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A kind of preparation method of antimony pentoxide composite dry powder

A technology of antimony pentoxide and antimony trioxide, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxyacid, antimony compounds, etc., which can solve the problem of reduced raw material utilization, allergies, and easy clogging operations Pores and other problems of personnel, to achieve good stability and improve the flame retardant effect

Inactive Publication Date: 2015-08-26
JIAXING VOCATIONAL TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Electrodialysis and ion exchange have the same disadvantages, namely long production cycle and low concentration of crude product
Moreover, it is currently difficult for our country to provide a large amount of antimonate (such as potassium pyroantimonate) industrial products required by the two methods, so the industrial production and application of these two technologies is relatively difficult
The production conversion rate of the reflux oxidation method is relatively high, and the process is simple, but when the dry powder is made into a dry powder by spray drying, the too fine powder is easy to block the pores of the operator during use, causing skin redness, allergies and other problems, which seriously damages the health of employees In addition, it is easy to cause the loss of antimony pentoxide after spray drying to make thousands of powders, which reduces the utilization rate of raw materials, and the energy consumption of spray drying is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Dissolve 60g of antimony trioxide in 720g of concentrated hydrochloric acid, control the temperature at 80°C, heat for 1.5 hours, then cool to room temperature; take the filtrate after filtration, add 0.6g of GB 2 # Antimony powder, control the temperature at 50°C for 1.5 hours of reduction reaction, then distill the filtrate, dilute the distilled antimony trichloride solution with water, and hydrolyze for 40 minutes; filter after hydrolysis, take the filter cake and wash it twice with hot water, wash Add ammonia water to the final filter cake, adjust the pH to 10, control the temperature at 100°C and carry out ammonolysis for 60 minutes to obtain a white precipitate, wash the white precipitate twice with distilled water, dry at 110°C for 16 hours, and obtain refined di antimony;

[0018] (2) Take 40g of refined antimony trioxide from step (1) and add it to water, fully dissolve it, then add 12g of stabilizer phosphoinositide, stir at 90°C at a speed of 250r / min unt...

Embodiment 2

[0021] (1) Add 40g of antimony trioxide into water, fully dissolve, then add 12g of stabilizer inositol phosphate, stir at 90°C at a speed of 250r / min until a white slurry is formed, and then Add 16g of hydrogen peroxide dropwise during heating and reflux, stir and react for 10 minutes, then continue to drop 16g of hydrogen peroxide, stir and react for 10 minutes, and finally add 16g of hydrogen peroxide and 24g polyethylene glycol dropwise at the same time, carry out oxidative reflux reaction for 15 minutes, and obtain five Antimony oxide hydrosol, wherein the mass fraction of hydrogen peroxide added is 30%; adding hydrogen peroxide three times can speed up the oxidation rate, and adding surfactant polyethylene glycol at the end can effectively disperse colloidal particles and prevent coagulation.

[0022] (2. Add 24g of zeolite powder with a particle size of 800 mesh to the antimony pentoxide hydrosol prepared in step (1), stir for 10 minutes, let stand and centrifuge to obta...

Embodiment 3

[0024] (1) Dissolve 60g of antimony trioxide in 720g of concentrated hydrochloric acid, control the temperature at 80°C, heat for 1.5 hours, then cool to room temperature; take the filtrate after filtration, add 0.6g of GB 2 # Antimony powder, control the temperature at 50°C for 1.5 hours of reduction reaction, then distill the filtrate, dilute the distilled antimony trichloride solution with water, and hydrolyze for 40 minutes; filter after hydrolysis, take the filter cake and wash it twice with hot water, wash Add ammonia water to the final filter cake, adjust the pH to 10, control the temperature at 100°C and carry out ammonolysis for 60 minutes to obtain a white precipitate, wash the white precipitate twice with distilled water, dry at 110°C for 16 hours, and obtain refined di antimony;

[0025] (2) Take 40g of refined antimony trioxide from step (1) and add it to water, fully dissolve it, then add 12g of stabilizer phosphoinositide, stir at 90°C at a speed of 250r / min unt...

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Abstract

The invention relates to a preparation method of an antimony pentoxide composite powder. The preparation method comprises the following steps: firstly, antimony trioxide is taken for refining; then the refined antimony trioxide dry powder is added into water, then creatinol-o-phosphate as a stabilizer and oxydol are added for oxidation reflux reaction, after the reaction, a reacting liquid is taken for dialysis for 2 to 3 times, redundant creation o-phosphate is removed, and an antimony pentoxide hydrosol is prepared; finally, the prepared antimony pentoxide hydrosol is added with zeolite powder, the mixture is stirred and then left to stand, precipitate is obtained through centrifugation, and the precipitate is filtered and dried so as to obtain the antimony pentoxide composite powder. The preparation method provided by the invention uses the creatinol-o-phosphate as the stabilizer, and the creatinol-o-phosphate contains a plurality of hydroxies and two inflaming retarding elements N and P, so that the stabilizing effect is good, the flame-retardant effect of the colloid of antimony pentoxide is improved, a zeolite powder is adopted for adsorbing the colloid of antimony pentoxide, so as to prepare the antimony pentoxide-zeolite powder composite powder, during the preparing process, the problem of much loss of antimony pentoxide dry powder during the drying process caused by relatively fine antimony pentoxide dry powder can be solved.

Description

technical field [0001] The invention relates to the field of chemical product preparation, in particular to a method for preparing antimony pentoxide composite dry powder. Background technique [0002] Colloidal antimony pentoxide can be used as a flame retardant additive in rubber, plastic, fiber, fabric, paint, paper, etc. In addition, colloidal antimony pentoxide can also be used as a catalyst component, a pigment component, and as a surface treatment agent for plastics and metals to improve the surface hardness and wear resistance of materials and enhance corrosion resistance. According to different raw materials, the preparation of colloidal antimony pentoxide can be divided into two categories: direct method and indirect method. The direct method directly obtains colloidal antimony pentoxide through processes such as ore alkali leaching, catalytic oxidation, solid-liquid separation, neutralization and peptization. The preparation process of this method is complicated...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00
CPCC01G30/005
Inventor 秦国栋庞权如
Owner JIAXING VOCATIONAL TECHN COLLEGE
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