Preparation method of sodium pyroantimonate with reduced grain size

A technology of sodium pyroantimonate and particle size, applied in the field of flame retardant materials, can solve the problem of excessive particle size of sodium pyroantimonate, and achieve high yield, no three-waste pollution, and good comprehensive recovery.

Active Publication Date: 2019-07-16
YIYANG SHENGLI CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the technical problem that the particle size of the existing sodium pyroantimonate is too large, the invention provides a pre

Method used

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  • Preparation method of sodium pyroantimonate with reduced grain size
  • Preparation method of sodium pyroantimonate with reduced grain size
  • Preparation method of sodium pyroantimonate with reduced grain size

Examples

Experimental program
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Effect test

Embodiment 1

[0061] Add 50kg of antimony trioxide and 200L of pure water into a 500L reactor, stir and mix evenly, then add 70L of hydrogen peroxide (concentration: 30%), stir evenly, control the pH to 7, and heat up to 70°C for constant temperature reaction (oxidation reaction) 2 Hours, after the reaction is over, the temperature is raised to 90°C, and sodium hydroxide (dosage is 0.6 times that of antimony trioxide) and surfactant sodium lauryl sulfate (0.5Kg) are added while stirring, and the constant temperature reaction (90°C )

[0062] After 1.5 hours, after the reaction, the filter cake was ultrasonically dispersed (in a buffer solution with a pH of 8-9 for 30 minutes), then cooled and crystallized, washed with pure water until the washing liquid was neutral, centrifuged, the liquid was reused, and washed with water The solid product is then dried at 80-90°C to obtain sodium pyroantimonate.

[0063] After testing, see the test results figure 1 , the particle size of sodium pyroanti...

Embodiment 2

[0065] Add 50kg of antimony trioxide and 200L of pure water into a 500L reactor, stir and mix well, then add 70L of hydrogen peroxide, stir well, adjust the pH to 13 with sodium hydroxide, heat up to 70°C and react at a constant temperature for 2 hours, after the reaction Raise the temperature to 90°C, add sodium hydroxide (0.6 times that of antimony trioxide) and surfactant sodium lauryl sulfate (0.5Kg) while stirring, and react at constant temperature for 1.5 hours. After the reaction, the filter cake is ultrasonically Dispersion (ultrasonic dispersion in a buffer solution with a pH of 8.0-9.0), cooling and crystallization, centrifugation, liquid reuse, washing the solid product with water, and drying at 80-90°C to obtain sodium pyroantimonate.

[0066] After testing, see the test results figure 2 , The particle size of sodium pyroantimonate is 6.06um, the whiteness is 78%, and the pH value is 7.32. (Note: The whiteness is tested by a whiteness tester, and the pH value is ...

Embodiment 3

[0068] Add 50kg of antimony trioxide and 200L of pure water into a 500L reactor, stir and mix well, then add 70L of hydrogen peroxide, stir evenly, adjust the pH to 2, raise the temperature to 70°C and react at a constant temperature for 2 hours, and then raise the temperature to 90°C after the reaction. Add sodium hydroxide (addition amount is 0.6 times of antimony trioxide) and surfactant sodium lauryl sulfate (0.5Kg) while stirring, constant temperature reaction 1.5 hours, after reaction finishes filter cake ultrasonic dispersion (in described Dispersed in the buffer solution), then cooled to crystallize, centrifuged, the liquid was reused, the solid product was washed with water and then dried at 80-90°C to obtain sodium pyroantimonate.

[0069] After testing, see the test results image 3 , the particle size of sodium pyroantimonate is 1.45um, the whiteness is 98%, and the pH value is 7.12. (Note: The whiteness is tested by a whiteness tester, and the pH value is tested ...

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Abstract

The invention discloses a preparation method of sodium pyroantimonate with a reduced grain size. The preparation method comprises the following steps: step (1), subjecting antimony trioxide and hydrogen peroxide to oxidation in advance; and step (2), after the reaction in the step (1) is finished, adding a surfactant and sodium hydroxide to the reaction system for precipitation reaction, and carrying out solid-liquid separation, washing and drying treatment after the precipitation reaction is finished, so as to obtain sodium pyroantimonate with a fine grain size. According to the preparation method of sodium pyroantimonate with a reduced grain size, antimony trioxide, as a raw material, is fully oxidized with hydrogen peroxide, the surfactant is added to promote the grain refinement, and then a sodium hydroxide solution is added for sufficient reaction so as to generate a precipitate, and the precipitate is washed, so that the final product superfine sodium pyroantimonate is obtained.Compared with a traditional process, the preparation method of sodium pyroantimonate with a reduced grain size adopts steps of firstly adding hydrogen peroxide for oxidization and then adding sodium hydroxide for reaction, while the traditional process adopts steps of firstly adding sodium hydroxide and then adding hydrogen peroxide. Sodium pyroantimonate obtained by the traditional process generally has a grain size of about 40 micron, while the sodium pyroantimonate obtained by the preparation method disclosed in the invention is significantly improved in grain size.

Description

technical field [0001] The invention relates to a preparation method of ultrafine sodium pyroantimonate, which is widely used in flame-retardant materials and belongs to the technical field of flame-retardant materials. Background technique [0002] Sodium pyroantimonate is a white powder with granular crystals and equiaxed crystals. It is resistant to high temperature and does not decompose at 1000°C. It can be used as a high-grade glass clarifier and decolorizer, a flame retardant for plastics and textiles, and for enamel and ceramics. Opalescent and opaque coatings for foundry paints. The production capacity of antimony-based processed products in my country is second only to antimony oxide. With the development of science and technology, glass is required to clarify and prevent fogging at a higher level, and plastics have better flame retardant effects. Correspondingly, higher requirements are placed on the performance of sodium antimonate. Particle size is one of the ...

Claims

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Application Information

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IPC IPC(8): C01G30/02C08K3/24C03C1/00
CPCC01G30/023C01P2004/52C01P2004/61C03C1/004C08K3/24
Inventor 杨喜云曹升李计深唐磊徐徽石西昌
Owner YIYANG SHENGLI CHEM IND
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