CN113174604A - Method for preparing sodium persulfate through direct electrooxidation - Google Patents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C25D3/00—Electroplating: Baths therefor
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Abstract
The invention discloses a direct power supplyThe method for preparing sodium persulfate through oxidation comprises the steps of preparing a titanium platinized electrode by adopting a roasting method as an anode, preparing an alloy electrode by adopting a fusion casting method as a cathode, greatly reducing the cell pressure, adopting a two-electrode system, wherein an anolyte is a mixed solution of 220-300 g/L sodium sulfate and 200-400 g/L sulfuric acid, a catholyte is a 20 wt% dilute sulfuric acid solution, an anode additive is 0-2 g/L sodium thiocyanate, and the current density is 0.5-1.5A/m at the temperature of 15-40 DEG C2After the electrolytic reaction in a plate-and-frame type electrolytic cell under the condition of constant current, the main product sodium persulfate is obtained, the current efficiency can reach 90.23 percent to the maximum, and the concentration of the sodium persulfate can reach 198.95g/L to the maximum. The method achieves low energy consumption, low cost, low raw material consumption, and higher current efficiency and yield by changing electrode materials and optimizing process conditions.
Description
(I) technical field
The invention relates to a method for preparing sodium persulfate by direct electrooxidation.
(II) background of the invention
Sodium persulfate is a strong oxidant, and can be used as oxidant for converting Cr3+，Mn2+Isoxidized to the corresponding high oxidation state compound when there is Ag+When present, the oxidation reaction can be promoted; the oxidability of the metal oxide can be used as a bleaching agent, a metal surface treating agent, a chemical agent and a medical raw material; a battery, an accelerator and an initiator for emulsion polymerization. The activated sodium persulfate can be used for the engineering of in-situ remediation of the petroleum-polluted soil. The traditional method for preparing sodium persulfate generally adopts an ammonium sulfate aqueous solution to carry out electrolytic oxidation to generate ammonium persulfate, then carries out double decomposition reaction with sodium hydroxide, drives out by-product ammonia, then carries out reduced pressure concentration, crystallization and drying to obtain sodium persulfate, and the reaction equation is as follows: (NH4)2+2NaOH→Na2S2O8+2NH3+2H2O or the cold sulfuric acid is electrolyzed to prepare the peroxodisulfuric acid which reacts with alkali to obtain the sodium persulfate, and the reaction principle is 2HS04 --2e-→H2S2O8，H2S2O8+2NaOH→Na2S2O8+2H2However, all the above methods have the disadvantages of high power consumption, low current efficiency, low yield, high cost, large raw material consumption, etc.
Japanese patent publication No. 31190/1980 (Sho 55) discloses a process for producing sodium persulfate by using a neutral raw material as an anode for electrolysis in the presence of ammonium ions, but this process is considered to be uneconomical because of its low current efficiency. Japanese patent application laid-open No. 56695 (Sho 50) discloses a method for producing sodium persulfate using sodium hydrogencarbonate as a raw material, but the current efficiency in electrolysis is extremely low although this method uses a specific electrolytic cell and an expensive titanium cathode.
Disclosure of the invention
Aiming at the defects of the prior art, the invention provides a method for preparing sodium persulfate by direct electrooxidation, which achieves the purposes of low energy consumption, low cost, low raw material consumption, higher current efficiency, higher yield and the like.
The technical scheme adopted by the invention is as follows:
a process for producing sodium persulfate by direct electrooxidation, the process comprising: the method comprises the steps of taking a titanium platinum-plated electrode manufactured by a roasting method as an anode, taking a Fe-C-Cr alloy electrode prepared by a smelting method as a cathode, adding 0-2 g/L of an anode additive into an anolyte which is a mixed solution of 220-300 g/L of sodium sulfate and 200-400 g/L of sulfuric acid, and adding 0.5-1.5A/m of a current density at a temperature of 15-40 ℃ when an anolyte is added with 10-20% of sulfuric acid solution2Carrying out electrolytic reaction for 1-6 h under the condition of constant current to prepare sodium persulfate; the anode additive is one of the following or a mixture of more than two of the following: sodium thiocyanate, sodium chloride, sodium fluoride, sodium polyphosphate and sodium persulfate.
After the electrolysis reaction is finished, the anolyte is cooled, crystallized, filtered and dried to obtain sodium persulfate crystals with the purity of about 90 percent.
