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Production method of high purity superfine bismuth oxide

A production method and technology of bismuth oxide, applied in chemical instruments and methods, inorganic chemistry, bismuth compounds, etc., can solve the problems of fine particle size, high requirements for equipment and process parameters, low synthesis temperature, etc., and achieve fine particle size, high purity, Good dispersion effect

Inactive Publication Date: 2009-05-27
CHENGDU SHUDU NANO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the introduction of sodium ions in this method, the purity of bismuth oxide is not easy to control, and the shape of bismuth oxide produced is rod-shaped, which is difficult to mix evenly in application.
In addition, there is also a method of directly reacting bismuth nitrate with ammonium bicarbonate to produce bismuth oxycarbonate, and then calcining to produce bismuth oxide. Due to the high pH value of the end point, it is difficult to remove impurity ions in the solution, and the purity of the product is difficult to guarantee.
The sol-gel method has high mixing uniformity of raw materials, low synthesis temperature, and easy to obtain nano-sized particles, but the cost of raw materials is high, and industrial production is unrealistic
Plasma products have fine particle size and high purity, but require high equipment and process parameters

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 1000 g of bismuth nitrate pentahydrate, 10 ml of Tween-80, 250 g of ammonium bicarbonate, and 200 ml of methanol into a ball mill. After the ball milling reaction, white bismuth oxycarbonate is obtained, filtered and washed with deionized water three times, and the filter cake is passed through 100 sieves The mixed ammonium bicarbonate is uniformly mixed and then placed in a calcination furnace for 6 hours at 600°C. The obtained bismuth oxide is spherical, with a particle size of 0.89 μm, and the content of impurities such as K, Na, Ca, Mg, Fe, Cd, Cu, Pb, and Cl is less than 20 ppm.

Embodiment 2

[0016] Add 1000 g of bismuth nitrate pentahydrate, 10 ml of Span-80 (foreign trade name: span, non-release emulsifier, scientific name: sorbitan fatty acid ester), 200 g of ammonium bicarbonate, and 200 ml of ethanol into the ball mill, and the ball mill reaction Afterwards, white bismuth oxycarbonate was obtained, which was filtered and washed with deionized water for three times, and the filter cake was uniformly mixed with ammonium bicarbonate passed through 100 sieves and then placed in a calciner for calcination at 550°C for 6 hours. The obtained bismuth oxide is spherical, with a particle size of 0.92 μm, and the content of impurities such as K, Na, Ca, Mg, Fe, Cd, Cu, Pb, and Cl is less than 20 ppm.

Embodiment 3

[0018] Add 1000 g of bismuth acetate, 10 ml of emulsifier OP-4, 250 g of ammonium bicarbonate, and 200 ml of acetone into the ball mill. After the ball milling reaction, white bismuth oxycarbonate is obtained, which is filtered and washed with deionized water for three times. Ammonium bicarbonate is mixed uniformly and put into a calciner for calcination at 450°C for 7 hours. The obtained bismuth oxide is spherical, with a particle size of 0.92 μm, and the content of impurities such as K, Na, Ca, Mg, Fe, Cd, Cu, Pb, and Cl is less than 20 ppm.

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Abstract

The invention relates to a method for producing high purity superfine bismuth oxide. The method comprises the following steps: a bismuth salt compound, a dispersant, ammonium bicarbonate and a small amount of solvent are subjected to ball milling to obtain bismuth carbonate, and the obtained bismuth carbonate is washed by using deionized water and is mixed evenly with a certain amount of ammonium bicarbonate and is calcined to obtain a target product; the solvent is taken from one of methanol, ethanol or acetone, the bismuth salt compound can be bismuth nitrate pentahydrate or bismuth acetate, and the dispersant can be one of tween, span or emulsifier OP; and the weight ratio of the bismuth in the bismuth salt compound to the dispersant is 1: 0.01-0.1. The bismuth oxide has high purity, low impurity content and good dispersibility and is particularly suitable for the electronic grade industrial ceramic industry.

Description

Technical field [0001] The invention relates to a production method of bismuth oxide, in particular to a production method of high-purity ultrafine bismuth oxide for preparing functional ceramic powder for the electronic industry. Background technique [0002] In the application of electronic varistor ceramics, the purity, particle size and morphology of bismuth oxide are critical to the performance of electronic components. The production methods of bismuth oxide include solid phase method and liquid phase method. The solid phase method includes chemical vapor deposition, plasma method, etc., and the liquid phase method includes precipitation method, hydrolysis method, sol-gel method, microemulsion method, etc. Each method has its own characteristics. The precipitation method has a simple process and is easy to industrialize. The production of bismuth oxide by the domestic precipitation method is mostly a one-time precipitation process. That is, bismuth metal is dissolved in nit...

Claims

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Application Information

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IPC IPC(8): C01G29/00
Inventor 刘春许则良付云德
Owner CHENGDU SHUDU NANO SCI
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