temperature is raised to carry out the main reaction to promote the final synthesis of titanium dioxide. The temperature of the main reaction is set to T2 (unit: °C), the reaction time is t2 (unit: hour), and the reaction rate r2 is expressed by the following formula: Among them, k r2 is the reaction rate constant at high temperature, C s is the concentration of reactants, m is the reaction order of the main reaction;
[0027] The total reaction time t of the low-temperature pre-reaction and the high-temperature main reaction is calculated by integrationtotal :t total =t1+t2.
[0028] Preferably, the dynamic reaction monitoring system uses a high-precision sensor to monitor the reaction temperature T(t) and the reactant concentration C in real time. s (t), the monitoring system collects data through the following formula:
[0029] T(t)=T0+ΔT·sin(ωt),C s (t) = C s0 ·e -k·t , where T0 is the initial temperature, ΔT is the temperature fluctuation amplitude, ω is the fluctuation frequency, C s0 is the initial concentration, k is the decay constant;
[0030] The reaction conditions are adjusted based on real-time data, and the reaction rate is optimized using a feedback control algorithm based on a proportional-integral-derivative (PID) controller: Among them, u(t) is the control input, e(t) is the error, K p ,K i ,K d are the proportional, integral and derivative gains respectively.
[0031] Preferably, the step 4: using a modified titanium source and an efficient addition method, the specific steps are as follows:
[0032] Select modified titanium source, specifically, chemically modify the surface of titanate to increase its reactivity and stability. The modifier reacts with the titanium source to form a modified product of the titanium source, thereby enhancing the reactivity of the titanium source. A dynamic reaction monitoring system is used to monitor the reaction conditions during the modification process in real time. In the reaction, efficient addition methods are used, including batch addition and continuous addition, to improve the reaction efficiency and product quality.
[0033] Sensors are used to monitor the concentration of the titanium source in the reaction in real time and perform feedback control. The monitoring data is used to adjust the addition method through a control algorithm to optimize the reaction conditions. Under the optimized modified titanium source and efficient addition method, large-scale experiments are carried out to verify product quality and reaction efficiency.
[0034] Preferably, in step 5: implementing high-efficiency cleaning and low-temperature freeze-drying technology to improve the purity and quality of titanium dioxide:
[0035] Efficient cleaning specifically includes: the cleaning solution needs to be accurately prepared, the cleaning solution includes deionized water and detergent, the concentration of the detergent should be 5% to 10% (volume ratio), the cleaning process is divided into three steps: pre-wash, main wash and rinse. Deionized water is used for the pre-wash stage, and the time is set to 5 to 10 minutes. The detergent solution is used in the main wash stage, and the time is set to 15 to 30 minutes. Deionized water is used in the rinse stage, and the time is set to 10 minutes;
[0036] Low-temperature freeze drying is specifically divided into two stages: freezing and sublimation drying. In the freezing stage, the cleaned sample is quickly cooled to -40°C to freeze the water in the sample. The freezing time is set to 4 to 6 hours. Then it enters the sublimation drying stage, and the sample is placed in a low-pressure environment of 0.1 to 1 torr and heated to -10°C to -20°C, so that the ice is directly sublimated into gas. The sublimation drying time is set to 12 to 24 hours.
[0037] Preferably, the process standardization process includes detailed operating procedures and large-scale verification.
[0038] Beneficial Effects
[0039] The present invention provides a method for preparing titanium dioxide for lithium batteries, which has the following beneficial effects:
[0040] (1) The method for preparing titanium dioxide for lithium batteries can optimize the reaction system and improve the crystal quality of titanium dioxide by using a solvent system of a new environmentally friendly solvent mixed with water. The innovative additives can increase the reaction rate and the purity of titanium dioxide, thereby improving the performance of the final product. The titanium dioxide prepared by this method has uniform particle size, high purity and good dispersion.
[0041] (2) This method for preparing titanium dioxide for lithium batteries uses a step-by-step reaction technology (low-temperature pre-reaction and high-temperature main reaction) and a dynamic reaction monitoring system (including real-time monitoring of temperature and concentration changes), which can accurately control the reaction conditions and improve the controllability and stability of the reaction. The use of a dynamic reaction monitoring system and a feedback control algorithm (such as a PID controller) can adjust the reaction conditions in real time, optimize the reaction rate, and ensure the consistency and high quality of the product.