The titanium platinized electrode is prepared by the following method:
(1) matrix treatment: selecting metal titanium as a matrix, wherein a layer of compact oxide film always exists on the surface of pure titanium, so that firstly, polishing is carried out by using metallographic abrasive paper until the surface presents uniform silvery white metal luster, then, the polished metal sheet is placed into an ultrasonic cleaner for cleaning for 20-30 min, then, taken out for drying, placed into NaOH alkaline liquor with the mass fraction of 20-30% and the temperature of 80-85 ℃ for alkaline cleaning, taken out after 1-2 h, placed into the ultrasonic cleaner for cleaning for 20-30 min, taken out, placed into oxalic acid solution with the mass fraction of 20-25% for etching operation for 1-2 h, taken out, fully washed by using distilled water, and placed into alcohol solution with the mass concentration of 75% for later use;
(2) preparing a titanium-plated platinum electrode by an electrodeposition method: the electroplating solution adopts a p salt-sulfamic acid system and comprises the following components: 10-20 g/L of p salt, 80-90 g/L of sulfamic acid, 1-2 of pH, 70-80 ℃ of temperature and 50-100A/m of current density2Under the condition, preparing a titanium platinum electrode by an electrodeposition method, fully drying the titanium platinum electrode in a nitrogen environment after electrolysis, and cutting the prepared titanium platinum electrode into sheets of 1cm by 1cm for later use.
The Fe-C-Cr alloy electrode is prepared by the following method:
(1) weighing nickel blocks, Ni-Si, Ni-Mn, Ni-Cr, Ni-Cu, Ni-Mo, Ni-Fe, Ni-C intermediate alloy and WO according to the mass percentage of 5.5-7% of Mn, 2-6% of Fe, 14-18% of Cr, 12-17% of Mo, 2-5% of W, 0.5-1% of Cu, 0.15-0.2% of C, 1-2% of Si and the balance of Ni2；
(2) Putting a nickel block into a melting furnace, heating for melting, continuously heating to 1200-1500 ℃, sequentially adding Ni-Si, Ni-Mn, Ni-Cr, Ni-Cu, Ni-Mo, Ni-Fe and Ni-C intermediate alloys, melting for 10-40 min under stirring after materials in the melting furnace are completely melted to obtain alloy melt, blowing a refining agent into the 2/3-5/6 area below the surface of the alloy melt by using argon, and adding WO2Refining for 10-30 min to obtain an alloy melt, adding an alloy refiner into the alloy melt after slagging off for grain refinement, uniformly covering a covering agent on the surface of the melt, standing for 10-30 min, introducing argon for degassing and refining for 20-40 min, slagging off, performing double filtration by an alumina ceramic filter, and then performing ingot casting at 675-740 ℃ to obtain an alloy ingot;
(3) and (3) milling the alloy ingot in the step (2), removing oil, performing homogenization annealing heat treatment for 1-8 hours at the temperature of 540-600 ℃, then sequentially performing hot rolling and medium-temperature rolling, then performing cold rolling, and performing finishing and fixed-length cutting to obtain the Fe-C-Cr alloy electrode material.
Specifically, the electrolytic reaction is carried out in a plate-and-frame type electrolytic cell, and the length-width ratio of a cathode to an anode is 6: 2: 9 respectively correspond to the length, the width and the height of the electrolytic cell, and the used membrane is a Nafion427 cation exchange membrane.
Preferably, the anode additive is sodium thiocyanate. Sodium thiocyanate is used as an additive, so that the occurrence of side reaction oxygen evolution reaction can be inhibited, and the yield and the current efficiency are improved.
The invention has the following beneficial effects: the method adopts the novel material electrode, can reduce the consumption of anode material platinum, has long service life, thereby reducing the production and maintenance cost, has higher current efficiency, simultaneously uses the alloy electrode to replace the traditional lead electrode, can reduce the original tank voltage from 5.2V to 4.7V or below under the actual condition, simultaneously solves the environmental protection problem of lead pollution discharge, simplifies the production flow and reduces the cost compared with the traditional sodium persulfate production enterprises.
(IV) description of the drawings
FIG. 1 is a schematic view of the structure of a plate and frame type electrolytic cell of the present invention; the novel titanium platinized anode is manufactured by a novel titanium platinized anode, a polytetrafluoroethylene membrane, a novel titanium platinized anode, a titanium exchange membrane, a novel titanium platinized anode, a polytetrafluoroethylene membrane, a silicone gasket, a novel titanium platinized anode, a titanium exchange membrane, a novel alloy electrode, and a self-made alloy electrode.
