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Preparation method of ultrafine granular sodium antimonate

A technology of ultra-fine particles and sodium antimonate, applied in chemical instruments and methods, antimonate/antimonite, antimony compounds, etc., can solve the problem of large particle size deviation of sodium antimonate products, which is difficult to meet market demand, etc. problems, to achieve the effect of low preparation equipment requirements, uniform particle size, and low energy consumption

Active Publication Date: 2018-09-11
CHANGSHA YEXING ANTIMONY IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particle size deviation of the sodium antimonate product prepared by this preparation method is large, and it is difficult to meet the demand of the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of ultrafine particle sodium antimonate preparation method of the present embodiment, comprises the following steps:

[0024] (1) Mix and dissolve 1 ton of antimony trioxide, 380Kg potassium hydroxide and water at 100r / min, then heat to 60°C, then slowly add 870Kg, 27.5% (W / W%) hydrogen peroxide solution, oxidation reaction Potassium antimonate solution was obtained;

[0025] (2) Slowly add the potassium antimonate solution obtained in step 1) into a 700g / L high-concentration sodium hydroxide solution, and stir and react at 95°C and 300r / min to obtain sodium antimonate with a particle size of ≤3.0μm. cooling standby;

[0026] (3) Separating the solid and liquid of the reaction liquid in step (2), the sodium antimonate solid is slurried and washed 3 times at a mass ratio of sodium antimonate: water of 1:1.7 to remove the free hydrogen entrapped in the crude sodium antimonate Sodium oxide and / or potassium hydroxide, after washing, spin-dry and dry in a drier at 1...

Embodiment 2

[0029] A kind of ultrafine particle sodium antimonate preparation method of the present embodiment, comprises the following steps:

[0030] (1) Mix and dissolve 2 tons of antimony trioxide, 760Kg potassium hydroxide and water at 100r / min, then heat to 60°C, then slowly add 800Kg, 27.5% (W / W%) hydrogen peroxide solution, oxidation reaction Potassium antimonate solution was obtained;

[0031] (2) Slowly add the potassium antimonate solution obtained in step 1) into a 750g / L high-concentration sodium hydroxide solution, and stir and react at 80°C and 350r / min to obtain sodium antimonate with a particle size of ≤3.0μm. cooling standby;

[0032] (3) Separating the solid and liquid of the reaction liquid in step (2), the sodium antimonate solid is slurried and washed 3 times at a mass ratio of sodium antimonate: water of 1:1.7 to remove the free hydrogen entrapped in the crude sodium antimonate Sodium oxide and / or potassium hydroxide, after washing, spin-dry and dry in a drier at ...

Embodiment 3

[0035] A kind of ultrafine particle sodium antimonate preparation method of the present embodiment, comprises the following steps:

[0036] (1) Mix and dissolve 1 ton of antimony trioxide, 400Kg potassium hydroxide and water at 100r / min, then heat to 60°C, then slowly add 870Kg, 27.5% (W / W%) hydrogen peroxide solution, oxidation reaction Potassium antimonate solution was obtained;

[0037] (2) Slowly add the potassium antimonate solution obtained in step 1) into a high-concentration sodium hydroxide solution of 800g / L, stir and react at 85°C and 350r / min to obtain sodium antimonate with a particle size of ≤3.0μm, cooling standby;

[0038] (3) Separating the solid and liquid of the reaction liquid in step (2), the solid sodium antimonate is slurry washed 3 times according to the mass ratio of sodium antimonate:distilled water of 1:1.7, and the free hydrogen entrapped in the crude sodium antimonate is removed Sodium oxide and / or potassium hydroxide, after washing, spin-dry and...

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Abstract

A preparation method of ultrafine granular sodium antimonate comprises the following steps: (1) stirring and mixing antimony trioxide and potassium hydroxide with water, dissolving, heating, then adding an aqueous solution of hydrogen peroxide, and oxidizing to obtain a potassium citrate solution; (2) slowly adding the potassium citrate solution obtained by the reaction in the step 1) into a high-concentration sodium hydroxide solution of 600-800 g / L, and stirring at a high speed at 80-95 DEG C and reacting to obtain sodium antimonate having a particle diameter of less than or equal to 3.0 microns, and cooling; (3) carrying out solid-liquid separation on the reaction liquid in the step (2), carrying out slurry washing on the sodium antimonate solid with water for 2 to 3 times, spin-dryingafter washing and drying through a dryer so as to obtain the finished product ultrafine granular sodium antimonate. The ultrafine granular sodium antimonate prepared by the above preparation method has uniform particle size which is less than or equal to 3 microns, and is mainly used as a flame retardant in fabrics such as fibers and a clarifying agent for glass shells of color kinescopes and high-grade glass. The preparation process is simple; requirements on preparation equipment are low; energy consumption is low; and the product purity is high.

Description

technical field [0001] The invention relates to a preparation method of sodium antimonate, in particular to a preparation method of ultrafine particle sodium antimonate. Background technique [0002] High-grade pure sodium antimonate is widely used in opaque fillers for cast iron paints, textile flame retardants, and clarifiers for color TV picture tube glass bulbs and high-grade glass. However, the traditional chlorination method combines antimony trioxide with Hydrochloric acid is mixed to produce sodium antimonate; the sodium antimonate prepared by the above method has low purity, high impurity content, large product particle size, and large deviation, which is difficult to meet the performance requirements of the market for sodium antimonate. [0003] CN 105314676 A A method for preparing high-grade pure sodium antimonate, the method is as follows: (1) Oxidation of antimony trioxide: put antimony trioxide and sodium hydroxide into a stainless steel bucket, add distilled ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/02
CPCC01G30/023C01P2004/61
Inventor 李丙乔崔佑民曹春安汤华辉唐潇
Owner CHANGSHA YEXING ANTIMONY IND
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