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Method for preparing reagent-grade grade stannic oxide powder

A technology of tin dioxide and reagent grade, applied in the field of preparation of tin chemical products, can solve the problems of high impurity content, unenvironmentally friendly process, restricted use, etc., achieve uniform powder particle size, reduce sodium ion content, and reduce the production process. Environmentally friendly effect

Active Publication Date: 2014-03-05
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 The method for preparing tin dioxide from tin waste as raw material 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 to The undersize is washed; (3) the washings are filtered, the filter residue is leached with sodium hydroxide solution and an oxidizing agent, the leachate is filtered, and the filtrate is a sodium stannate solution; (4) carbon dioxide is passed into the sodium stannate solution, filtered, Washing obtains the tin dioxide product; This preparation method process route is long, and the demand to carbon dioxide is big, and utilization rate is low, and actual consumption is 10-50 times of theoretical calculation amount, and this is little in industrial feasibility, 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 Only after crushing can it reach 10um fine tin dioxide products, 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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  • Method for preparing reagent-grade grade stannic oxide powder

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Embodiment 1

[0024] Take a certain amount of reagent grade sodium stannate, use pure water to prepare a sodium stannate solution with a concentration of 50g / L, add ethanol to the sodium stannate solution at a rate of 5g of ethanol per liter of sodium stannate solution, and heat in a water bath To 50-60 ° C, while stirring for 30 minutes, pass into carbon dioxide, react until the pH value of the reaction solution is 9.0, filter to obtain hydrated tin hydroxide solid, use pure water to obtain the hydrated tin hydroxide solid at a liquid-solid ratio of 4: 1 is beaten, and the pH value of the hydrated tin hydroxide slurry is adjusted to 2 with nitric acid. At this time, the hydrated tin hydroxide has been converted into metastannic acid, and the residual sodium carbonate has been completely decomposed into more water-soluble nitrates. Pure water was poured and washed 5 times, the liquid-solid ratio was 4:1, and then solid-liquid separation was carried out, and the sodium ion content of the obta...

Embodiment 2

[0026] Take a certain amount of reagent grade sodium stannate, use pure water to prepare a sodium stannate solution with a concentration of 100g / L, and add ethylene glycol to the sodium stannate solution at a rate of 20g of ethylene glycol per liter of sodium stannate solution , heated to 70°C in a water bath while stirring for 40 minutes, and then introduced carbon dioxide until the pH value of the reaction solution was 10.0, filtered to obtain a hydrated tin hydroxide solid, and purified the obtained hydrated tin hydroxide solid with pure water at a liquid-to-solid ratio 5:1 for beating, adjust the pH value of the hydrated tin hydroxide slurry to 2.5 with formic acid, at this time, the hydrated tin hydroxide has been converted into metastannic acid, and the residual sodium carbonate has been completely decomposed into more water-soluble formic acid Salt, pouring and washing with pure water for 5 times, the liquid-solid ratio is 3:1, and then performing solid-liquid separation...

Embodiment 3

[0028] 1, the preparation of hydrated tin hydroxide:

[0029]Put tin flower and sodium hydroxide into the reaction kettle at a mass ratio of 1:1, then add pure water into the reaction kettle so that the concentration of sodium hydroxide is 100g / L, then raise the temperature to 95°C, inject ozone, and keep The pressure in the reaction kettle is 0.1Mpa, and the concentration of free sodium hydroxide in the reaction solution in the reaction kettle is detected while reacting. When the free sodium hydroxide in the reaction solution in the reaction kettle is detected to be 50g / L, the tin-containing alkaline solution is taken out , filter out the unreacted tin slag, then put the tin-containing alkaline solution into the synthesis reaction kettle, turn on the stirring device, and feed carbon dioxide gas. When the pH value of the reaction solution is detected to be 9.0, stop feeding carbon dioxide. Filter the reaction solution to obtain a white solid, wash the white solid with pure wat...

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Abstract

The invention provides a method for preparing reagent-grade grade stannic oxide powder, which is applicable to chemical analysis, conductive glass, semiconductor materials, and high-end ceramic colored glaze materials. The method comprises steps of firstly inletting carbon dioxide into reagent-grade sodium stannate in the presence of a certain proportion of alcohol dispersing agent, and controlling the pH value of reaction liquid so as to prepare hydronium stannic oxide; then preparing the hydronium stannic oxide into thick liquid through pure water, adjusting the pH value of the thick liquid of the hydronium stannic oxide through strong acid so as to obtain metastannic acid; finally, placing the metastannic acid solid in a high temperature furnace for calcining and dehydrating, thereby obtaining high-purity nanoscale stannic oxide powder. According to the method, nanoscale powder can be obtained without grinding, the production process is environment-friendly, the production equipment is simple, and the method is beneficial to industrialization. The product prepared by the method has high purity and single component, and can meet the requirements of various industries such as chemical analysis, conductive glass, semiconductor materials, and high-end ceramic colored glaze materials.

Description

Technical field [0001] The present invention involves a method of preparation of a tin chemical product, especially the preparation method of a tin dioxide, and it is more specifically involved in a reagent level two suitable for chemical analysis, conductive glass, semiconductor materials, and high -end ceramic glaze.Preparation method of tin oxide powder. Background technique [0002] Tin dioxide is an important tin chemical product, which is widely used in ceramic color glaze, conductive glass, nano -tin tin metal oxides, semiconductor materials, electronic tentacles, electrical appliances, gas -sensitive sensors, catalysts and other industries.It can be seen from the published documents that the preparation methods of tin dioxide mainly include chemical synthesis method based on tin -containing waste and high temperature gasification method based on tin ingot as raw materials; Chinese patent CN102102150A discloses a kind of containing containing containingThe method of prepar...

Claims

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Application Information

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IPC IPC(8): C01G19/02
Inventor 高东瑞翟文辉谭泽
Owner GUANGDONG GUANGHUA SCI TECH
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