CN1121486A

CN1121486A - Process for producing superfine bismuth oxide

Info

Publication number: CN1121486A
Application number: CN 94113621
Authority: CN
Inventors: 康云川; 梁汉贤; 李月秀; 唐丽雅; 符晓惠; 马子鹤
Original assignee: Yunnan Normal University
Current assignee: Yunnan University YNU; Yunnan Normal University
Priority date: 1994-10-24
Filing date: 1994-10-24
Publication date: 1996-05-01

Abstract

The invented process is mainly that under the condition of adding a small quantity of disperser, the superfine bismuth oxide is formed by one-step reaction of bismuth nitrate and lye. The advantages are simple productive process, low productive cost, low consumption of energy source and investment and the grain size of bismuth oxide is less than 0.010 mm.

Description

Process for producing superfine bismuth oxide

The invention relates to a process method for producing chemical products, in particular to a process method for producing superfine bismuth oxide.

The existing process method for producing the superfine bismuth oxide can be divided into a wet method and a fire method, the bismuth oxide particles produced by the wet method are all relatively coarse and are generally larger than 0.050MM, and if the superfine bismuth oxide with the particle size of less than 0.010MM is to be obtained, superfine grinding or long-time ball milling is needed; the plasma heating technology is implemented by necessarily providing a microwave regeneration vessel and an evacuating device, and although the plasma heating technology can quickly produce bismuth oxide particles with the particle size of less than 0.010MM, the two methods have large equipment investment and energy consumption, high production cost and complex process, so that the industrial production is generally difficult to realize.

The invention aims to overcome the defects of the prior art and provides a process method for producing superfine bismuth oxide, which has the advantages of simple production process, low production cost, less equipment investment and granularity less than 0.010 MM.

The technical scheme of the invention is as follows:

1. the principle of production and preparation:

2. the technical conditions and the technical process of the production are as follows:

2.1 preparing sodium hydroxide into a solution with the concentration of 25-35%;

2.2 preparing a bismuth nitrate solution, preparing the bismuth nitrate solution, water and 65% nitric acid according to the proportion of 2: 1: 0.05-0.01, standing and clarifying, and taking supernatant for later use;

2.3, preparing a dispersing agent, wherein the ratio of glycerol to water is 1: 1, and the adding amount of glycerol is 100: 0.015-2 according to the ratio of bismuth nitrate to 50% of glycerol for later use;

2.4 accurately adding 25-35% alkali liquor with the concentration exceeding 5% of the theoretical amount into the enamel reaction kettle or the plastic reaction vessel, adding 1: 1 glycerol solution, and uniformly stirring;

2.5 slowly adding bismuth nitrate solution under the conditions of normal temperature and stirring, wherein the reaction temperature is gradually increased along with the addition of bismuth nitrate, and bismuth nitrate also generates pale yellow bismuth oxide particles through reaction;

2.6 washing the bismuth oxide generated by the reaction with deionized water, filtering, and drying at the temperature of 100-250 ℃ to obtain a bismuth oxide product with the granularity of less than 0.010MM and light yellow appearance color.

Compared with the prior art, the invention has the following advantages:

1. under the condition of adding a small amount of dispersant, bismuth nitrate and sodium hydroxide are utilized to react in one step to generate superfine bismuth oxide with the granularity of less than 0.010 MM;

2. the energy consumption in the production is greatly reduced compared with the original method, and the ultrafine grinding or ball milling which is required by other methods for producing the ultrafine bismuth oxide is omitted;

3. the production time and the working procedures are shortened compared with the prior art, the working procedures such as calcination, pulverization and the like in the prior production working procedure and the investment of calcination and pulverization equipment are saved, thereby greatly reducing the production cost of the superfine bismuth oxide.

The first embodiment is as follows:

300g of bismuth nitrate are dissolved in 150ml of water and a dilute acid solution to which 21ml (65%) of nitric acid is added; dissolving 105g of 95% sodium hydroxide in 270ml of water to prepare 28% alkali liquor, standing until the alkali liquoris cooled to room temperature, and adding 0.9ml of 1: 1 glycerol solution for later use;

slowly adding the bismuth nitrate solution into the alkali liquor under the conditions of normal temperature and stirring, gradually increasing the reaction temperature to 40-60 ℃ along with the addition of the bismuth nitrate solution, gradually converting the bismuth nitrate into pale yellow bismuth oxide, continuously stirring for reaction for 30 minutes after the addition of the bismuth nitrate solution is finished, filtering, washing with deionized water until the nitrate radical is detected to be qualified, and drying at the temperature of 120 ℃ to obtain the superfine bismuth oxide product.

Example two:

300g of bismuth nitrate is dissolved in 150ml of water and a dilute acid solution added with 21ml (65%) of nitric acid, 105g of sodium hydroxide with the content of 95% is dissolved in 270ml of water to prepare about 28% of alkali liquor, the alkali liquor is placed until the alkali liquor is cooled to room temperature, and 3ml of glycerol solution with the ratio of 1: 1 is added for later use;

Claims

1. Process for producing ultrafine bismuth oxide, and method thereofIs characterized in that the principle of production and preparation is as follows:

2. the process according to claim 1, characterized in that the sodium hydroxide is formulated as a 25-35% strength solution;

3. the process method of claim 1, wherein the bismuth nitrate solution is prepared by mixing bismuth nitrate, water and 65% nitric acid in a ratio of 2: 1: 0.05-0.01;

4. the process according to claim 1, wherein the dispersant is formulated as 1: 1 ratio of glycerol to water;

5. the process of claim 4, wherein the glycerol is added in an amount of bismuth nitrate to 50% glycerol to 100: (0.015-2);

6. the process method according to claim 1 or 4, characterized in that 25-35% alkali solution with the concentration exceeding 5% of the theoretical amount is added into an enamel reaction kettle or a plastic reaction vessel, and then 1: 1 glycerol solution is added and stirred uniformly;

7. the process method according to claim 1, wherein the bismuth oxide produced by the reaction is washed with deionized water, filtered and dried at 100-250 ℃.