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Preparation method of raw material low-Fe-ion and low-Ca-ion nano oxide for MLCC

A nano-oxide and ion technology, applied in the preparation/processing of rare earth metal compounds, nanotechnology for materials and surface science, rare earth metal oxides/hydroxides, etc., can solve the problem of high impurities, difficult to dry, Cost increase and other issues, to achieve the effect of reducing impurity content and high purity of precipitant

Pending Publication Date: 2020-12-08
CHANGZHOU GEOQUIN NANO NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The general preparation process of nano-rare earth oxides is to dissolve the alkali salt in water and then directly precipitate it, and add it dropwise to the feed liquid. The alkali salt used is generally industrial grade, which contains relatively high impurities, and the precipitated Nanoscale particles, because the particles are nanoscale and very small, it is difficult to drain when washing with water, making it difficult to remove impurities by washing with water
If the alkali salt used for precipitation is food-grade, the impurities will be less, but the cost will increase accordingly

Method used

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  • Preparation method of raw material low-Fe-ion and low-Ca-ion nano oxide for MLCC
  • Preparation method of raw material low-Fe-ion and low-Ca-ion nano oxide for MLCC
  • Preparation method of raw material low-Fe-ion and low-Ca-ion nano oxide for MLCC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) preparation concentration is the yttrium chloride feed liquid of 0.4mol / l, and the acidity of control yttrium chloride feed liquid is less than 0.3mol / l;

[0025] (2) According to the mol ratio of yttrium chloride and precipitating agent, add sodium carbonate at 1:1.6, the concentration of sodium carbonate solution is 0.5mol / l, then add 2% dispersant PEG2000, add dropwise precipitation; sodium carbonate solution It needs to be filtered through membrane filtration equipment before use. Time required to filter sodium carbonate solution: 1.5h.

[0026] (3) After the dropwise addition, control the pH of the precipitate to be 6.5-7, stir for 1h, and age for 2h;

[0027] (4) Put the slurry into the plate and frame filter press first, press the mother liquor as dry as possible, then put the filter cake into the suction filter barrel, stir and wash with water at a temperature of 50°C, and wash until the waste water is titrated with silver nitrate without precipitation . ...

Embodiment 2

[0030] 1) preparation concentration is the holmium cerium chloride feed liquid of 0.3mol / l, and the control holmium chloride feed liquid acidity is less than 0.3mol / l;

[0031] (2) According to the molar ratio of holmium chloride and precipitant: add sodium bicarbonate at 1:1.5, the concentration of sodium bicarbonate solution is 0.5mol / l, then add 2.5% dispersant PEG2000, add dropwise precipitation; The sodium hydrogen solution needs to be filtered through an improved membrane filtration device before use, and the time required to filter the sodium carbonate solution: 1h.

[0032] (3) After the dropwise addition, control the pH of the precipitate to be 6.5-7, stir for 1h, and age for 2h;

[0033] (4) Put the slurry into the plate and frame filter press first, press the mother liquor as dry as possible, then put the filter cake into the suction filter barrel, stir and wash with water at a temperature of 55°C, and wash until the waste water is titrated with silver nitrate witho...

Embodiment 3

[0036] (1) preparation concentration is the erbium chloride feed liquid of 0.6mol / l, and the control erbium chloride feed liquid acidity is less than 0.3mol / l;

[0037] (2) According to the mol ratio of erbium chloride and precipitating agent, add sodium carbonate at 1:1.6, the concentration of sodium carbonate solution is 0.6mol / l, then add 3% dispersant PEG2000, add dropwise precipitation; sodium carbonate solution It needs to be filtered through improved membrane filtration equipment before use. Time required to filter sodium carbonate solution: 1.5h.

[0038] (3) After the dropwise addition, control the pH of the precipitate to be 6.5-7, stir for 1h, and age for 2h;

[0039] (4) Put the slurry into the plate and frame filter press first, press the mother liquor as dry as possible, then put the filter cake into the suction filter barrel, stir and wash with water at a temperature of 60°C, and wash until the waste water is titrated with silver nitrate without precipitation ...

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Abstract

The invention belongs to the technical field of rare earth oxide preparation. The invention particularly relates to a preparation method of a raw material low-Fe-ion and low-Ca-ion nano oxide for MLCC. A precipitation method is adopted, low-Fe-ion and low-Ca-ion alkali salt obtained after membrane filtration is selected as a precipitant, an anionic surfactant is selected as an additive, rare earthions are precipitated, precipitates are washed through combination of a plate-and-frame filter press and a suction filtration barrel, the content of Fe ions and Ca ions is controlled, then burning and sieving are carried out to prepare nano rare earth oxide with a content of Fe3+ less than 5 ppm and a content of Ca2+ less than 5 ppm.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth oxides, and in particular relates to a method for preparing nano-oxides with low Fe ions and low Ca ions as raw materials for MLCC. Background technique [0002] Nano-rare earth oxides are widely used, especially in glass, ceramics, electronics and other fields. In many applications, there are not only strict requirements on the particle size of rare earth oxide powders, but also higher requirements on non-rare earth impurities. For example, when nano-oxides are used as raw materials for MLCC (multilayer ceramic capacitors), in order to improve the heat resistance and insulation properties of capacitors, as well as increase the frequency of use of capacitors and prolong their service life, it is generally required that non- Rare earth impurity iron ions, the lower the calcium ions, the better. [0003] The general preparation process of nano-rare earth oxides is to dissolve the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/206C01F17/218C01F17/10B82Y30/00B82Y40/00
CPCC01F17/218C01F17/206C01F17/10B82Y30/00B82Y40/00C01P2004/03C01P2004/64C01P2004/32
Inventor 杨应亚
Owner CHANGZHOU GEOQUIN NANO NEW MATERIALS
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