(V) detailed description of the preferred embodiments
For the purpose of enhancing understanding of the present invention, the present invention will be described in further detail with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1:
the electrolytic cell adopts a plate-and-frame electrolytic cell with the structure shown in figure 1, and an anode titanium platinized electrode is prepared according to the following method: selecting metal titanium as a matrix, wherein a layer of compact oxide film often exists on the surface of pure titanium, polishing the pure titanium by using 400-mesh metallographic abrasive paper until the surface of the pure titanium presents uniform silvery white metal luster, then putting the polished metal sheet into an ultrasonic cleaner for cleaning, taking out the metal sheet for blow-drying after thirty minutes, putting the metal sheet into NaOH alkaline liquor with the mass fraction of 30% and the temperature of 85 ℃ for alkali cleaning, and taking the metal sheet after 2 hours for alkali cleaningAnd (3) continuously putting the glass into an ultrasonic cleaner for cleaning, taking out the glass after 20min, putting the glass into an oxalic acid solution with the mass fraction of 25% for etching operation to enable the surface of the glass to be in a pitted state, taking out the glass after 2h, fully washing the glass with distilled water, and putting the glass in an alcohol solution with the mass fraction of 75% for later use. The plating solution adopts a p salt-sulfamic acid system, and comprises the following components: p salt (10g/L), sulfamic acid (90g/L), pH 1, temperature 70 deg.C, current density 100A/m2Under the condition, preparing a titanium platinum electrode by an electrodeposition method, fully drying the titanium platinum electrode in a nitrogen environment after electrolysis, and cutting a 1 cm-1 cm slice for later use.
The cathode self-made alloy electrode is prepared by the following method:
(1) weighing nickel blocks, Ni-Si, Ni-Mn, Ni-Cr, Ni-Cu, Ni-Mo, Ni-Fe, Ni-C intermediate alloy and WO according to the mass percentage composition of Mn 6%, Fe 4.5%, Cr 16%, Mo 14%, W4%, Cu 0.5%, C0.15%, Si 1.5% and the balance of Ni2；
(2) Putting a nickel block into a melting furnace, heating for melting, continuously heating to 1200-1500 ℃, sequentially adding Ni-Si, Ni-Mn, Ni-Cr, Ni-Cu, Ni-Mo, Ni-Fe and Ni-C intermediate alloys, melting for 30min under stirring after materials in the melting furnace are completely melted to obtain an alloy melt, blowing a refining agent (hexachloroethane) into an 2/3-5/6 area below the alloy melt surface by using argon, and adding WO2Refining for 20min to obtain an alloy melt, adding an alloy refiner Ni-5% Ti-1% B into the alloy melt after slagging off for grain refinement, uniformly covering the surface of the melt with a covering agent Ni-5% Ti-1% B, standing for 20min, introducing argon for degassing and refining for 30min, slagging off, performing double filtration by an alumina ceramic filter, and performing ingot casting at 675-740 ℃ to obtain an alloy ingot;
(3) milling the alloy ingot obtained in the step (2), removing oil, placing the alloy ingot at 540-600 ℃ for carrying out homogenization annealing heat treatment for 6 hours, then sequentially carrying out hot rolling and medium-temperature rolling, then carrying out cold rolling, and carrying out finishing and fixed-length cutting to obtain the nickel alloy cathode material; wherein the hot rolling temperature is 750 ℃, and the rolling thickness is 6 cm; the rolling temperature at the middle temperature is 500 ℃, and the rolling thickness is 2 cm; cold rolling is room temperature rolling, and the rolling thickness is 5 mm; the surface roughness Ra of the alloy plate after finishing is not more than 0.5um, so that the surface has no phenomena of spots, oxidation, oil stain and the like.
The length-width-height ratio of the cathode and the anode is 6: 2: 9.
adding an anolyte with the composition of 300g/L of sodium sulfate and 250g/L of sulfuric acid into an anodic electrolytic cell, adding a dilute sulfuric acid solution with the concentration of 25 wt% into a cathodic electrolytic cell, wherein the electrolysis temperature is 25 ℃, and the current density is 1A/m2The method comprises the steps of taking a self-made titanium platinum-plated electrode as an anode, taking a cathode as a self-made alloy electrode, taking sodium thiocyanate as an anode inhibitor, controlling the concentration to be 0.5g/L, electrolyzing for 1h, leading out anolyte, distilling and drying to obtain sodium persulfate crystals, controlling the tank pressure to be 4.3v, controlling the current efficiency to be 80.45% and controlling the concentration of sodium persulfate to be 167.23 g/L.
