Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof

A low-volatility, antimony dry powder technology, used in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems affecting the appearance and use of products, the finished product has micropores, and the surface is not smooth, and achieves excellent high-temperature heating performance. The effect of high adhesion and large surface area

Active Publication Date: 2015-08-12
锡矿山闪星锑业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its coarse particle size, antimony trioxide cannot be compared with colloidal antimony pentoxide or colloidal antimony trioxide dry powder as a flame retardant additive
The preparation method of colloidal antimony trioxide usually adopts antimony trioxide to be dissolved in an organic solvent, and then the colloidal antimony trioxide in the organic medium is obtained by replacement, but because it contains an organic carbon source, it will be carbonized and blackened at high temperature, and Colloids contain large amounts of water or organic solvents, which limit their use in many applications
The making of existing antimony pentoxide dry powder generally all is to make sol earlier, then drying obtains, because antimony pentoxide is with Sb 2 o 5 3.5H 2 It exists in the form of O, that is, the crystal water accounts for about 16.3%. This part of crystal water will decompose and volatilize when heated at high temperature. When it is added as a flame retardant additive under high temperature heating conditions, it will cause micropores in the finished product and rough surface. , dull phenomenon, affecting product appearance and use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of antimony pentoxide hydrosol: Add 584mL water into a beaker, start stirring, add 0.7g phosphoric acid, then add 146g Sb 2 o 3 Slurry, then dropwise add 131.4gH 2 o 2 (concentration is 27.5wt%), at 30 ℃, react for 90min, get colloidal Sb 2 o 5 615mL, of which: Sb 2 o 5 : 259.2g / L, Sb 2 o 3 : 0.28g / L.

[0029] Preparation of colloidal antimony oxide dry powder with low volatility at high temperature:

[0030] (1) Reduction: At a temperature of 30°C, adjust the pH value of 615mL of antimony pentoxide hydrosol to 7.1 with NaOH, then add 14.6g of hydrazine hydrate for partial reduction, and react at 80°C for 30 minutes to obtain antimony oxide sol 600mL, of which: Sb 2 o 5 : 199.78g / L, Sb 2 o 3 : 59.48g / L;

[0031] (2) Removal of alkali metal ions: Use cation exchange resin at 30°C for 30 minutes to remove Na in the antimony oxide sol obtained in step (2). + , the pH value in the sol after ion exchange is 6.0;

[0032](3) Drying: Spray-dry the ...

Embodiment 2

[0035] Preparation of antimony pentoxide hydrosol: Add 1460mL water into a beaker, start stirring, add 4.4g phosphoric acid, then add 292g Sb 2 o 3 Slurry, then add 292g H 2 o 2 (concentration is 27.5wt%), at 50 ℃, reacted for 120min to get colloidal Sb 2 o 5 1600mL, of which, Sb 2 o 5 : 199.2g / L, Sb 2 o 3 : 0.27g / L.

[0036] Preparation of colloidal antimony oxide dry powder with low volatility at high temperature:

[0037] (1) Reduction: At a temperature of 40°C, adjust the pH value of 1600mL of antimony pentoxide hydrosol to 7.5 with KOH, then add 35.0g of hydrazine hydrate for partial reduction, and react at 90°C for 50 minutes to obtain antimony oxide sol 1550mL, of which: Sb 2 o 5 : 155.48g / L, Sb 2 o 3 : 45.12g / L;

[0038] (2) Removal of alkali metal ions: use cation exchange resin at 45°C for 40 minutes to remove K in the antimony oxide sol obtained in step (2) + , the pH value in the sol after ion exchange is 6.5;

[0039] (3) Drying: Spray-dry the ant...

Embodiment 3

[0042] Preparation of antimony pentoxide hydrosol: Add 4664mL water into a beaker, start stirring, add 17.5g phosphoric acid, then add 583g Sb 2 o 3 Slurry, then dropwise add 549.7g H 2 o 2 (Concentration is 35wt%), at 90°C, react for 180min to get colloidal Sb 2 o 5 4850mL, of which, Sb 2 o 5 : 131.1g / L, Sb 2 o 3 : 0.25g / L.

[0043] Preparation of colloidal antimony oxide dry powder with low volatility at high temperature:

[0044] (1) Reduction: At a temperature of 50°C, adjust the pH value of 4850mL of antimony pentoxide hydrosol to 8.0 with NaOH, then add 87.5g of hydrazine hydrate for partial reduction, and react at 95°C for 60 minutes to obtain antimony oxide sol 4750mL, of which: Sb 2 o 5 : 102.46g / L, Sb 2 o 3 : 28.49g / L;

[0045] (2) Removal of alkali metal ions: Use cation exchange resin at 55°C for 60 minutes to remove Na in the antimony oxide sol obtained in step (2) + , the pH value in the sol after ion exchange is 7.0;

[0046] (3) Drying: Spray-d...

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PUM

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Abstract

The invention relates to colloidal antimony oxide powder low in volatility at high temperature and a preparing method thereof. The colloidal antimony oxide powder is made by 1, performing reduction, to be specific, adjusting pH value of antimony pentoxide hydrosol to 7.0 to 8.0 via alkali metal hydroxide, and adding reducing agent to allow partial reduction to obtain antimony oxide sol; 2, removing alkali metal ions, to be specific, removing the alkali metal ions in the antimony oxide sol by ion exchange; 3, performing drying, to be specific, drying the antimony oxide sol with the alkali metal ions removed, to obtain the colloidal antimony oxide powder low in volatility at high temperature. The colloidal antimony oxide powder has lower crystal water content than common colloidal antimony pentoxide powder, the high-temperature burning loss rate of the colloidal antimony pentoxide powder made by the conventional methods is decreased from 16% to 6% below, and high-temperature heating performance is excellent; when heated to 400 DEG C, the colloidal antimony oxide powder never carbonizes or blackens and has stable white appearance; the preparation process is easy to control and has no three wastes.

Description

technical field [0001] The invention relates to an antimony oxide dry powder and a preparation method thereof, in particular to a colloidal antimony oxide dry powder with low volatility at high temperature and a preparation method thereof. Background technique [0002] Antimony trioxide and antimony pentoxide are widely used as flame retardant additives for flammable materials such as plastics, chemical fibers, rubber, cotton and linen fabrics, paints and copper clad boards. Colloidal antimony pentoxide or colloidal antimony trioxide has extremely fine particle size, large surface area, high activity, high permeability, high adhesion, and does not affect the coloring degree. Therefore, it is a kind of flame retardant with excellent performance. additive. Due to its coarse particle size, antimony trioxide cannot be compared with colloidal antimony pentoxide or colloidal antimony trioxide dry powder as a flame retardant additive. The preparation method of colloidal antimony ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/00
Inventor 廖佳乐单桃云廖光荣欧阳慧刘鹊鸣金承永
Owner 锡矿山闪星锑业有限责任公司
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