Method for preparing micron-grade stannic oxide powder

A tin dioxide, micron-level technology, applied in tin oxide and other directions, can solve the problems of incomplete reaction, high production cost, long process route, etc., and achieve the effect of simple production equipment, prevention of agglomeration polymerization, and easy agglomeration polymerization.

Active Publication Date: 2014-03-12
GUANGDONG GUANGHUA SCI TECH
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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 produ

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  • Method for preparing micron-grade stannic oxide powder

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Example Embodiment

[0020] Example 1

[0021] Take a certain amount of reagent-grade sodium stannate, prepare it with pure water to form a sodium stannate solution with a concentration of 50g / L, heat the water bath to 60 ℃, turn on the stirring, add dropwise ammonium bicarbonate solution with a concentration of 100g / L, and react to The pH 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-to-solid ratio of 4:1, and adjust the pH value of the hydrated tin hydroxide slurry with nitric acid At this time, the hydrated tin hydroxide has been converted into metastannic acid, and the remaining sodium carbonate has been completely decomposed into more water-soluble nitrates, and washed with pure water for 5 times. The liquid-solid ratio is 3:1. Then wash with 95% ethanol with a mass ratio of 95%, liquid-solid ratio is 2:1, solid-liquid separation, the solid is tin dioxide precursor m...

Example Embodiment

[0022] Example 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 per liter of sodium stannate solution to a sodium sulfide solution with a mass ratio of 5%, and stir to react 30 minutes, then filter, heat the filtrate to 70℃, add 30%-50% hydrogen peroxide in the proportion of 20g per liter of sodium stannate solution, stir and react for 30 minutes, then raise the temperature to 80 Stir and react at -90°C for 20 minutes. The excess hydrogen peroxide is removed. Cool the reaction solution to room temperature and filter. Add reagent grade hydrated tin hydroxide to the filtrate at a rate of 5g per liter of filtrate. Stir and absorb for 1 hour. After filtration, it is purified. Sodium stannate solution; add sodium lauryl sulfate at the ratio of 0.5g per liter of sodium stannate solution, heat to 80°C, turn on stirring, add dropwise ammonium bicarbonate solution with a conce...

Example Embodiment

[0024] Example 3

[0025] Take a certain amount of reagent-grade sodium stannate and prepare a 200g / L sodium stannate solution with pure water. Add 0.1g sodium dodecylbenzene sulfonate per liter of sodium stannate solution, and heat to Start stirring at 90°C, add dropwise ammonium carbonate solution with a concentration of 100g / L, react until the pH of the reaction solution is 9.5, stop the dropwise addition, filter to obtain hydrated tin hydroxide solid; use pure water to obtain hydrated tin hydroxide The solid is beaten with a liquid-solid ratio of 4:1, and the pH 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 remaining carbonate has been completely decomposed into water-soluble Oxalate, which is more flexible, is washed with pure water for 3 times, the liquid-solid ratio is 6:1, and then washed with absolute ethanol 2 times, the liquid-solid ratio is 3:1, and sol...

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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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IPC IPC(8): C01G19/02
Inventor 高东瑞岳都元谭泽
Owner GUANGDONG GUANGHUA SCI TECH
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