Example 2:
adding an anolyte with the composition of 280g/L of sodium sulfate and 200g/L of sulfuric acid into an anodic electrolytic cell, adding a dilute sulfuric acid solution with the concentration of 25 wt% into a cathodic electrolytic cell, wherein the electrolysis temperature is 35 ℃, and the current density is 0.5A/m2Taking a self-made titanium platinum-plated electrode as an anode, a cathode as a self-made alloy electrode, an anode inhibitor of 1g/L NaCl, electrolyzing for 1.5h, leading out anolyte, distilling and drying to obtain sodium persulfate crystals, wherein the pressure of an electrolytic bath is 3.9v, the current efficiency is 78.23%, and the concentration of sodium persulfate is 150.49 g/L.
Example 3:
adding an anolyte with the composition of 290g/L of sodium sulfate and 220g/L of sulfuric acid into an anodic electrolytic cell, adding a dilute sulfuric acid solution with the concentration of 25 wt% into a cathodic electrolytic cell, wherein the electrolysis temperature is 30 ℃, and the current density is 0.5A/m2Taking a self-made titanium platinum-plated electrode as an anode, a cathode as a self-made alloy electrode, an anode inhibitor of 1g/L NaCl, electrolyzing for 1.5h, leading out anolyte, distilling and drying to obtain sodium persulfate crystals, wherein the pressure of an electrolytic bath is 3.9v, the current efficiency is 78.23%, and the concentration of sodium persulfate is 150.49 g/L.
Example 4:
adding an anolyte with the composition of 350g/L of sodium sulfate and 200g/L of sulfuric acid into an anodic electrolytic cell, adding a dilute sulfuric acid solution with the concentration of 25 wt% into a cathodic electrolytic cell, and electrolyzing at the temperatureAt 20 ℃ and a current density of 0.5A/m2Taking a self-made titanium platinum-plated electrode as an anode, a cathode as a self-made alloy electrode, an anode inhibitor of 1g/L sodium fluoride, electrolyzing for 1.5h, leading out anolyte, distilling and drying to obtain sodium persulfate crystals, wherein the pressure of an electrolytic cell is 3.9v, the current efficiency is 88.23%, and the concentration of sodium persulfate is 190.64 g/L.
Example 4:
adding an anolyte with the composition of 350g/L of sodium sulfate and 300g/L of sulfuric acid into an anodic electrolytic cell, adding a dilute sulfuric acid solution with the concentration of 25 wt% into a cathodic electrolytic cell, wherein the electrolysis temperature is 15 ℃, and the current density is 2A/m2The method comprises the steps of taking a self-made titanium platinum-plated electrode as an anode, taking a cathode as a self-made alloy electrode, taking 1g/L sodium polyphosphate as an anode inhibitor, electrolyzing for 2 hours, leading out anolyte, distilling and drying to obtain sodium persulfate crystals, and controlling the pressure of an electrolytic cell to be 3.8v, the current efficiency to be 90.23% and the concentration of sodium persulfate to be 198.95 g/L.
Test example:
adding an anolyte with the composition of 350g/L of sodium sulfate and 300g/L of sulfuric acid into an anodic electrolytic tank, adding a dilute sulfuric acid solution with the concentration of 25 wt% into a cathodic electrolytic tank, wherein the electrolysis temperature is 15 ℃, the current density is 2A/m2, a self-made titanium platinum-plated electrode, a platinum sheet, a platinum net, an iridium-tin electrode, an iridium-tantalum electrode and ruthenium-iridium-tin are used as anodes, a cathode is a self-made alloy electrode, an anode inhibitor is 1g/L of sodium polyphosphate, electrolyzing for 2 hours, and the current efficiency is shown in Table 1:
TABLE 1
Claims (5)
1. A process for producing sodium persulfate by direct electrooxidation, the process comprising: the method comprises the steps of taking a titanium platinum-plated electrode manufactured by a roasting method as an anode, taking a Fe-C-Cr alloy electrode manufactured by a smelting method as a cathode, adding 0-2 g/L of an anode additive into an anolyte which is a mixed solution of 220-300 g/L of sodium sulfate and 200-400 g/L of sulfuric acid, and adding the anolyte into a sulfuric acid solution with the mass concentration of 10-20%, wherein the anolyte is a solution of the sulfuric acid, and the current density is controlled at the temperature of 15-40 DEG CThe degree of the reaction is 0.5 to 1.5A/m2Carrying out electrolytic reaction for 1-6 h under the condition of constant current to prepare sodium persulfate; the anode additive is one of the following or a mixture of more than two of the following: sodium thiocyanate, sodium chloride, sodium fluoride, sodium polyphosphate and sodium persulfate.