[0042] (3) The preparation method of titanium dioxide for lithium batteries, the application of modified titanium source and efficient addition method can improve reaction efficiency, reduce production time, and improve the consistency and quality of the final product. Through process standardization and large-scale verification, the stability and repeatability of the production process can be ensured, which is convenient for industrial production and large-scale application.
[0043] (4) The preparation method of titanium dioxide for lithium batteries, the high-efficiency cleaning and low-temperature freeze-drying technology help to remove impurities and improve the purity of titanium dioxide, ensuring the quality of the final product. Precisely controlled cleaning and drying parameters (such as cleaning solution concentration, cleaning time, freezing temperature and sublimation drying time) can effectively remove residues in the sample and improve the stability and performance of the product. DETAILED DESCRIPTION
[0044] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0045] Embodiment: A method for preparing titanium dioxide for lithium battery comprises the following steps:
[0046] Step 1: using a solvent system in which a new environmentally friendly solvent is mixed with water in the reaction system;
[0047] Step 2: Introducing innovative additives into the reaction to improve the crystal quality of titanium dioxide;
[0048] Step 3: Use step-by-step reaction technology and dynamic reaction monitoring system to precisely control reaction conditions;
[0049] Step 4: Use modified titanium source and efficient addition method;
[0050] Step 5: Implement high-efficiency cleaning and low-temperature freeze-drying technology;
[0051] Step 6: Develop standardized process flow and conduct large-scale verification.
[0052] Further, the ratio of the novel environmentally friendly solvent to water is 1:(10-20), and comprises a combination of a green organic solvent and water;
[0053] The specific solvent selection and ratio are as follows: select a solvent system that is a mixture of green organic solvent and water, and set the volume of the environmentally friendly solvent to V s (Unit: ml), the volume of water is V w (Unit: ml), the volume ratio of the two is 1:(10 to 20), the set ratio is R, where the value range of R is 10 to 20. The ratio relationship is as follows: Combined with the value range of ratio R, we get:
[0054] The specific volume ratio steps are as follows: Set the required environmentally friendly solvent volume V s is 100mL, calculate the water volume V according to the ratio Rw , for R = 10: V w =10×V s =10×100=1000mL, for R=20:V w =20×V s =20×100=2000mL, therefore, for an environmentally friendly solvent volume of 100mL, the water volume is controlled between 1000mL and 2000mL.
[0055] Furthermore, the mixing process mixes the environmentally friendly solvent and water according to a calculated ratio to ensure sufficient mixing to form a uniform solvent system. The mixing process includes the following steps:
[0056] Use a stirrer or ultrasonic mixer for mixing, and use linear regression or polynomial regression method to analyze the effect of different ratios R on the quality of titanium dioxide. The formula is as follows: Y=β0+β1R+ò, where Y is the quality index of titanium dioxide, β0 and β1 are regression coefficients, and ò is the error term. Select the ratio R with the best performance in the regression analysis and apply it in production. After determining the optimal ratio, conduct verification experiments to ensure the stability and repeatability of the production process, and adjust the production parameters to maintain the stability of the selected ratio.
[0057] Furthermore, the innovative auxiliary agent is a functionalized polymer material or a nano-scale catalyst, the polymer material is specifically polyethyleneimine (PEI) or polyvinyl alcohol (PVA), and its functionalized form can enhance the stability of the titanium source and improve the crystallization quality of titanium dioxide, and the nano-scale catalyst is specifically nano-molybdenum sulfide (MoS2) or nano-alumina (Al2O3), which can increase the reaction rate and the purity of titanium dioxide;
[0058] The amount of functional polymer material added is calculated as follows:
[0059] Set the concentration of functionalized polymer material to C f (Unit: grams per liter), the amount added to the reaction system is V f (Unit: ml), in the reaction system, the total mass of the functionalized polymer material is: M f =C f ×V f ;
[0060] The amount of nano-scale catalyst added is calculated as follows:
[0061] Set the concentration of nanocatalyst to C c (Unit: grams per liter), the amount added to the reaction system is V c (Unit: ml), the total mass of the nanocatalyst is: M c =C c ×V c ;
[0062] In the experiment, multiple addition amounts were selected for comparison to optimize the concentration and amount of additives. Taking polymer materials as an example, the following experiments were conducted:
[0063] Low concentration experiment: Set C f 0.1g / L, V f is 10mL.
[0064] Medium concentration experiment: Set C f 0.5g / L, V f is 20mL.
[0065] High concentration experiment: Set C f 1.0g / L, V f is 30mL.
