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Crystallization method of monodisperse lithium carbonate crystals and method for improving product yield by adopting multistage gradient crystallization

A gradient crystallization and lithium carbonate technology, applied in the direction of lithium carbonate;/acid carbonate, etc., to achieve the effect of complete shape, uniform distribution, and avoiding product agglomeration

Active Publication Date: 2020-09-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to comprehensive literature and patent reports, the preparation of monodisperse lithium carbonate crystals with complete crystal morphology by aqueous phase reaction crystallization method is still a blank in this field.

Method used

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  • Crystallization method of monodisperse lithium carbonate crystals and method for improving product yield by adopting multistage gradient crystallization
  • Crystallization method of monodisperse lithium carbonate crystals and method for improving product yield by adopting multistage gradient crystallization
  • Crystallization method of monodisperse lithium carbonate crystals and method for improving product yield by adopting multistage gradient crystallization

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Embodiment 1

[0056] In the present embodiment, a crystallization method of monodisperse lithium carbonate crystals is provided, comprising the following steps: using a one-step reaction crystallization method of equimolar and equal volumes of lithium sulfate and sodium carbonate solution, directly adding 40 mL of 9.07 mL of crystallization to a 100 mL crystallization kettle %wt lithium sulfate solution and 40mL sodium carbonate solution with a concentration of 8.74%wt, the temperature is controlled at 65°C, and the laser method is used to control the rapid sampling at the moment of crystallization, that is, a beam of laser light is transmitted through the solution through a laser transmitter. When the laser intensity When the signal dropped suddenly, the slurry was taken out for solid-liquid separation, and the obtained solid was air-dried at 50°C for 10 hours to obtain monodisperse lithium carbonate crystals.

Embodiment 2

[0058] In the present embodiment, a crystallization method of monodisperse lithium carbonate crystals is provided, comprising the following steps: using a one-step reaction crystallization method of equimolar and equal volumes of lithium sulfate and sodium carbonate solution, directly adding 40 mL of crystallization pot with a concentration of 8.44 %wt lithium sulfate solution and 40mL sodium carbonate solution with a concentration of 8.13%wt, the temperature is controlled at 80°C, and the laser method is used to control the rapid sampling at the moment of crystallization, that is, a beam of laser light is transmitted through the solution through a laser transmitter. When the laser intensity When the signal dropped suddenly, the slurry was taken out for solid-liquid separation, and the obtained solid was air-dried at 50°C for 10 hours to obtain monodisperse lithium carbonate crystals.

Embodiment 3

[0060] In the present embodiment, a method for crystallization of monodisperse lithium carbonate crystals is provided, comprising the following steps: using a one-step reaction crystallization method of equimolar and equal volumes of lithium sulfate and sodium carbonate solutions, directly adding 40 mL of 7.87 mL of the crystallization pot to a 100 mL crystallization kettle. %wt lithium sulfate solution and 40mL sodium carbonate solution with a concentration of 7.58%wt, the temperature is controlled at 95°C, and the laser method is used to control the rapid sampling at the moment of crystallization, that is, a beam of laser light is transmitted through the solution through a laser transmitter. When the laser intensity When the signal dropped suddenly, the slurry was taken out for solid-liquid separation, and the obtained solid was air-dried at 50°C for 10 hours to obtain monodisperse lithium carbonate crystals.

[0061] figure 1 The scanning electron micrograph of the monodisp...

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Abstract

The invention provides a crystallization method of monodisperse lithium carbonate crystals and a method for improving the product yield by adopting multistage gradient crystallization. Firstly, a lithium sulfate and sodium carbonate reaction crystallization method is adopted, a crystallization instant sampling method is adopted, and solid is obtained and dried to obtain monodisperse lithium carbonate crystals. Meanwhile, a plurality of crystallization kettles are connected in series, and the product yield is improved through a multi-stage crystallization and mother liquor circulation method. The mixed material liquid enters a first-stage crystallization kettle; controlling the kettle temperature, enabling the slurry to flow out from the bottom of the crystallization kettle and enter a solid-liquid separation system, enabling mother liquor after solid separation to enter the next crystallization kettle, controlling the kettle temperature, enabling the slurry to flow out from the bottomof the final crystallization kettle and enter the solid-liquid separation system, enabling the mother liquor after solid separation to return to the mixing kettle for recycling, and enabling the circulation amount to be 40-80% of the volume of the mother liquor. The monodisperse lithium carbonate crystal prepared by the method is complete in morphology, almost free of coalescence, small in particle size and uniform in distribution, and the crystallization method is simple to operate, high in production efficiency and suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of industrialized production of lithium carbonate, and relates to a crystallization method of monodisperse lithium carbonate crystals and a method for improving product yield by adopting multi-stage gradient crystallization. Background technique [0002] Lithium carbonate is a key raw material for lithium-ion battery electrode materials (lithium cobaltate, lithium manganate, lithium iron phosphate, etc.), electrolytes (lithium hexafluorophosphate, etc.) and additives (lithium dioxalate borate, etc.). In recent years, with the warming up of global new energy development, lithium-ion batteries for power and energy storage are developing at a high speed, which has promoted the rapid growth of lithium carbonate market consumption, and lithium carbonate and its preparation have attracted extensive attention from the industry. [0003] The current commercially used lithium-ion battery cathode materials are mainly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2004/03C01P2002/72C01P2004/52C01P2004/61C01P2006/12C01P2002/20C01P2002/10
Inventor 龚俊波汤伟伟赵绍磊侯宝红王艳吴送姑尹秋响
Owner TIANJIN UNIV
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