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Method for controlling crystallization growth of potassium peroxymonosulfate composite salt

A potassium hydrogen peroxymonosulfate complex salt, crystallization technology, used in chemical instruments and methods, peroxyhydrate/peroxyacid, peroxide/peroxyhydrate/peroxyacid/superoxide/ozone, etc. It can solve the problems of reducing product purity, product particle size description, increasing equipment requirements and production links, etc., to achieve the effect of good anti-caking performance, high product active oxygen stability and large particle size.

Pending Publication Date: 2021-02-12
ZHEJIANG JINKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Potassium monopersulfate compound salt products with active oxygen greater than or equal to 4.7% can be prepared by using this method, but there is no special description on the particle size of the prepared product
In addition, the patented method still needs to prepare KHSO with a K / S molar ratio of 0.8-1 4 Aqueous solution or KHSO 4 with H 2 SO 4 The mixed solution, the neutralization process is required to be carried out under vacuum conditions, which also increases the equipment requirements and production links
The prepared potassium peroxymonosulfate compound salt product needs to add stabilizers such as magnesium carbonate after drying, which also reduces the product purity.

Method used

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  • Method for controlling crystallization growth of potassium peroxymonosulfate composite salt
  • Method for controlling crystallization growth of potassium peroxymonosulfate composite salt
  • Method for controlling crystallization growth of potassium peroxymonosulfate composite salt

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A kind of potassium hydrogen persulfate compound salt crystallization growth control method, comprises the steps:

[0036] (1) 0.5kg stabilizer HEDP is added into 97kg, and mass fraction is 70% in the hydrogen peroxide solution and mixes evenly, then 213kg mass fraction is that 65% oleum is added dropwise in the hydrogen peroxide solution, control reaction system temperature At 5°C, an oxidizing solution was prepared.

[0037] (2) 600kg centrifuged mother liquor (containing KHSO obtained after centrifugation process) 5 、KHSO 4 , K 2 solution of SO4 and other substances) into the neutralization tank, slowly add the oxidizing solution prepared in step (1) and 170kg of potassium carbonate particles into the neutralization tank at the same time, control the reaction temperature at 5°C, and carry out the neutralization reaction under normal pressure .

[0038] (3) After the feeding is completed, the reaction solution after neutralization is transferred to the crystalliza...

Embodiment 2

[0040] Example 2 is basically the same as Example 1, except that 17.5 kg of the crystallization agent sodium tripolyphosphate and 24 kg of seed crystal slurry with a solid content of 40% are added in step (3). Stir, cool and crystallize, the crystallization temperature is -10°C, the cooling rate is 3.5°C / h, and the crystallization time is 5h, to obtain potassium monopersulfate compound salt crystals.

Embodiment 3

[0042] Example 3 is basically the same as Example 1, except that 15 kg of the crystallization agent sodium hexametaphosphate and 25 kg of seed crystal slurry with a solid content of 50% are added in step (3). Stir, cool and crystallize, the crystallization temperature is -15°C, the cooling rate is 5°C / h, and the crystallization time is 8h, to obtain potassium monopersulfate compound salt crystals. Carry out solid-liquid separation of the potassium monopersulfate compound salt crystal, dry the solid, and sieve the potassium monopersulfate compound salt with a particle size of 10 to 200 meshes. The obtained optical diagram of the potassium monopersulfate compound salt is as follows figure 1 As shown, the SEM image is shown in figure 2 shown.

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PUM

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Abstract

The invention discloses a method for controlling crystallization growth of potassium peroxymonosulfate composite salt. The method comprises the following steps: (1) adding 1-hydroxyethylidene-1,1-diphosphonic acid into a hydrogen peroxide solution, and adding fuming sulfuric acid into the hydrogen peroxide solution to obtain an oxidation solution of peroxymonosulfate; (2) adding the oxidation liquid prepared in the step (1) and potassium carbonate into a neutralization kettle of water or centrifugal mother liquor, and carrying out a neutralization reaction; (3) transferring the reaction solution neutralized in the step (2) into a crystallization kettle, adding a crystal modifier and seed crystal slurry containing potassium peroxymonosulfate composite salt, stirring, cooling and crystallizing; and (4) carrying out solid-liquid separation on the cooled and crystallized material in the step (3), and drying and screening the solid to obtain the potassium peroxymonosulfate composite salt with the particle size of more than 200 meshes. The potassium peroxymonosulfate composite salt prepared by the crystallization method disclosed by the invention is relatively large in particle size andhigh in yield, and has natural moisture absorption resistance and anti-caking property, so that the stability of active oxygen of the product is higher.

Description

technical field [0001] The invention relates to the technical field of peroxide preparation, more specifically, it relates to a method for controlling the growth of potassium monopersulfate compound salt crystals. Background technique [0002] The following background art is provided to help the reader understand the present invention and is not to be admitted as prior art. [0003] Potassium monopersulfate compound (Potassium monopersulfate compound, abbreviated as PMPS or PMS or KMPS) is a compound salt composed of three inorganic salts of potassium persulfate, potassium hydrogen sulfate and potassium sulfate, and its molecular formula is 2KHSO 5 ·KHSO 4 ·K 2 SO 4 . It is a free-flowing white granule with a solubility of about 256g / L at room temperature and is easily soluble in water with a bulk density of 1.1-1.2. The compound salt is stable at normal temperature, and easily decomposes to generate oxygen and sulfur-containing compounds when the temperature is high. ...

Claims

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Application Information

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IPC IPC(8): C01B15/08
CPCC01B15/085C01P2004/02C01P2004/03
Inventor 张晓栋魏一帆殷飞张敏敏杨栋栋
Owner ZHEJIANG JINKE CHEM
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