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Continuous reactor for synthesizing high-crystallinity nanoscale solid electrolyte precursor and synthesis method

A solid-state electrolyte and high crystallinity technology, applied in chemical/physical/physicochemical fixed reactors, chemical instruments and methods, electrochemical generators, etc., can solve batches that are not suitable for industrial mass production and hydrothermal reduction methods The problem of small amount and large particle size of the material can be solved, and the particle size of the product is fine and uniform, the synthesis method is time-saving, and the effect of high energy density is achieved.

Pending Publication Date: 2022-05-06
瑟瑞米(洛阳)新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The batch size of the hydrothermal reduction method is too small to be suitable for industrial mass production; the material obtained by the solid-state sintering method has a large particle size and poor uniformity, and it is difficult to match the electrode material when assembling the battery because of stoichiometry and heating. The temperature is difficult to control; the production time of the sol-gel method is too long, and the requirements for the pH control and temperature control of the system are strict, and the existing equipment is difficult to meet

Method used

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  • Continuous reactor for synthesizing high-crystallinity nanoscale solid electrolyte precursor and synthesis method
  • Continuous reactor for synthesizing high-crystallinity nanoscale solid electrolyte precursor and synthesis method
  • Continuous reactor for synthesizing high-crystallinity nanoscale solid electrolyte precursor and synthesis method

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Embodiment 1

[0049] refer to figure 1 , this embodiment provides a continuous reactor for synthesizing a highly crystalline nanoscale solid electrolyte precursor, the continuous reactor 1 includes a reactor body 11;

[0050] The reactor body 11 is provided with a stirring device 12, a heating device 15 and a charging controller 16; wherein,

[0051] The stirring device 12 is used to stir the reaction materials;

[0052] The heating device 15 is used to change the temperature in the reaction process;

[0053] The feed controller 16 is used to add reaction materials;

[0054] The reaction kettle body 11 also includes a temperature sensor 13 and a pH sensor 14, wherein,

[0055] The temperature sensor 13 is arranged inside the reactor body 11 and is electrically connected to the heating device 15 for detecting the reaction temperature and controlling the opening and closing of the heating device 15;

[0056] The pH sensor 14 is arranged inside the reactor body 11 and is electrically conne...

Embodiment 2

[0058] On the basis of Example 1, as an optional implementation, refer to figure 2 , the outside of the reaction kettle body 11 is wrapped with a cooling liquid interlayer 111, and the cooling liquid interlayer 111 can be filled with cooling liquid; the cooling liquid interlayer 111 is communicated with a cooling inlet 112 and a cooling outlet 113, and the cooling inlet 112 is located in the The cooling liquid interlayer 111 is at the bottom, and the cooling outlet 113 is located at the top of the cooling liquid interlayer 111 . In actual operation, the size of the reactor body 11 will change with different reaction requirements. When the reaction kettle body 11 is relatively large and the reaction temperature is too high and needs to be cooled quickly, the effect of only turning off the heating device is limited. Therefore, a cooling liquid interlayer 111, a cooling inlet 112, and a cooling outlet 113 are arranged outside the reactor body 11, and the effect of rapid cooling...

Embodiment 3

[0068] This embodiment provides a kind of synthetic method of highly crystalline nanoscale solid-state electrolyte precursor, and target product is Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 (LATP), including the following steps:

[0069] (S1) Solvent preheating: water and ethylene glycol are mixed according to the weight ratio of 2:1 and used as a solvent, put into the reactor body 11, the stirring device 12 is turned on and preheated to a temperature of 55° C. to obtain a mixture a;

[0070] (S2) dissolving the dispersant: adding polyvinylpyrrolidone to the mixture a, the amount of the polyvinylpyrrolidone added is 0.3% of the weight of the solvent, and stirring evenly to obtain the mixture b;

[0071] (S3)AO 6 Octahedral pre-nucleation: Ti(OC 4 h 9 ) 4 , Al(NO 3 ) 9H 2 O, the Ti 4+ Concentration is 18000ppm, the Al(NO 3 )·9H 2 O and the Ti(OC 4 h 9 ) 4 The molar ratio is 0.4. At this time, use low-speed stirring and turn on the microwave generator. The method is: the mi...

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Abstract

The invention relates to a continuous reactor for synthesizing a high-crystallinity nanoscale solid electrolyte precursor and a synthesis method. The continuous reactor comprises a reaction kettle body, and a stirring device, a heating device and a feeding controller are arranged on the reaction kettle body; the stirring device is used for stirring reaction materials; the heating device is used for changing the reaction temperature; the feeding controller is used for adding reaction materials; the reaction kettle body further comprises a temperature sensor and a pH sensor, and the temperature sensor is arranged in the reaction kettle body, connected with the heating device and used for detecting the reaction temperature and controlling starting and stopping of the heating device; the pH sensor is arranged in the reaction kettle body, is connected with the feeding controller, and is used for detecting a reaction pH value and controlling the feeding controller to start and stop. The continuous reactor can monitor the temperature and the pH value of a reaction system in real time and transmit signals to the heating device and the feeding controller, so that the temperature and the pH value in the reaction process are automatically and accurately adjusted, and the reaction is smoothly carried out.

Description

technical field [0001] The invention belongs to the field of solid electrolytes, and in particular relates to a continuous reactor and a synthesis method for synthesizing a highly crystalline nanoscale solid electrolyte precursor. Background technique [0002] Most of the lithium-ion secondary batteries currently on the market use liquid electrolytes, which greatly limits the production process. In terms of environmental requirements for assembly, moisture control is very strict, and in subsequent product applications, liquid electrolytes have Safety issues such as packaging leakage, current collector corrosion, over-temperature explosion, etc. In addition, because the liquid electrolyte is accompanied by the formation of protective film (SEI), side reaction gas generation, and decomposition under high temperature and high pressure during the electrochemical reaction, the battery generally suffers from the phenomenon of cycle capacity decay. If a solid electrolyte is used, ...

Claims

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Application Information

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IPC IPC(8): B01J19/18B01J19/12H01M10/0562H01M10/0525
CPCB01J19/18B01J19/126H01M10/0562H01M10/0525B01J2219/00141B01J2219/00033B01J2219/00063B01J2219/00177
Inventor 陈钰夫赵振浩刘元中
Owner 瑟瑞米(洛阳)新能源科技有限公司
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