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Colloidal antimony oxide dry powder with low volatility at high temperature and preparation method thereof

A low-volatility, antimony dry powder technology, applied in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems that affect the appearance and use of the product, 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: 2016-06-01
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 a...

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 dropwise add 292gH 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 ...

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, add dropwise 549.7gH 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-dry the ...

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PUM

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Abstract

A low-volatility colloidal antimony oxide dry powder at high temperature and its preparation method. The colloidal antimony oxide dry powder is prepared according to the following method: (1) Reduction: adjust the pH value of antimony pentoxide hydrosol with alkali metal hydroxide After reaching 7.0 to 8.0, add a reducing agent for partial reduction to obtain antimony oxide sol; (2) Removal of alkali metal ions: remove alkali metal ions in the antimony oxide sol obtained in step (1) by ion exchange; (3) dry : drying the antimony oxide sol after removing alkali metal ions to obtain colloidal antimony oxide dry powder with low volatility at high temperature. The crystallization water content of the colloidal antimony oxide dry powder of the present invention is lower than that of the commonly used colloidal antimony pentoxide dry powder, and the ignition loss rate at high temperature is reduced from 16% to less than 6% of the colloidal antimony pentoxide dry powder prepared by conventional methods, and has excellent high temperature Heating performance; when heated to 400°C, it will not carbonize and turn black, and has a stable white appearance; the preparation process is easy to control, and there is no three wastes generated.

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 Patents(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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