2. The method of claim 1, wherein the titanium platinized electrode is prepared by:
(1) matrix treatment: selecting metal titanium as a substrate, firstly polishing by using metallographic abrasive paper until the surface of the metal titanium presents uniform silvery white metal luster, then putting the metal titanium into an ultrasonic cleaner for cleaning for 20-30 min, taking out the metal titanium for drying, putting the metal titanium into NaOH alkali liquor with the mass fraction of 20-30% and the temperature of 80-85 ℃ for alkali cleaning, taking out the metal titanium after 1-2 h, putting the metal titanium into the ultrasonic cleaner for cleaning for 20-30 min, taking out the metal titanium, putting oxalic acid solution with the mass fraction of 20-25% for etching operation for 1-2 h, taking out the metal titanium, fully washing the metal titanium with distilled water, and putting the metal titanium into alcohol solution with the mass concentration of 75% for later use;
(2) preparing a titanium-plated platinum electrode by an electrodeposition method: the electroplating solution adopts a p salt-sulfamic acid system and comprises the following components: 10-20 g/L of p salt, 80-90 g/L of sulfamic acid, 1-2 of pH, 70-80 ℃ of temperature and 50-100A/m of current density2Under the condition, preparing the titanium platinum electrode by an electrodeposition method, fully drying the titanium platinum electrode in a nitrogen environment after electrolysis, and cutting the prepared titanium platinum electrode into thin sheets for later use.
3. The method of claim 1, wherein the Fe-C-Cr alloy electrode is prepared by:
(1) weighing nickel blocks, Ni-Si, Ni-Mn, Ni-Cr, Ni-Cu, Ni-Mo, Ni-Fe, Ni-C intermediate alloy and WO according to the mass percentage of 5.5-7% of Mn, 2-6% of Fe, 14-18% of Cr, 12-17% of Mo, 2-5% of W, 0.5-1% of Cu, 0.15-0.2% of C, 1-2% of Si and the balance of Ni2；
(2) Putting a nickel block into a melting furnace, heating for melting, continuously heating to 1200-1500 ℃, sequentially adding Ni-Si, Ni-Mn, Ni-Cr, Ni-Cu,Ni-Mo, Ni-Fe and Ni-C intermediate alloy, smelting for 10-40 min under stirring after materials in a melting furnace are completely melted to obtain alloy melt, blowing a refining agent into 2/3-5/6 area below the surface of the alloy melt by utilizing argon, and adding WO2Refining for 10-30 min to obtain an alloy melt, adding an alloy refiner into the alloy melt after slagging off for grain refinement, uniformly covering a covering agent on the surface of the melt, standing for 10-30 min, introducing argon for degassing and refining for 20-40 min, slagging off, performing double filtration by an alumina ceramic filter, and then performing ingot casting at 675-740 ℃ to obtain an alloy ingot;
(3) and (3) milling the alloy ingot in the step (2), removing oil, performing homogenization annealing heat treatment for 1-8 hours at the temperature of 540-600 ℃, then sequentially performing hot rolling and medium-temperature rolling, then performing cold rolling, and performing finishing and fixed-length cutting to obtain the Fe-C-Cr alloy electrode material.
4. The process of claim 1, wherein the electrolysis reaction is carried out in a plate and frame cell with a cathode to anode aspect ratio of 6: 2: 9, the membrane used is a Nafion427 cation exchange membrane.
5. The method of claim 1, wherein the anode additive is sodium thiocyanate.
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| CN113881952A (en) * | 2021-10-28 | 2022-01-04 | 浙江工业大学 | Electrolytic synthesis method of high sodium sulfate |
| CN116657162A (en) * | 2023-05-16 | 2023-08-29 | 亚泰电化有限公司 | Preparation method of high-purity ammonium persulfate |
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| CN116657162B (en) * | 2023-05-16 | 2024-02-02 | 亚泰电化有限公司 | Preparation method of high-purity ammonium persulfate |
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