Superfine and high-purity bismuth oxide and preparation method thereof

A technology of bismuth oxide and high fineness, which is applied in chemical instruments and methods, inorganic chemistry, bismuth compounds, etc., can solve the problems of unreached product particle size, complicated process, complicated separation procedure, etc., and achieve high purity and good product uniformity , the effect of controlling the reaction speed

Inactive Publication Date: 2010-08-25
ZHUZHOU SMELTER GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent 200810147959.2 discloses a production method of high-purity ultra-fine bismuth oxide. The steps are as follows: ball mill bismuth salt compound, dispersant, ammonium bicarbonate and a small amount of solvent to obtain bismuth oxycarbonate, wash with deionized water, and mix with certain A certain amount of ammonium bicarbonate is mixed evenly and calcined to obtain the target product; the above-mentioned dispersant is taken from one of Tween, Span or emulsifier OP; the fine powder with a particle size of less than 1 μm can be obtained, and the process conditions of the above-mentioned method are easy to control , the product uniformity is good, but the process is more complicated and the production cost is higher
It still needs to use a dispersant, adding a dispersant is easy to introduce impurities, but also increases the cost, the separation procedure is complicated, and more importantly, the particle size of the obtained product does not meet the requirement of a particle size of 10-100nm

Method used

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  • Superfine and high-purity bismuth oxide and preparation method thereof
  • Superfine and high-purity bismuth oxide and preparation method thereof

Examples

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Embodiment 1

[0039] A preparation method of ultra-fine and high-purity bismuth oxide, which uses solid bismuth with a purity of 4N as raw material. It pretreats 500g of 4N bismuth with a mixed solution of 2g / L nitric acid and 3g / L hydrochloric acid, that is, the soaking time is 50 minutes Then take it out and react with nitric acid, that is, slowly add about 900 mL of nitric acid with a concentration (wt%) of 60% under constant stirring, and add an appropriate amount of soluble SiO with a conductivity of less than 500us / cm 2 Distilled water less than 0.02mg / L to obtain a bismuth nitrate solution, add 0.001 times the volume of bismuth nitrate solution to the obtained bismuth nitrate solution; cm, soluble SiO 2 Distilled water of less than 0.02 mg / L is prepared at a volume ratio of 1:1 to obtain an aqueous ammonia solution with a mass percentage concentration of 12.8%. Add the above-mentioned bismuth nitrate solution and aqueous ammonia solution under constant stirring conditions with conducti...

Embodiment 2

[0041] A preparation method of ultra-fine and high-purity bismuth oxide, which uses 4N solid bismuth as raw material to synthesize ultra-fine and high-purity bismuth oxide. It pretreats 500g 4N solid bismuth with 3g / L nitric acid and 5g / L hydrochloric acid solution. That is, the immersion time is 40 minutes and then take it out to react with nitric acid, that is, slowly add about 1050 mL of nitric acid with a concentration (wt%) of 50% under constant stirring, and add an appropriate amount of soluble SiO with a conductivity of less than 500us / cm 2 Deionized water less than 0.02mg / L, the obtained bismuth nitrate solution is treated with sulfuric acid 0.002 times the volume of the bismuth nitrate solution; 450mL ammonia water with a mass percentage of 27% and 900mL conductivity less than 500us / cm, soluble SiO 2 The deionized water of less than 0.02 mg / L is prepared with a volume ratio of 1:2 to obtain an ammonia aqueous solution with a concentration of 8.3% by mass. The above-menti...

Embodiment 3

[0043] A preparation method of ultra-fine and high-purity bismuth oxide. It uses 4N solid bismuth as raw material to synthesize ultra-fine and high-purity bismuth oxide. It pretreats 500g of 4N solid bismuth with 4g / L nitric acid and 5g / L hydrochloric acid solution. That is, the immersion time is 30 minutes and then take it out to react with nitric acid, that is, slowly add about 1300 mL of nitric acid with a concentration (wt%) of 40% under constant stirring, and add an appropriate amount of soluble SiO with a conductivity of less than 500us / cm 2 Distilled water less than 0.02mg / L, the obtained bismuth nitrate solution is treated with sulfuric acid 0.002 times the volume of the bismuth nitrate solution; 450mL ammonia water with a mass percentage concentration of 27% and 900mL conductivity less than 500us / cm, soluble SiO 2 Distilled water of less than 0.02 mg / L is prepared with a volume ratio of 1:2 to obtain an ammonia aqueous solution with a mass percentage concentration of 8.3%...

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Abstract

The invention relates to a superfine and high-purity bismuth oxide with the granularity of 10-1000nm and a preparation method thereof. The method takes the solid bismuth with the purity of 4N as a raw material to synthesize the superfine and high-purity bismuth oxide, and is characterized in comprising the following steps of: firstly, soaking the solid bismuth with the purity of 4N into mixed acid solution which is prepared by hydrogen nitrate and muriatic acid; taking out the soaked solid bismuth, and enabling the soaked solid bismuth to react with hydrogen nitrate solution to obtain the bismuth nitrate solution and keep the excessive status of the hydrogen nitrate; mixing the bismuth nitrate solution with the ammonia water solution to perform synthetic reaction; filtrating to obtain white bismuth hydroxide deposition; and washing, drying, calcining and preparing powder according to a conventional method to obtain the superfine and high-purity bismuth oxide with the phase of alpha-Bi2O3, the granularity of 10-100nm and the purity of 5N. The technological condition is easily controlled, has good product homogeneity, and does not need to an add dispersing agent, thereby being capable of obtaining the superfine bismuth oxide powder with even granularity, preventing impurity from being induced, and reducing the preparation cost.

Description

Technical field [0001] The invention relates to a bismuth oxide used in the electronics industry and a production method thereof, in particular to an ultrafine high-purity bismuth oxide with a particle size of 10-100 nm and a production method thereof. Background technique [0002] Ultra-fine high-purity bismuth oxide is a light yellow powder with a phase of α-Bi 2 O 3 , A spherical aggregate with a particle size of 10-100nm and a purity of 5N. Wide range of uses, mainly used in the production of electronic ceramic powder materials, ferrite magnetic materials, electrolyte materials, photoelectric materials and superconducting materials, etc., and can be used as organic synthesis catalysts, special glass, chemical fiber flame retardants and environmental protection Battery additives, etc. [0003] At present, there are two main types of methods for preparing ultra-fine high-purity bismuth oxide. One is to directly use 5N or above high-purity bismuth to synthesize through a series o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G29/00
Inventor 刘一宁林文军廖贻鹏窦传龙赵为上
Owner ZHUZHOU SMELTER GRP
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