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Preparation method of high-purity low-nitrogen potassium persulfate

A potassium persulfate, high-purity technology, applied in the direction of peroxyhydrate/peroxyacid, etc., can solve the problems of low production capacity, excess, instability, etc., and achieve the effects of reducing decomposition opportunities, improving productivity, and reducing costs

Inactive Publication Date: 2016-05-11
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The weak point of its prior art is reflected in: 1, potassium persulfate is used for ammonium persulfate synthesis and obtains, causes wherein NH4 + Large excess; 2. This is the main reason for potassium persulfate nitrogen exceeding the standard. Potassium persulfate is a strong oxidant and unstable. During the purification process, the operating temperature should not exceed 60°C, otherwise it will decompose into potassium sulfate and reduce the content of potassium persulfate.
[0005] Utility model patent CN201020203455.0 has developed a device for preparing high-purity potassium persulfate, but its production capacity is low and it is difficult to be used in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of high-purity low-nitrogen potassium persulfate, the steps are as follows:

[0022] ⑴In a pressure vessel, add 15L of distilled water, heat it to 20-50°C, add 2-5Kg of potassium persulfate, install a decompression device and a stirring device, carry out vacuum distillation under stirring, control the pressure at 10-20mmHg, and control the temperature At 40-50°C, the stirring speed is 100-150 rpm, about 1-2L of water is evaporated, and the heating is stopped;

[0023] (2) Pour the solution into a crystallization tank, cool the outside with ice water, a large amount of crystals are precipitated, filter the crystals, and wash with a small amount of cold ethanol once or twice;

[0024] (3) In the dissolving tank, add 7L of distilled water, add the above-mentioned crystals, heat to 20-50°C to dissolve them all, filter, take the clear liquid, pour it into the above-mentioned distillation device, and continue to distill under reduced pressure. When 3L of ...

Embodiment 2

[0026] A preparation method of high-purity low-nitrogen potassium persulfate, the steps are as follows:

[0027] ⑴In a pressure vessel, add 15L distilled water, 3-5Kg potassium persulfate, install a decompression device and a stirring device, carry out vacuum distillation under stirring, control the pressure at 20-30mmHg, control the temperature at 20-50°C, and stir The speed is 160 rpm, about 2-3L of water will be steamed, and the heating will be stopped;

[0028] ⑵ Pour the solution into a crystallization tank, cool with ice water, a large amount of crystals are precipitated, dry the crystals, and wash twice with a small amount of cold water;

[0029] (3) In the dissolving tank, add 6L of distilled water, add the above-mentioned crystals, heat to 60°C to dissolve them all, add 20g of activated carbon, stir for 2 minutes, filter while hot, put the filtrate into the concentration tank, keep at 60°C, concentrate for 2-3 Put it into a crystallization tank, cool with ice water t...

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Abstract

The invention relates to a preparation method of high-purity low-nitrogen potassium persulfate. The method includes the steps of: (1) adding distilled water into a pressure vessel, conducting heating to 20-50DEG C, adding 2-5Kg of potassium persulfate, mounting a decompression device and a stirring device, conducting decompression distillation under stirring, controlling the pressure at 10-20mmHg, the temperature at 20-50DEG C and the stirring speed at 100-160rpm, distilling off about 1 / 7-1 / 5 of water, and stopping heating; (2) pouring the solution into a crystallization tank, conducting ice water cooling externally, precipitating crystals, filtering the crystals, and performing washing with cold ethanol 1-2 times; and (3) carrying out dissolution, washing and crystallization again, and finally performing drying in a vacuum drying box at 60DEG C so as to obtain low-nitrogen potassium persulfate. The method provided by the invention adopts low temperature and decompression operation, accelerates the concentration speed, reduces the decomposition opportunity of potassium persulfate, and increases the yield.

Description

technical field [0001] This patent belongs to the field of high-purity chemical reagents, in particular to a preparation method of high-purity low-nitrogen potassium persulfate. technical background [0002] Ammonium persulfate is a white, odorless crystal, often used as a strong oxidizing reagent, and is a key reagent for the determination of total nitrogen in "Alkaline Potassium Persulfate Digestion UV Spectrophotometry". Total nitrogen is the total nitrogen content of all nitrogen-containing compounds in the water body, and is an important indicator reflecting the degree of pollution and eutrophication of the water body. Domestic sewage, agricultural drainage, and industrial wastewater are directly discharged into the water body, which increases the content of organic nitrogen and inorganic nitrogen-containing compounds in the water body, causing a large number of plankton to multiply, consuming dissolved oxygen in the water body, and seriously deteriorating the water bod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B15/08
Inventor 张贵珠贾伟青
Owner TIANJIN GUANGFU TECH DEV
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