[0066] For each addition amount, the crystal quality indicators of titanium dioxide, such as grain size (d) and crystallinity (β), were recorded. Statistical methods were used to analyze the effect of different addition amounts on crystal quality:
[0067] Where d is the grain size, β is the crystallinity, and k is a constant.
[0068] Optimization of reaction conditions
[0069] Combined with the optimal amount of additives, optimize the reaction conditions. Set the reaction temperature to T (unit: °C) and the reaction time to t (unit: hours). Perform the following calculations to optimize the conditions:
[0070] Reaction rate: Set the reaction rate constant to k r , the reaction rate r is expressed as:
[0071] Among them, C s is the titanium source concentration, and n is the reaction order.
[0072] Optimum temperature: Calculate the optimal reaction temperature using the Arrhenius equation:
[0073] Among them, A is the pre-factor, E a is the activation energy, R is the gas constant, and T is the absolute temperature.
[0074] Effect verification and adjustment
[0075] Implement the optimized reaction conditions and conduct large-scale experiments to verify the improvement in crystal quality. By analyzing the experimental results, adjust the type and amount of additives to ensure the desired effect. Use a microscope to observe the morphology of titanium dioxide crystals to confirm their quality improvement.
[0076] Through the above steps, the amount of additives added and the reaction conditions can be systematically optimized to ensure that the quality of titanium dioxide crystals meets the expected standards.
[0077] Further, the stepwise reaction technique includes a low-temperature pre-reaction and a high-temperature main reaction;
[0078] The low-temperature pre-reaction is specifically: pre-reaction is carried out under low-temperature conditions to promote the initial reaction of the reactants. The temperature of the low-temperature pre-reaction is set to T1 (unit: °C), the reaction time is t1 (unit: hour), and the reaction rate r1 is expressed by the following formula: Among them, k r1 is the reaction rate constant at low temperature, C s is the concentration of reactants, n is the reaction order;
[0079] The high-temperature main reaction is specifically as follows: after the pre-reaction, the temperature is raised to carry out the main reaction to promote the final synthesis of titanium dioxide. The temperature of the main reaction is set to T2 (unit: °C), the reaction time is t2 (unit: hour), and the reaction rate r2 is expressed by the following formula: Among them, k r2 is the reaction rate constant at high temperature, C s is the concentration of reactants, m is the reaction order of the main reaction;
[0080] The total reaction time t of the low-temperature pre-reaction and the high-temperature main reaction is calculated by integration total :t total =t1+t2.
[0081] Furthermore, the dynamic reaction monitoring system uses high-precision sensors to monitor the reaction temperature T(t) and the reactant concentration C in real time. s (t), the monitoring system collects data through the following formula:
[0082] T(t)=T0+ΔT·sin(ωt),C s (t) = C s0 ·e -k·t , where T0 is the initial temperature, ΔT is the temperature fluctuation amplitude, ω is the fluctuation frequency, C s0 is the initial concentration, k is the decay constant;
[0083] The reaction conditions are adjusted based on real-time data, and the reaction rate is optimized using a feedback control algorithm based on a proportional-integral-derivative (PID) controller: Among them, u(t) is the control input, e(t) is the error, K p ,K i ,K d are proportional, integral and derivative gains respectively;
[0084] Through experimental data analysis, the temperature and time of low-temperature pre-reaction and high-temperature main reaction are optimized to ensure the best reaction effect. Statistical methods are used to analyze the effects of different conditions on the quality of titanium dioxide crystals, such as:
[0085] Response effect evaluation: The response effect was evaluated using the following indicators: The optimization scheme is to use response surface methodology to analyze the effect index under different reaction conditions in order to select the best reaction conditions.
[0086] Verification experiment: Carry out large-scale verification experiments under optimized conditions to ensure the stability and repeatability of the set step-by-step reaction technology and dynamic reaction monitoring system.
[0087] Implement adjustments: Adjust operating parameters based on validation results to maintain optimal production conditions and ensure high-quality TiO2 production.
[0088] Through the above steps, the step-by-step reaction technology and dynamic reaction monitoring system can be systematically implemented to accurately control the reaction conditions and improve the production efficiency and quality of titanium dioxide.
[0089] Furthermore, the step 4: using a modified titanium source and an efficient addition method, the specific steps are as follows:
[0090] Select modified titanium source, specifically, chemically modify the surface of titanate to increase its reactivity and stability. The modifier reacts with the titanium source to form a modified product of the titanium source, thereby enhancing the reactivity of the titanium source. A dynamic reaction monitoring system is used to monitor the reaction conditions during the modification process in real time. In the reaction, efficient addition methods are used, including batch addition and continuous addition, to improve the reaction efficiency and product quality.
