Preparation method of rate type lithium iron phosphate
A technology of lithium iron phosphate and rate, which is applied in the field of preparation of rate-type lithium iron phosphate, can solve the problems of incapable of large-scale industrialization, high energy consumption, and high degree of automation, and achieve the goal of increasing mileage, low energy consumption, and environment optimization Effect
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[0033] The invention discloses a preparation method of rate type lithium iron phosphate, comprising the following steps:
[0034] Adding carbon source and phosphorus iron source into deionized water for mixed reaction to obtain slurry A;
[0035] Add lithium source and additives to the slurry A, and use mechanical stirring and self-circulation system to run together for 3-5 hours to form slurry B. During the operation, the reaction temperature is controlled at 25-41 ° C. The viscosity of the slurry B The control range does not exceed 180mPa·S, preferably 50-180mPa·S;
[0036] Grinding the slurry B to a nano-sized slurry C by a sand mill system;
[0037] Removing the moisture of the slurry C by dynamic drying to obtain the material D;
[0038] The material D is crystallized by six-stage sintering in a protective atmosphere to obtain a sintered material. The protective atmosphere is nitrogen or an inert gas. It can be understood that the inert gas here is conventionally used i...
Embodiment 1
[0053] Glucose and ferric phosphate are added to deionized water according to the mass fraction of carbon source: phosphorus and iron source being 10%, and mixed to prepare slurry A;
[0054] Add lithium carbonate and tetrabutyl titanate (1000ppm) into the slurry A according to the molar ratio Li / Fe=1.035, mechanically stir and run the self-circulation system together for 3 hours to form a uniformly mixed slurry B. The temperature of the reaction process is controlled at 25-41 °C, the viscosity control range of slurry B does not exceed 180mPa·s;
[0055] Grind slurry B to D50 = 0.35 μm slurry C through a sand mill system;
[0056] After the slurry C is spray-dried, the water content of the material is removed to reach the particle size range of D50=8μm;
[0057] The six heating times of the dried material are: 230°C for the first stage, 250°C for the second stage, 450°C for the third stage, 580°C for the fourth stage, 580°C for the fifth stage, and 680°C for the sixth stage. ...
Embodiment 2
[0062] Glucose and ferric phosphate are added to deionized water according to the mass fraction of carbon source: phosphorus and iron source being 11%, and mixed to prepare slurry A;
[0063] According to the molar ratio Li / Fe=1.035, add lithium carbonate + lithium hydroxide composite lithium salt and titanium dioxide (5000ppm) into the slurry A for mechanical stirring and self-circulation system to run together for 3 hours to form a uniformly mixed slurry B, and the temperature of the reaction process is controlled At 25-41°C, the viscosity control range of slurry B does not exceed 180mPa·s;
[0064] Grind slurry B to D50 = 0.3 μm slurry C through a sand milling system;
[0065] After the slurry C is spray-dried, the water content of the material is removed to reach the particle size range of D50=7.5 μm;
[0066] The six heating times of the dried material are: 230°C for the first stage, 250°C for the second stage, 450°C for the third stage, 580°C for the fourth stage, 580°C...
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