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Preparation method and device of high-purity tellurium dioxide

A tellurium dioxide preparation device technology, applied in the direction of binary selenium/tellurium compounds, selenium/tellurium oxides/hydroxides, etc., can solve the problems of affecting the environment, insufficient product purity, and the lack of precise control of the amount of hydrogen peroxide, etc., to achieve The effect of improving efficiency and ensuring purity

Active Publication Date: 2018-11-13
石棉阔山新材料科技有限公司
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the preparation of high-purity tellurium dioxide is mostly prepared by 5N tellurium powder. Using nitric acid to oxidize, a large amount of acid mist will be generated during the oxidation process, which will affect the environment. Moreover, after the product oxidized by nitric acid is cracked at high temperature, there will be nitric acid residue in the product. The purity of the product is not enough, and some are oxidized by hydrogen peroxide, but due to the lack of precise control of the amount of hydrogen peroxide, local overoxidation is caused, and a large amount of tellurium trioxide is formed. Seriously affect the crystal forming rate

Method used

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  • Preparation method and device of high-purity tellurium dioxide

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Embodiment 1

[0015] Embodiment 1: as figure 1 Shown, a kind of preparation method of high-purity tellurium dioxide comprises the following steps:

[0016] a, oxidation reaction, adopt hydrogen peroxide to oxidize 4N tellurium powder, use flow pump 15 to accurately control the addition and addition rate of hydrogen peroxide, add hydrogen peroxide and 4N tellurium powder to reaction tank 1 to carry out oxidation reaction, the liquid-solid ratio of hydrogen peroxide and 4N tellurium powder The control is 2.5-3.5:1, and the concentration of hydrogen peroxide is controlled between 10% and 25%;

[0017] B, purify, add cleaning agent by the dose of 2g / L in the solution obtained after carrying out oxidation reaction in reaction tank 1, and cleaning agent is organic flocculant, after adding cleaning agent, pass stirring bar 9 and stirring blade in reaction tank 1 10 Fully stir, then stand still, and filter the sediment through a pipeline filter after standing;

[0018] c. Concentrate and crystall...

Embodiment 2

[0021] Embodiment 2: Same as the above embodiment 1, wherein the reaction tank 1 is provided with a hydrogen peroxide concentration detection sensor, and the hydrogen peroxide concentration detection sensor is wirelessly connected to the flow pump 15 .

Embodiment 3

[0022] Embodiment 3: Same as the above embodiment 1, wherein a liquid level sensor is provided at the lower part of the hydrogen peroxide storage tank 13, and a liquid replenishment pipe 21 is provided at the top of the hydrogen peroxide storage tank 13.

[0023] The present invention precisely controls the dosage of hydrogen peroxide through the flow pump 1513, so that 4N tellurium powder is oxidized in hydrogen peroxide with a concentration of 10%-25%, without causing local overoxidation and ensuring the quality of the product. During the oxidation process, the stirring rod 9 Drive the stirring blade 10 to stir, so that the 4N tellurium powder is fully contacted with hydrogen peroxide. After the oxidation is completed, add the organic flocculant through the addition funnel 17 in a dose of 2g / L, then stir, and let stand to make the iron, copper, nickel, zinc, etc. The oxides of impurities are polymerized and precipitated, filtered through the pipeline filter, and discharged th...

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Abstract

The invention discloses a high-purity tellurium dioxide preparation method and device. The method includes the steps: a, oxidizing reaction: oxidizing 4N tellurium powder by hydrogen peroxide, accurately controlling the adding quantity and the adding rate of the hydrogen peroxide by a flow pump and controlling the concentration of the hydrogen peroxide to range from 10% to 25%; b, purification: adding 2g / L of purifying agents into solution obtained after oxidizing reaction, stirring the solution and then standing for 20-30 minutes; c, concentration and crystallization: distilling and crystallizing the purified and settled solution at high temperature; d, high-temperature cracking: cracking crystals at high temperature to obtain high-purity tellurium dioxide. The usage and the concentration of the hydrogen peroxide are accurately controlled, so that peroxidation is avoided, the purity of products is ensured, and production efficiency and product yield are effectively improved.

Description

technical field [0001] The invention belongs to the technical field of high-purity tellurium dioxide production, and in particular relates to a preparation method and device of high-purity tellurium dioxide. Background technique [0002] At present, the preparation of high-purity tellurium dioxide is mostly prepared by 5N tellurium powder. Using nitric acid to oxidize, a large amount of acid mist will be generated during the oxidation process, which will affect the environment. Moreover, after the product oxidized by nitric acid is cracked at high temperature, there will be nitric acid residue in the product. The purity of the product is not enough, and some are oxidized by hydrogen peroxide, but due to the lack of precise control of the amount of hydrogen peroxide, local overoxidation is caused, and a large amount of tellurium trioxide is formed. Seriously affect the crystal forming rate. Contents of the invention [0003] The technical problem to be solved by the presen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/04
CPCC01B19/004
Inventor 曾小龙余学田李香林余涛
Owner 石棉阔山新材料科技有限公司
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