Preparation method of ammonium persulfate crystal

A technology of ammonium persulfate and ammonium sulfate, applied in the direction of peroxyhydrate/peroxyacid, etc., can solve the problems such as the average particle size of ammonium persulfate crystals and the anti-caking performance to be further improved.

Active Publication Date: 2021-04-20
TIANJIN UNIV
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  • Abstract
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Problems solved by technology

[0003]CN109665498A proposes a kind of method for preparing ammonium persulfate crystal, concrete operation steps are: provide the mixture liquid of ammonium persulfate and ammonium sulfate, in the described mixture liquid The mass concentration ratio of ammonium persulfate and ammonium sulfate is 1: (2-3); when the temperature of the mixed material liquid is controlled to be 20-25°C, ammonium persulfate seed is added, and then the cooling rate is 5-15°C / h Cool down to -2~-6°C to obtain ammonium persulfate crystals, and the particle size of the obtained ammonium persulfate crystals is greater than 500 μm; however, the average particle size and anti-caking performance of the ammonium persulfate crystals obtained by this method need to be further improved

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  • Preparation method of ammonium persulfate crystal
  • Preparation method of ammonium persulfate crystal
  • Preparation method of ammonium persulfate crystal

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Embodiment 1

[0049] The present embodiment provides a kind of crystallization method of ammonium persulfate crystal, comprises the steps:

[0050] (1) Ammonium persulfate and ammonium sulfate are dissolved in distilled water according to the mass ratio of 1:1.25 to make a mixture liquid, and the concentration of ammonium persulfate is 0.4g / mL;

[0051] (2) Place the mixed material liquid obtained in step (1) in a crystallizer with a draft tube, turn on the propeller stirrer, control the stirring rate to 230rpm, and control the temperature of the mixed material liquid at 30°C to add particle size Ammonium persulfate seed crystals of 80-100 mesh, the concentration of the seed crystals in the mixed material liquid is 6mg / mL, and then the temperature is slowly raised to 0.5°C, and then cooled to -5°C at a cooling rate of 10°C / h for cooling and crystallization to obtain crystalline mixture;

[0052] (3) Filter the crystallization mixture obtained in step (2) to obtain a solid, then wash and dr...

Embodiment 2

[0067] The only difference from Example 1 is that the concentration of ammonium sulfate is 0.8g / mL, and the rest of the preparation methods are the same as in Example 1.

[0068] The ammonium persulfate crystal obtained in the present embodiment adopts the same test method as in Example 1, and it can be known that the purity of the ammonium persulfate crystal obtained is 98%, and the average particle diameter is 822 μm.

Embodiment 3

[0070] The only difference from Example 1 is that the concentration of ammonium persulfate is 0.5g / mL, the concentration of ammonium sulfate is 0.625g / mL, and the rest of the preparation methods are the same as in Example 1.

[0071] The ammonium persulfate crystal obtained in the present embodiment adopts the same test method as in Example 1, and it can be known that the purity of the ammonium persulfate crystal obtained is 99%, and the average particle diameter is 831 μm.

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Abstract

The invention provides a preparation method of an ammonium persulfate crystal. The preparation method comprises the following steps of: adding an ammonium persulfate seed crystal into a mixed solution of ammonium persulfate and ammonium sulfate at 25-35 DEG C under the stirring action of a push-type stirrer with a guide cylinder to carrying out seeding; slowly heating to 0.5-1 DEG C; and cooling to -3 to -10 DEG C at a cooling rate of 3-18 DEG C / h, and carrying out cooling crystallization to obtain the ammonium persulfate crystal. The average particle size of the ammonium persulfate crystal is greater than 800 microns. According to the preparation method of the ammonium persulfate crystal of the present invention, the push-type stirrer with the guide cylinder is used, the micro-amplitude 0.5-1 DEG C heating process is performed, and a cooling range is extended; and the growth and crystallization process of the crystal can be well controlled through the synergistic effect of a plurality of factors, and therefore, the purity, the uniformity and the average particle size of the crystal can be increased, the anti-caking performance of the ammonium persulfate crystal can be improved, and the application range of the product is greatly extended.

Description

technical field [0001] The invention belongs to the field of industrial crystallization, and relates to a method for preparing ammonium persulfate crystals, in particular to a method for crystallizing ammonium persulfate crystals with a purity higher than 99% and an average particle diameter higher than 800 μm. Background technique [0002] Ammonium persulfate, also known as ammonium persulfate, ammonium persulfate, the English name is Ammonium Persulfate, referred to as APS, molecular formula (NH4) 2 S 2 o 8 , in the form of white monoclinic crystals or white powdery crystals, easily soluble in water. Dry ammonium persulfate has good stability, and it is easy to be damp and agglomerated in humid air. After absorbing moisture, ammonium persulfate can undergo hydrolysis reaction in aqueous solution; when heated or under the catalysis of silver salt and other substances, it can undergo oxidative decomposition and release a large amount of heat energy. Ammonium persulfate i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B15/08
Inventor 龚俊波郭石麟郭盛争陈明洋王平生张俊杰赵建威刘荣泉刘思询尹秋响侯宝红王静康
Owner TIANJIN UNIV
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