[0091] Sensors are used to monitor the concentration of the titanium source in the reaction in real time and perform feedback control. The monitoring data is used to adjust the addition method through a control algorithm to optimize the reaction conditions. Under the optimized modified titanium source and efficient addition method, large-scale experiments are carried out to verify product quality and reaction efficiency.
[0092] Furthermore, in step 6: implementing efficient cleaning and low-temperature freeze-drying technology to improve the purity and quality of titanium dioxide:
[0093] Efficient cleaning specifically requires: the cleaning solution needs to be accurately prepared, the cleaning solution includes deionized water and detergent, the concentration of the detergent should be 5% to 10% (volume ratio), and the cleaning process is divided into three steps: pre-wash, main wash and rinse. Deionized water is used for the pre-wash stage, and the time is set to 5 to 10 minutes. The detergent solution is used in the main wash stage, and the time is set to 15 to 30 minutes. Deionized water is used in the rinse stage, and the time is set to 10 minutes;
[0094] Low-temperature freeze drying is specifically divided into two stages: freezing and sublimation drying. In the freezing stage, the cleaned sample is quickly cooled to -40°C to freeze the water in the sample. The freezing time is set to 4 to 6 hours. Then it enters the sublimation drying stage, and the sample is placed in a low-pressure environment of 0.1 to 1 torr and heated to -10°C to -20°C, so that the ice is directly sublimated into gas. The sublimation drying time is set to 12 to 24 hours.
[0095] Furthermore, the process standardization process includes detailed operating procedures and large-scale verification.
[0096] Implementation cases and data comparison:
[0097] According to the above technical scheme, rutile titanium dioxide with product model RP500 is prepared. The parameters of RP-500 technology are titanium oxide content (%)>94, inorganic treatment using Al2O3 or SiO2, L* value≥98, tinting power (TCS)≥2000, base color (SCX≥3.8, oil absorption (g / 100g)≤20, its particle size (μmm) is 0.22, and density (g / ml)≈4.1.
[0098] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.
Claims
1. A method for preparing titanium dioxide for lithium batteries, characterized in that: The following steps are involved: Step 1: using a solvent system in which a new environmentally friendly solvent is mixed with water in the reaction system; Step 2: Introducing innovative additives into the reaction to improve the crystal quality of titanium dioxide; Step 3: Use step-by-step reaction technology and dynamic reaction monitoring system to precisely control reaction conditions; Step 4: Use modified titanium source and efficient addition method; Step 5: Implement high-efficiency cleaning and low-temperature freeze-drying technology; Step 6: Develop standardized process flow and conduct large-scale verification.
2. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: The ratio of the novel environmentally friendly solvent to water is 1:(10-20), and comprises a combination of a green organic solvent and water; The specific solvent selection and ratio are as follows: select a solvent system that is a mixture of green organic solvent and water, and set the volume of the environmentally friendly solvent to V s (Unit: ml), the volume of water is V w (Unit: ml), the volume ratio of the two is 1:(10 to 20), the set ratio is R, where the value range of R is 10 to 20, and the ratio relationship is as follows: Combined with the value range of ratio R, we get:
3. The method for preparing titanium dioxide for lithium battery according to claim 2, characterized in that: The mixing process mixes the environmentally friendly solvent and water according to the calculated ratio to ensure that they are fully mixed to form a uniform solvent system. The following steps are involved: Use a stirrer or ultrasonic mixer for mixing, and use linear regression or polynomial regression method to analyze the effect of different ratios R on the quality of titanium dioxide. The formula is as follows: Y=β0+β1R+ò, where Y is the quality index of titanium dioxide, β0 and β1 are regression coefficients, and ò is the error term. Select the ratio R with the best performance in the regression analysis and apply it in production. After determining the optimal ratio, conduct verification experiments to ensure the stability and repeatability of the production process, and adjust the production parameters to maintain the stability of the selected ratio.
4. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: The innovative auxiliary agent is a functionalized polymer material or a nano-scale catalyst. The polymer material is specifically polyethyleneimine (PEI) or polyvinyl alcohol (PVA), and its functionalized form can enhance the stability of the titanium source and improve the crystallization quality of titanium dioxide. The nano-scale catalyst is specifically nano-molybdenum sulfide (MoS2) or nano-alumina (Al2O3), which can increase the reaction rate and the purity of titanium dioxide. The amount of functional polymer material added is calculated as follows: Set the concentration of functionalized polymer material to C f (Unit: grams per liter), the amount added to the reaction system is V f (Unit: ml), in the reaction system, the total mass of the functionalized polymer material is: M f =C f ×V f ; The amount of nano-scale catalyst added is calculated as follows: Set the concentration of nanocatalyst to C c (Unit: grams per liter), the amount added to the reaction system is V c (Unit: ml), the total mass of the nanocatalyst is: M c =C c ×V c .
5. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: The step-by-step reaction technology includes a low-temperature pre-reaction and a high-temperature main reaction; The low-temperature pre-reaction is specifically: pre-reaction is carried out under low-temperature conditions to promote the initial reaction of the reactants. The temperature of the low-temperature pre-reaction is set to T1 (unit: °C), the reaction time is t1 (unit: hour), and the reaction rate r1 is expressed by the following formula: Among them, k r1 is the reaction rate constant at low temperature, C s is the concentration of reactants, n is the reaction order; The high-temperature main reaction is specifically as follows: after the pre-reaction, the temperature is raised to carry out the main reaction to promote the final synthesis of titanium dioxide. The temperature of the main reaction is set to T2 (unit: °C), the reaction time is t2 (unit: hour), and the reaction rate r2 is expressed by the following formula: Among them, k r2 is the reaction rate constant at high temperature, C s is the concentration of reactants, m is the reaction order of the main reaction; The total reaction time t of the low-temperature pre-reaction and the high-temperature main reaction is calculated by integration total :t total =t1+t2.
6. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: The dynamic reaction monitoring system uses high-precision sensors to monitor the reaction temperature T(t) and reactant concentration C in real time. s (t), the monitoring system collects data through the following formula: T(t)=T0+ΔT·sin(ωt),C s (t) = C s0 ·e -k·t , where T0 is the initial temperature, ΔT is the temperature fluctuation amplitude, ω is the fluctuation frequency, C s0 is the initial concentration, k is the decay constant; The reaction conditions are adjusted based on real-time data, and the reaction rate is optimized using a feedback control algorithm based on a proportional-integral-derivative (PID) controller: Among them, u(t) is the control input, e(t) is the error, K p ,K i ,K d are the proportional, integral and derivative gains respectively.
7. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: The fourth step: using a modified titanium source and an efficient addition method, the specific steps are as follows: Select modified titanium source, specifically, chemically modify the surface of titanate to increase its reactivity and stability. The modifier reacts with the titanium source to form a modified product of the titanium source, thereby enhancing the reactivity of the titanium source. A dynamic reaction monitoring system is used to monitor the reaction conditions during the modification process in real time. In the reaction, efficient addition methods are used, including batch addition and continuous addition, to improve the reaction efficiency and product quality. Sensors are used to monitor the concentration of the titanium source in the reaction in real time and perform feedback control. The monitoring data is used to adjust the addition method through a control algorithm to optimize the reaction conditions. Under the optimized modified titanium source and efficient addition method, large-scale experiments are carried out to verify product quality and reaction efficiency.
8. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: Step 5: Implementing high-efficiency cleaning and low-temperature freeze-drying technology to improve the purity and quality of titanium dioxide: Efficient cleaning specifically includes: the cleaning solution needs to be accurately prepared, the cleaning solution includes deionized water and detergent, the concentration of the detergent should be 5% to 10% (volume ratio), the cleaning process is divided into three steps: pre-wash, main wash and rinse. Deionized water is used for the pre-wash stage, and the time is set to 5 to 10 minutes. The detergent solution is used in the main wash stage, and the time is set to 15 to 30 minutes. Deionized water is used in the rinse stage, and the time is set to 10 minutes; Low-temperature freeze drying is specifically divided into two stages: freezing and sublimation drying. In the freezing stage, the cleaned sample is quickly cooled to -40°C to freeze the water in the sample. The freezing time is set to 4 to 6 hours. Then it enters the sublimation drying stage, and the sample is placed in a low-pressure environment of 0.1 to 1 torr and heated to -10°C to -20°C, so that the ice is directly sublimated into gas. The sublimation drying time is set to 12 to 24 hours.
9. The method for preparing titanium dioxide for lithium battery according to claim 1, characterized in that: The process standardization process includes detailed operating procedures and large-scale validation.
Citation Information
Patent Citations
Preparation method of titanium dioxide for lithium battery
CN117317207A
Cited By
Preparation method of ORR reaction catalyst
CN120261608A