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A kind of preparation method of micron tin dioxide powder

A tin dioxide, micron-scale technology, applied in tin oxide and other directions, can solve the problems of restricted use, incomplete reaction, high production cost, and achieve the effects of environmental protection in the production process, simple production equipment, and prevention of agglomeration and polymerization.

Active Publication Date: 2015-10-28
GUANGDONG GUANGHUA SCI TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen from the published literature that the preparation methods of tin dioxide mainly include the chemical synthesis method using tin-containing waste as raw material and the nitric acid method or high-temperature gasification method using tin ingot as raw material; Chinese patent CN102102150A discloses a A method for preparing tin dioxide from tin-containing waste as a raw material. The method is a method for separating tin from waste tinplate and preparing tin dioxide. The main steps are: (1) crushing and screening the waste tinplate; (2) using soda aqueous solution Wash the undersize; (3) filter the washings, leach the filter residue with sodium hydroxide solution and an oxidizing agent, filter the leachate, and the filtrate is sodium stannate solution; (4) pass carbon dioxide into the sodium stannate solution, filter , washing to obtain a tin dioxide product; this preparation method has a long process route, a large demand for carbon dioxide, and a low utilization rate. The actual usage is 10-50 times that of the theoretical calculation, which is not very industrially feasible, and the product The impurity content is still high
Chinese patent CN1657417 discloses a method for producing tin dioxide by nitric acid method, which is a method for wet manufacturing metastannic acid and tin dioxide powder, the main steps of which are under the condition of airtight pressurization and oxygen addition, Control a certain temperature and reaction time, so that tin and nitric acid fully react to generate metastannic acid intermediate product, metastannic acid intermediate product is neutralized, washed and dried to obtain metastannic acid product; metastannic acid is calcined and crushed to obtain a particle size smaller than 10um fine tin dioxide product; this method uses nitric acid to prepare metastannic acid, a large amount of nitrogen oxides are produced, the process is not environmentally friendly, and nitric acid is a strong acid, and the product is easily polluted due to equipment corrosion. In addition, the product requires Fine tin dioxide products of 10um can only be achieved after crushing, which limits the use of products in high-end electronics and other fields
The technology for preparing high-purity tin dioxide by high-temperature gasification is relatively complicated, and is limited by equipment, resulting in high production costs and weak market competitiveness
[0003]Because the high-end fields such as electronic materials have high requirements on the purity and material properties of tin dioxide, the tin dioxide produced by traditional production methods cannot meet this demand. Most still rely on imported products
Chinese patent CN101532096 discloses a method for recovering tin from tin stripping waste liquid. The process is to use strong alkali to convert tin into sodium stannate solution, and then introduce carbon dioxide to prepare metastannic acid. Metastannic acid is washed and calcined to prepare di Tin oxide, because carbon dioxide is a weak acid, the reaction with sodium stannate solution is not complete, and metastannic acid is an amorphous colloid with strong adsorption capacity. Washing metastannic acid with pure water, the sodium carbonate ion wrapped in metastannic acid is still very high , up to 3%, sodium carbonate reacts with metastannic acid to form sodium stannate during calcination, which seriously corrodes the calcination equipment, and the finished product of tin dioxide cannot meet the needs of electronic industries such as conductive glass due to high impurities

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  • A kind of preparation method of micron tin dioxide powder

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Effect test

Embodiment 1

[0021] Take a certain amount of reagent grade sodium stannate, use pure water to prepare a sodium stannate solution with a concentration of 50g / L, heat it in a water bath to 60°C, start stirring, add dropwise an ammonium bicarbonate solution with a concentration of 100g / L, and react to The pH value of the reaction solution is 9.0, stop the dripping, and filter to obtain the hydrated tin hydroxide solid; use pure water to beat the hydrated tin hydroxide solid with a liquid-solid ratio of 4:1, and adjust the pH value of the hydrated tin hydroxide slurry with nitric acid To 2, at this time, the hydrated tin hydroxide has been converted into metastannic acid, and the residual sodium carbonate has been completely decomposed into nitrates with stronger water solubility, washed 5 times with pure water, and the liquid-solid ratio is 3:1. Then wash once with ethanol with a mass ratio of 95%, the liquid-solid ratio is 2:1, and carry out solid-liquid separation. The solid is metastannic a...

