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A method for preparing ultrafine antimony oxides by solution atomization

A technology of antimony oxide and solution atomization, which is applied in chemical instruments and methods, antimony compounds, antimony oxide/antimony hydroxide/antimony oxyacid, etc., can solve the problems of large equipment investment and long preparation process, and achieve Requires simple, uniform and fine particles, high purity effect

Active Publication Date: 2017-07-14
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Sb Prepared by Arc and Plasma 2 o 3 The purity of the powder is relatively high, but the preparation process is long and the investment in equipment is large

Method used

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  • A method for preparing ultrafine antimony oxides by solution atomization
  • A method for preparing ultrafine antimony oxides by solution atomization
  • A method for preparing ultrafine antimony oxides by solution atomization

Examples

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Effect test

Embodiment 1

[0058] A kind of method that the solution atomization method of the present invention prepares superfine antimony oxide, its process flow chart is as follows figure 1 As shown, it specifically includes the following steps:

[0059] (1) Weigh 50.00g SbCl 3 Solid, add 4.5mol / L hydrochloric acid solution diluted with pure water to prepare 0.55mol / L SbCl 3 solution;

[0060] (2) utilize ozone gas to above-mentioned SbCl 3 The solution is oxidized and the potential of the solution is detected. When the potential of the solution is about 0.75V, the ozone is stopped;

[0061] (3) Use an ultrasonic atomizer to atomize the above-mentioned oxidized solution and control the atomization flow rate to 30mL / h, and use a vacuum pump to draw negative pressure on the reaction device, so that the atomized solution enters the vertical tubular resistance furnace, Thermal decomposition reaction is carried out at a temperature of 500°C to obtain antimony oxide powder;

[0062] (4) The antimony ...

Embodiment 2

[0066] A kind of method that the solution atomization method of the present invention prepares superfine antimony oxide, its process flow chart is as follows figure 1 As shown, it specifically includes the following steps:

[0067] (1) Prepare 400mL of 5.0mol / L hydrochloric acid in a beaker, heat it in a water bath to the set temperature, then weigh 40.00g of stibnite and add it to the beaker. During the experiment, use a magnetic stirrer to stir and control the stirring speed to extract During the process, continuously feed ozone gas into the solution, react for 4 hours, and filter to obtain the leachate after the reaction is completed;

[0068] (2) Utilize ozone gas to carry out oxidation operation to above-mentioned leaching liquid solution and detect solution potential, when solution potential is about 0.75V, stop feeding ozone;

[0069] (3) Use an ultrasonic atomizer to atomize the above-mentioned oxidized solution and control the atomization flow rate to be 50mL / h, and ...

Embodiment 3

[0074] A kind of method that the solution atomization method of the present invention prepares superfine antimony oxide, its process flow chart is as follows figure 1 As shown, it specifically includes the following steps:

[0075] (1) Weigh 50.00g SbCl 3 Solid, added to the 4.5mol / L hydrochloric acid solution diluted with pure water to prepare 0.55mol / L SbCl 3 solution;

[0076] (2) Use oxygen gas to treat the above-mentioned SbCl 3 The solution is oxidized and the potential of the solution is detected. When the potential of the solution is about 0.75V, stop feeding oxygen;

[0077] (3) Use an ultrasonic atomizer to atomize the above-mentioned oxidized solution and control the atomization flow rate to 50mL / h, and use a vacuum pump to draw negative pressure on the reaction device, so that the atomized solution enters the vertical tubular resistance furnace. Perform thermal decomposition reaction at a temperature of 900°C to obtain antimony oxide powder;

[0078](4) The an...

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Abstract

The invention discloses a method of using a solution atomization method to prepare superfine Sb oxide. The method comprises the following steps: (1) trivalent Sb is added into a hydrochlric solution to prepare a Sb solution with the molar concentration of 0.05-0.8 mol / L; (2) clean oxidant is used to oxidize the solution obtained in step (1), and a pentavalent Sb solution is obtained; (3) Sb oxide powder is obtained after spray pyrolysis of the pentavalent Sb solution is obtained in step (2). According to the invention, trivalent Sb solution is used as a raw material, superfine Sb oxide powder materials are directly prepared through oxidization and spray pyrolysis, and the technological process is simple. Alternatively, lixivium from the conventional process of using an acid method in antimony smelting is directly used as the raw material. Therefore, the process of preparing the superfine Sb oxide powder materials is shortened; the conventional metallurgical process and the material preparation process are effectively combined; added value of products from conventional non-ferrous metal metallurgy is significantly increased; recycling of hydrochloric acid from lixivium is realized.

Description

technical field [0001] The invention belongs to the technical field of powder material preparation, and in particular relates to a method for preparing ultrafine antimony oxide by solution atomization. Background technique [0002] Antimony reacts with oxygen to form a series of oxides, such as Sb 2 o 5 , Sb 6 o 13 , Sb 2 o 4 , Sb 2 o 3 , Sb 2 O, SbO 2 And gaseous SbO, among which the most widely studied and applied is Sb 2 o 5 and Sb 2 o 3 . Antimony oxide has been used in industries such as enamel, rubber, plastics and weaving and dyeing as covering agent, filler and catalyst. In recent years, the application of antimony oxide in flame retardant and fire protection has developed rapidly, and its application prospects in optical and electrical technologies are very optimistic. [0003] According to different raw materials, the preparation of colloidal antimony pentoxide can be divided into direct method and indirect method. The direct method is to directly p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00
CPCC01G30/005C01P2002/72C01P2004/03C01P2004/61C01P2004/62C01P2006/80
Inventor 田庆华辛云涛郭学益王恒利李栋
Owner CENT SOUTH UNIV
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