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Method for preparing hexagonal crystal system hydroxyl lanthanum carbonate by adopting hydrothermal synthesis

A technology of lanthanum hydroxycarbonate and hexagonal crystal system, which is applied in the preparation/processing of rare earth metal compounds, rare earth metal carbonate, etc., can solve the problem of increasing the difficulty and cost of preparation, the hexagonal lanthanum hydroxycarbonate has no relevant instructions, and the auxiliary materials are special. And other problems, to achieve the effect of low price, stable product quality, and increase the cost of auxiliary materials

Pending Publication Date: 2021-09-03
CHINA NORTHERN RARE EARTH (GROUP) HIGH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the equipment and process require special auxiliary materials, which increases the difficulty and cost of preparation
[0007] At present, in the rare earth hydrometallurgy industry, there is no relevant statement on the preparation of hexagonal lanthanum hydroxycarbonate by atmospheric pressure hydrothermal synthesis

Method used

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  • Method for preparing hexagonal crystal system hydroxyl lanthanum carbonate by adopting hydrothermal synthesis
  • Method for preparing hexagonal crystal system hydroxyl lanthanum carbonate by adopting hydrothermal synthesis

Examples

Experimental program
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Effect test

Embodiment 1

[0048] In the precipitation reactor, use deionized water to prepare the lanthanum chloride solution into a bottom solution with a concentration of 0.7mol / L, add 30% lanthanum carbonate as a seed crystal, and after stirring evenly, use the co-current precipitation method to control the addition of chloride The flow rate of lanthanum feed liquid and precipitant (ammonium bicarbonate solution); feed liquid concentration is 1.5mol / L, precipitant concentration is 3mol / L, reaction temperature is controlled at 32°C, reaction time is 6h, precipitation endpoint pH=6.7.

[0049] After filtering, the filter cake was rinsed with deionized water and vacuum-dried to obtain lanthanum carbonate. Add lanthanum carbonate and deionized water into the reactor in a mass ratio of 1:4, control the reaction temperature at 110°C, keep it warm for 20 hours, wash the obtained product with deionized water, put it in an oven, and dry it at 150°C for 12 hours , to obtain hexagonal basic lanthanum carbonate...

Embodiment 2

[0053] Use deionized water to prepare the lanthanum chloride solution as a bottom solution with a concentration of 0.5mol / L, add 20% lanthanum carbonate as a seed crystal, and after stirring evenly, adopt a co-current precipitation method to simultaneously control the addition of lanthanum chloride feed solution and precipitation Agent (mixed solution of ammonium bicarbonate and ammonia water) and control the flow rate, the concentration of the precipitating agent is 2mol / L, the reaction temperature is controlled at 48°C, the reaction time is 8h, and the pH of the precipitation end point is 6.5.

[0054] After filtering, the filter cake was rinsed with deionized water and vacuum-dried to obtain lanthanum carbonate. Add lanthanum carbonate and deionized water into the reactor in a mass ratio of 1:3, control the reaction temperature at 150°C, keep it warm for 10 hours, wash the obtained product with deionized water, put it in an oven, and dry it at 180°C for 8 hours , to obtain ...

Embodiment 3

[0056] Use the supernatant of the previous batch to prepare the lanthanum chloride solution into a bottom solution with a concentration of 0.3mol / L, add 40% lanthanum carbonate as a seed crystal, and stir evenly, and then control the addition of lanthanum chloride material at the same time by means of co-current precipitation The flow rate of liquid and precipitant (mixed solution of ammonium bicarbonate and ammonia water); the concentration of feed liquid is 1.8mol / L, the concentration of precipitant is 4mol / L, the reaction temperature is controlled at 40°C, the reaction time is 12h, and the pH of the precipitation end point is 6.7.

[0057] After filtering, the filter cake was rinsed with deionized water and vacuum-dried to obtain lanthanum carbonate. Add lanthanum carbonate and deionized water into the reactor at a mass / volume ratio of 1:6, control the reaction temperature at 130°C, and keep it warm for 11 hours. The obtained product is washed with deionized water and placed...

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Abstract

The invention discloses a method for preparing hexagonal crystal system hydroxyl lanthanum carbonate by adopting hydrothermal synthesis.. The method comprises the following steps: in a precipitation reaction kettle, diluting a lanthanum chloride solution by using deionized water to serve as a base solution, and adding lanthanum carbonate to serve as a seed crystal; adding a feed liquid and a precipitant into the precipitation reaction kettle in a parallel flow precipitation manner, and carrying out precipitation reaction to generate lanthanum carbonate; taking out the precipitate lanthanum carbonate in the precipitation reaction kettle, filtering and drying to obtain lanthanum carbonate serving as a precursor; adding lanthanum carbonate and deionized water into a reactor, controlling the temperature at 110-160 DEG C, stirring, carrying out hydrothermal synthesis reaction, and keeping the temperature for 6-20 hours; and washing the obtained final product with deionized water, carrying out suction filtration or centrifugation to obtain a white solid, placing the white solid in a drying oven, and drying at 150-200 DEG C to obtain the hexagonal crystal system hydroxyl lanthanum carbonate. The method is simple in production process and suitable for industrial batch production of hexagonal crystal system hydroxyl lanthanum carbonate.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy, and in particular relates to a method for preparing hexagonal lanthanum hydroxycarbonate by hydrothermal synthesis. Background technique [0002] Rare earth luminescent materials are mainly used in rare earth energy-saving lamps and white LED lighting devices. Rare earth energy-saving lamps are high-quality and efficient green lighting products. Compared with incandescent lamps and phosphors made of halogen powder, they have the advantages of high luminous efficiency, energy saving, low light decay, and long life. At present, the export volume of tri-color energy-saving lamps produced in my country has reached about 80%, and it is the largest manufacturing base of energy-saving light sources in the world. With the gradual promotion of green lighting, the market demand for tri-color phosphors for energy-saving lamps will be even greater in the future. [0003] There are many factors that affect the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/247C01F17/10
CPCC01F17/247C01F17/10C01P2002/72C01P2002/77C01P2004/03C01P2004/32C01P2004/50
Inventor 李婷婷张文斌赵治华桑晓云徐占宇刘瑞金张国光高媛张永华刘磊郑超李治国张正中张磊
Owner CHINA NORTHERN RARE EARTH (GROUP) HIGH TECH CO LTD
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