Embodiment 2

[0023] Take a certain amount of industrial-grade sodium stannate, use pure water to prepare a sodium stannate solution with a concentration of 100g / L, add 10g of sodium stannate solution per liter of sodium stannate solution, add a 5% sodium sulfide solution by mass, and stir to react 30 minutes, then filter, heat the filtrate to 70°C, then add 20g of hydrogen peroxide with a mass ratio of 30%-50% per liter of sodium stannate solution, stir and react for 30 minutes, and then raise the temperature to 80 Stir and react at -90°C for 20 minutes, remove excess hydrogen peroxide, cool the reaction solution to room temperature, filter, add reagent grade hydrated tin hydroxide to the filtrate at a rate of 5 g per liter of filtrate, stir and adsorb for 1 hour, filter to obtain purified sodium stannate solution; add sodium dodecyl sulfate at a rate of 0.5 g per liter of sodium stannate solution, heat up to 80°C, start stirring, add dropwise ammonium bicarbonate solution with a concentrat...

example 3

[0025]Take a certain amount of reagent grade sodium stannate, use pure water to configure a sodium stannate solution with a concentration of 200g / L, add sodium dodecylbenzenesulfonate at a rate of 0.1g per liter of sodium stannate solution, and heat up to 90°C, start stirring, dropwise add ammonium carbonate solution with a concentration of 100g / L, react until the pH value of the reaction solution is 9.5, stop dropping, filter to obtain hydrated tin hydroxide solid; The solid is beaten with a liquid-solid ratio of 4:1, and the pH value of the hydrated tin hydroxide slurry is adjusted to 4 with oxalic acid. At this time, the hydrated tin hydroxide has been converted into metastannic acid, and the residual carbonate has been completely decomposed into water-soluble For the stronger oxalate, wash 3 times with pure water, the liquid-solid ratio is 6:1, then wash 2 times with absolute ethanol, the liquid-solid ratio is 3:1, carry out solid-liquid separation, and the solid is carbon ...

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Abstract

The invention discloses a method for preparing micron-grade stannic oxide powder which is applicable to conductive glass, semiconductor materials, high-class ceramic colored glaze materials or electric operation. The method comprises the following steps: dropping an ammonium bicarbonate solution, an ammonium carbonate solution or a mixture solution of ammonium bicarbonate and ammonium carbonate into a reagent-grade sodium stannate solution, controlling the pH value of a reaction liquid to be within the range of 9.0-10.0 so as to prepare tin hydroxide hydrate with high-dispersity, subsequently pulping the tin hydroxide hydrate by using pure water, further conditioning the pH value of the tin hydroxide hydrate pulp so as to obtain metastannic acid, and finally putting metastannic acid solid into a high-temperature furnace to be calcined and dehydrated so as to obtain the high-purity micron-grade stannic oxide powder. According to the method disclosed by the invention, micron-grade powder can be prepared without crushing, the production process is environment-friendly, the production equipment is simple, industrialization is easy to achieve, the micron-grade stannic oxide powder product prepared by using the method disclosed by the invention is small in particle size, high in purity, single in component and capable of meeting the requirements of conductive glass, semiconductor materials, high-class ceramic colored glaze materials or electric operation.

Description

technical field [0001] The present invention relates to a preparation method of tin chemical products, in particular to a preparation method of tin dioxide, more specifically to a micron-scale tin dioxide suitable for conductive glass, semiconductor materials, high-end ceramic color glazes or electricians. The preparation method of tin powder. Background technique [0002] Tin dioxide is an important tin chemical product, which is widely used in ceramic color glaze, conductive glass, nano-indium tin metal oxide, semiconductor materials, electronic contacts, electrical appliances, gas sensors, catalysts and other industries. It can be seen from the published literature that the preparation methods of tin dioxide mainly include the chemical synthesis method using tin-containing waste as raw material and the nitric acid method or high-temperature gasification method using tin ingot as raw material; Chinese patent CN102102150A discloses a A method for preparing tin dioxide from...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02
Inventor 高东瑞岳都元谭泽
Owner GUANGDONG GUANGHUA SCI TECH