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Method for preparing potassium hydrogen peroxymonosulfate composite salt

The technology of a potassium hydrogen peroxymonosulfate composite salt and potassium hydrogen sulfate is applied in the preparation field of designing a potassium hydrogen peroxymonosulfate composite salt, which can solve the problems of adverse effects on the human body and the environment, low vacuum concentration efficiency, and high product impurity content. , to achieve the effect of not easy to agglomerate, improve product stability, and simple operation

Active Publication Date: 2012-01-11
宋海鹏
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  • Description
  • Claims
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Problems solved by technology

However, there are still high impurity content of the product due to the addition of stabilizers and crystal modifiers, low vacuum concentration efficiency, large water content after concentration, serious pollution in the open preparation process, adverse effects on human body and environment, large-scale industrial application There are still some problems in

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  • Method for preparing potassium hydrogen peroxymonosulfate composite salt
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preparation example Construction

[0036] figure 1 It is the flow chart of the preparation method of potassium peroxymonosulfate composite salt, as shown in the figure. The method for preparing potassium peroxymonosulfate composite salt of the present invention has simple equipment, low investment, low process condition requirements, easy operation, safety, no process waste water pollution, high yield, low impurities, high quality, and low cost, which mainly include The following steps:

[0037] (1) The hydrogen peroxide is oxidized with fuming sulfuric acid to obtain a strong acid, also known as Caro’s acid. The reaction formula is:

[0038] H 2 O 2 +H 2 SO 4 =H 2 SO 5 +H 2 O;

[0039] The reaction temperature is 0-20°C, the best is 10°C, and the reaction time is 1 to 3 hours;

[0040] The molar ratio of hydrogen peroxide to fuming sulfuric acid is:

[0041] Hydrogen peroxide: oleum = 1:0.90~1.05;

[0042] It is best to use hydrogen peroxide with a weight concentration of 50 to 70%;

[0043] The sulfuric acid can be ol...

Embodiment 1

[0068] (1) Oxidize 140 kg of hydrogen peroxide with a weight concentration of 70% and 250 kg of fuming sulfuric acid with a concentration of 65% at a reaction temperature of 10°C and a reaction time of 120 minutes; add 15% by weight potassium hydrogen sulfate solution 480KG

[0069] (2) React 405 kg of 48% potassium hydroxide solution with the product obtained in step (1) to obtain an aqueous solution of potassium monopersulfate. The reaction temperature is 23°C and the reaction time is 70 minutes; the reaction is in a vacuum The vacuum is 0.1 MPa;

[0070] (3) Add 30kg of potassium hydrogen sulfate to the concentration kettle, add the aqueous solution of potassium monopersulfate in a vacuum, and slowly (15 minutes) at a vacuum of 0.1 MPa to warm up to a temperature of 28 ℃ for 15 minutes. ;

[0071] (4) Cool to 5°C to crystallize. Repeat steps (1), (2), (3) (this time step (3) only raises the temperature without adding potassium hydrogen sulfate), and add the resulting mixed solu...

Embodiment 2

[0078] Using the same method as in Example 1, the difference is that the process water used in step (1) is the mother liquor produced in Example 1, and the additive in step (3) is the concentrated product of the mother liquor in Example 1, with a yield of 800 kg. The results are as follows:

[0079] The purity of the product is: active oxygen ≥4.75%.

[0080] The content of potassium persulfate is 0.

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Abstract

The invention relates to a method for preparing potassium hydrogen peroxymonosulfate composite salt. The method comprises the following steps: (1) firstly carrying out oxidation reaction on hydrogen peroxide and fuming sulfuric acid; (2) adding potassium hydrogen sulfate aqueous solution with the ratio of K to S being 0.8 to 1 or a mixed solution of potassium hydrogen sulfate and sulfuric acid or mother liquor after crystallization and centrifugation processes to the product obtained in the step (1), mixing and reacting to obtain the target product mixed solution of relatively stable H2SO5, KHSO5, KHSO4, H2SO4 and the like; (3) adding a 48wt% KOH solution produced by an ionic membrane process into the mixed solution produced in the step (2), and reacting under the vacuum condition; (4) adding potassium hydrogen sulfate solid or the mixture of KHSO5, KHSO4 and K2SO4 evaporated in the redundant mother liquor in the subsequent process into the mixed solution produced in the step (3), slowly heating for dissolving in vacuum, and concentrating; and (5) cooling and crystallizing, then collecting solid potassium hydrogen peroxymonosulfate by adopting a conventional method, and drying to obtain the product.

Description

Technical field [0001] The invention relates to a potassium peroxymonosulfate composite salt, in particular to a preparation method of potassium persulfate composite salt. Background technique [0002] Potassium persulfate composite salt, also known as potassium hydrogen persulfate composite salt, potassium monopersulfate composite salt, potassium monopersulfate composite salt or potassium monopersulfate composite salt, is a free-flowing white granular powder. Easily soluble in water, its molecular formula is KHSO 5 . [0003] Potassium peroxymonosulfate compound salt is a very effective oxidant and disinfectant. It is stable, convenient and has a wide range of uses. Its application fields involve oral cleaning, swimming pool and hot spring water disinfection, circuit board microetching agent, pulp bleaching, wool Fabric shrink-proof treatment, precious metal extraction, tap water pre-oxidation and subsequent disinfection, aquaculture and public environment disinfection, oil extra...

Claims

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Application Information

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IPC IPC(8): C01B15/08
Inventor 宋海鹏
Owner 宋海鹏
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