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Superfine nano barium carbonate and preparation method thereof

An ultra-fine nano and barium carbonate technology, applied in the direction of barium carbonate, calcium carbonate/strontium/barium, nanotechnology, etc., can solve the problems of energy consumption, affecting the back-end application of barium carbonate powder, grain growth, etc.

Pending Publication Date: 2021-12-21
福建贝思科电子材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, a mixed solution of ethanol, methanol, isopropanol and water is used as a solvent, so it is difficult to control the grain shape of barium carbonate, and the barium carbonate produced is generally needle-like or irregular in shape, which does not meet the requirements
[0003] Chinese patent CN101177293 discloses a preparation method of nano-barium carbonate, which cannot obtain high-purity barium carbonate powder in the next step at normal temperature and pressure. In order to improve the purity, a second high-temperature heat treatment is required. High-temperature secondary heat treatment will lead to further growth of grains, and the grain size distribution is between 150 and 310nm
In addition, the grain shape of barium carbonate obtained in the prior art is mostly irregular, and these defects will seriously affect the back-end application of barium carbonate powder

Method used

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  • Superfine nano barium carbonate and preparation method thereof
  • Superfine nano barium carbonate and preparation method thereof
  • Superfine nano barium carbonate and preparation method thereof

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preparation example Construction

[0030] The present invention provides a method for preparing nano ultrafine barium carbonate, comprising the steps of:

[0031] A) The alcohol solution of barium hydroxide octahydrate and mixing, to give an alcohol solution of barium hydroxide octahydrate;

[0032] B) The alcohol solution of barium hydroxide octahydrate, and the reaction was stirred for dimethyl carbonate, the pH is ≤8, stirring was stopped by adding ammonia was allowed to stand to give a liquid mixture;

[0033] C) The mixture of the solid-liquid separation, dried, ultrafine nano barium carbonate.

[0034] Step a) in:

[0035] In certain embodiments of the present invention, the alcohol solution of the alcohol include ethylene glycol or glycerol; the alcohol solvent in the solution is water.

[0036] In certain embodiments of the present invention, the alcohol solution, the volume ratio of alcohol to water is 0.4 to 15: 1. In certain embodiments, the alcohol solution, the volume ratio of alcohol to water is 15: 1...

Embodiment 1

[0064] 1) 468.75 ml of ethylene glycol and 31.25 ml of water were mixed to obtain a glycol solution, and an octohydride is dissolved to give an alcohol solution having a mass concentration of 6% octhyde hydroxide;

[0065] 2) In the alcohol solution of the octamite in the octohydrofluide, the molar ratio of dimethyl carbonate and octhyde hydroxide is 1: 1 at a rate of 3 g / min, and stirred at normal temperature. The reaction, the pH was stopped at 7 to 8, and the mixture was added, and ammonia water (in the stirred solution, the amount of ammonia was 1 vol%) was allowed to stand, resulting in a mixture liquid;

[0066] 3) The mixture was separated, and the material after centrifugation was washed twice with water, and ethanol was purified twice, and the purity was 99.9% ultrafine nanocarbonate. Bismuth.

[0067] In this embodiment, the obtained ultrafine nanocarbonate is scanned electron microscopy, as a result, figure 1 and figure 2 Indicated. figure 1 The SEM diagram of the ult...

Embodiment 2

[0069] 1) 450 ml of ethylene glycol with 50 ml of water to obtain an ethylene glycol solution, and octose hydroxide is dissolved, and an alcohol solution having a mass concentration of 3% octohydride;

[0070] 2) In the alcohol solution of the octamite in the octohydrocarbon hydroxide, the molar ratio of dimethyl carbonate and octhyde is 0.5: 1, stirring at normal temperature. The reaction, the pH was stopped at 7 to 8, and the mixture was added, and an ammonia water (in the stirred solution, the amount of ammonia was 5 vol%) was allowed to allow the mixture liquid;

[0071] 3) The mixture was separated, and the material after centrifugation was washed twice with water, and ethanol was washed twice, and the purity was 99.7% ultrafine nanocarbonate.

[0072] The ultrafine nanocarbonate was scanned electron microscopy, and the experimental results show that the grain size of the ultrafine nanocarbonate is 35 to 50 nm.

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Abstract

The invention relates to the technical field of functional ceramic raw materials, in particular to superfine nano barium carbonate and a preparation method thereof. The preparation method of the superfine nano barium carbonate comprises the following steps of A) mixing an alcoholic solution and barium hydroxide octahydrate to obtain an alcoholic solution of barium hydroxide octahydrate, B) stirring the alcoholic solution of barium hydroxide octahydrate and dimethyl carbonate to react, stopping stirring when the pH value is less than or equal to 8, adding ammonia water, and standing to obtain a mixed solution, and C) carrying out solid-liquid separation on the mixed material liquid, and drying to obtain the superfine nano barium carbonate. The mixed solution of alcohol and water is used as a reaction medium, a barium source and dimethyl carbonate are subjected to one-step reaction at normal temperature and normal pressure to synthesize the sphere-like superfine nano barium carbonate powder, the particle size of the powder is small, and the purity of the powder is high; meanwhile, secondary high-temperature heat treatment can be avoided, steps are simplified, and energy is saved.

Description

Technical field [0001] The present invention relates to a functional ceramic materials technology, and in particular, to a method for preparation of ultrafine and nano barium carbonate. Background technique [0002] Barium carbonate is widely used in the synthesis of barium titanate, and barium carbonate powder properties will largely affect the structure of the backend application barium titanate, and barium titanate powder is applied to the MLCC generally it is expected to be spherical. The prior art ethanol, mixed solution of methanol and isopropyl alcohol and water as a solvent, it is difficult to control the shape of the crystal grains of the barium carbonate, barium carbonate output pin typically is a rod-like or irregularly shaped, does not meet the requirements of . [0003] Chinese patent CN101177293 discloses a method for preparing nano-barium carbonate, which can not obtain high purity barium carbonate in the next normal temperature and pressure, in order to improve th...

Claims

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Application Information

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IPC IPC(8): C01F11/18B82Y40/00
CPCC01F11/188B82Y40/00C01P2004/32C01P2004/64C01P2006/80
Inventor 胡新龙戴书云
Owner 福建贝思科电子材料股份有限公司
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