Method for preparing sodium persulfate through direct electrooxidation

A technology of sodium persulfate and electro-oxidation, applied in electrolysis process, non-precious metal oxide coating, electrode, etc., can solve the problems of low current efficiency, low current efficiency, large raw material consumption, etc., achieve long service life and simplify production Process, effect of reducing dosage

Active Publication Date: 2021-07-27
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional preparation of sodium persulfate generally uses electrolytic oxidation of ammonium sulfate aqueous solution to generate ammonium persulfate, and then undergoes metathesis reaction with sodium hydroxide to drive out the by-product ammonia, then concentrate under reduced pressure, crystallize, and dry to obtain sodium persulfate. The equation is: (NH4) 2 +2NaOH→Na 2 S 2 o 8 +2NH 3 +2H 2 O, or use electrolytic cold sulfuric acid to obtain peroxodisulfuric acid, and then react with alkali to obtain sodium persulfate. The reaction principle is 2HS0 4 - -2e - →H 2 S 2 o 8 , H 2 S 2 o 8 +2NaOH→Na 2 S 2 o 8 +2H 2 O, but the above methods all have disadvantages such as high power consumption, low current efficiency, low yield, high cost, and large consumption of raw materials
[0005] Japanese patent publication 31190 / 1980 (shown 55) discloses a kind of preparation method of sodium persulfate, is in the presence of ammonium ion, carries out electrolysis by using neutral raw material as anode, but this method is because of having lower electric current efficiency so considered uneconomical
Japanese patent application delay publication 56395 (shown 50) discloses a kind of preparation method of sodium persulfate, and the raw material of use is sodium bicarbonate, but although this method has used specific electrolytic cell and expensive titanium negative electrode, current in electrolysis extremely inefficient

Method used

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  • Method for preparing sodium persulfate through direct electrooxidation
  • Method for preparing sodium persulfate through direct electrooxidation

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Experimental program
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Effect test

Embodiment 1

[0026] The electrolytic cell adopts a structure such as figure 1 In the plate-and-frame electrolytic cell shown, the anode titanium-plated electrode is prepared as follows: metal titanium is selected as the substrate, and there is often a layer of dense oxide film on the surface of pure titanium, so it is firstly polished with 400-mesh metallographic sandpaper until Until the metal surface shows a uniform silver-white metallic luster, put the polished metal flakes into an ultrasonic cleaner for cleaning. After cleaning for 30 minutes, take them out and blow dry them. Alkali washing in NaOH lye, take it out after 2 hours, continue to put it in an ultrasonic cleaner for cleaning, take it out after 20 minutes and put it into an oxalic acid solution with a mass fraction of 25% for etching operation, so that the surface appears numb. After 2 hours, take it out and rinse it thoroughly with distilled water and place it in an alcohol solution with a mass fraction of 75% for later use....

Embodiment 2

[0034] Add an anolyte composed of sodium sulfate 280g / L and sulfuric acid 200g / L to the anode electrolyzer, add 25wt% dilute sulfuric acid solution to the cathode electrolyzer, the electrolysis temperature is 35°C, and the current density is 0.5A / m 2 , using a self-made titanium platinum-plated electrode as the anode, the cathode as a self-made alloy electrode, the anode inhibitor as 1g / L NaCl, electrolysis for 1.5h, the anolyte was exported, distilled and dried to obtain sodium persulfate crystals, the electrolytic cell pressure was 3.9v, The current efficiency was 78.23%, and the concentration of sodium persulfate was 150.49g / L.

Embodiment 3

[0036] Add an anolyte composed of sodium sulfate 290g / L and sulfuric acid 220g / L to the anode electrolyzer, add 25wt% dilute sulfuric acid solution to the cathode electrolyzer, the electrolysis temperature is 30°C, and the current density is 0.5A / m 2 , using a self-made titanium platinum-plated electrode as the anode, the cathode as a self-made alloy electrode, the anode inhibitor as 1g / L NaCl, electrolysis for 1.5h, the anolyte was exported, distilled and dried to obtain sodium persulfate crystals, the electrolytic cell pressure was 3.9v, The current efficiency was 78.23%, and the concentration of sodium persulfate was 150.49g / L.

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Abstract

The invention discloses a method for preparing sodium persulfate by direct electrooxidation. The method is characterized in that an anode is a titanium-plated platinum electrode prepared by a roasting method, a cathode is an alloy electrode prepared by a casting method, a bath pressure is greatly reduced, a two-electrode system is adopted, an anode electrolytic solution is a mixed solution of 220-300g/L of sodium sulfate and 200-400g/L of sulfuric acid, a cathode electrolytic solutionis a 20% wt dilute sulfuric acid solution, an anode additive is 0-2g/L sodium thiocyanate, the main product sodium persulfate is obtained after the electrolytic reaction is carried out in a plate frame type electrolytic cell under the constant current conditions that the temperature is 15-40 DEG C and the current density is 0.5-1.5 A/m<2>, the current efficiency can be up to 90.23%, and the concentration of the sodium persulfate can be up to 198.95 g/L. According to the method, by changing electrode materials and optimizing process conditions, the purposes of low energy consumption, low cost, low raw material consumption and relatively high current efficiency and yield are achieved.

Description

[0001] (1) Technical field [0002] The invention relates to a method for preparing sodium persulfate by direct electrooxidation. [0003] (2) Background technology [0004] Sodium persulfate is a strong oxidizing agent and can be used as an oxidizing agent to convert Cr 3+ , Mn 2+ and so on are oxidized to the corresponding high oxidation state compounds, when there is Ag + When it exists, it can promote the above oxidation reaction; it can be used as bleaching agent, metal surface treatment agent, chemical reagent, pharmaceutical raw material; battery, accelerator and initiator of emulsion polymerization. Activated sodium persulfate can be used in in-situ remediation of oil-contaminated soil. The traditional preparation of sodium persulfate generally uses electrolytic oxidation of ammonium sulfate aqueous solution to generate ammonium persulfate, and then undergoes metathesis reaction with sodium hydroxide to drive out the by-product ammonia, then concentrate under reduced...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/29C25B1/14C25B1/50C25D3/50C25B11/052C25B11/063C25B11/081C25B11/046C22C19/05C22C1/03
CPCC25D3/50C25B11/04C22C19/056C22C1/03C22C1/023
Inventor 毛信表赵瑞阳高龙强陈赵扬
Owner ZHEJIANG UNIV OF TECH
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