CN101392386A - Electrochemistry method for simultaneously producing sodium chlorate and alkaline peroxide - Google Patents
Electrochemistry method for simultaneously producing sodium chlorate and alkaline peroxide Download PDFInfo
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- CN101392386A CN101392386A CNA2008102016297A CN200810201629A CN101392386A CN 101392386 A CN101392386 A CN 101392386A CN A2008102016297 A CNA2008102016297 A CN A2008102016297A CN 200810201629 A CN200810201629 A CN 200810201629A CN 101392386 A CN101392386 A CN 101392386A
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Abstract
The invention relates to an electrochemical method which produces sodium chloride and alkaline hydrogen peroxide simultaneously. The method can improve the use efficiency of the two poles of the electricity, and lower the production cost. The method adopts an electrolytic tank consisting of an anode, a cation exchange membrane, an anion exchange membrane and a cathode, wherein, the electrodes combine with the membranes in sequence to form an anode chamber, an intermediate chamber and a cathode chamber; sodium chloride solution and sodium chlorate solution are circulated to the anode chamber, sodium hydroxide solution and air is circulated to the cathode chamber and sodium hydroxide solution is circulated to the intermediate chamber; after direct current circulating among the electrodes, chlorine is produced in the anode while the oxygen in the cathode deoxidizes and produces hydrogen peroxide and the concentration of the sodium hydroxide solution in the intermediate chamber is increased; the anolyte flowing out of the anode chamber flows into an external heated reaction tank, and chlorine is transferred into sodium chlorate; the anolyte is circulated back to the anode chamber of the electrolytic tank; a part of the concentrated sodium hydroxide solution which flows out of the intermediate chamber can be used for adjusting the pH value of the anolyte without using extra sodium hydroxide, thereby lowering the running cost.
Description
Technical field
The present invention relates to the electrochemical method of a kind of production sodium chlorate simultaneously and alkaline hydrogen peroxide, belong to chemical production field.
Background technology
The technology for preparing sodium chlorate or alkaline hydrogen peroxide with electrochemical method separately is comparatively ripe.For example, J.Coleman is in the traditional oxymuriate preparation method described in " Electrolytic production of sodium chlorate " (A.I.Ch.E.Symposium 204 vol 77 1981.pp244-263).The electrolytic chlorination sodium solution prepares sodium chlorate in a single-cell, and anode produces chlorine, and negative electrode produces hydrogen and hydroxide ion.The chlorine hydrolysis generates hypochlorous acid, further independently in the reacting by heating groove homogeneous chemical reaction generation oxymuriate takes place at one.Electrochemical method production sodium chlorate is generally used 60-80 ℃ saturated nacl aqueous solution, and current density is 1-3kA/m
2
United States Patent (USP) 3,969,201,4,118,305 and 4,406,758 have illustrated the electrochemical method for preparing alkaline hydrogen peroxide solution by cathodic reduction oxygen in basic solution.The employed negative electrode of these patents is three-dimensional graphite cathode, and electrolytic solution is the NaOH aqueous solution.The concentration of NaOH solution is 1-3mol/L, and temperature is 20-30 ℃, and apparent cathode current density is 0.1-1kA/m
2, oxygen pressure can be greater than a normal atmosphere, to improve the space-time yield of hydrogen peroxide.
Anode and negative electrode electrolysis simultaneously at same electrolyzer produce useful product.Separate with porous diaphragm when anolyte compartment and cathode compartment, brine electrolysis can obtain hydrogen and oxygen simultaneously.When using cationic exchange to touch or porous diaphragm separation anolyte compartment and cathode compartment, electrolytic sodium chloride can obtain chlorine and sodium hydroxide.United States Patent (USP) 3,884,777 have described by the invention of electrolytic preparation dioxide peroxide, hydrogen peroxide, sodium hydroxide and chlorine simultaneously of one three Room electrolyzer, and wherein, hydrogen peroxide produces by anodic oxidation sulfuric acid.
Japanese Patent 61-284591 relates to a kind of electrochemical method for preparing alkaline hydrogen peroxide and chlorine or sodium chlorate simultaneously.Used electrolyzer is the locellus electrolyzer, and electrode is respectively graphite cathode and precious metal anode, and anode and negative electrode are separated by porous diaphragm.The example of this invention has only adopted cationic exchange membrane, as the Nafion 315 of Du Pont.Owing to adopt cationic exchange membrane, the pH to 6-7 that stoichiometric sodium hydroxide is regulated anolyte such as need in anolyte, to add in the electrolytic process, make the running cost increase.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the electrochemical method of a kind of production sodium chlorate simultaneously and alkaline hydrogen peroxide is provided, can improve the two poles of the earth utilising efficiency of electric current, reduce production costs.
For realizing such purpose, technical scheme of the present invention is:
(1) uses a kind of electrolyzer of forming by anode, cationic exchange membrane, anion-exchange membrane and negative electrode, wherein anode and cationic exchange membrane form the anolyte compartment, cationic exchange membrane and anion-exchange membrane form intermediate chamber, and anion-exchange membrane and negative electrode form cathode compartment; (2) logical sodium-chlor in anolyte compartment and sodium chlorate solution, logical sodium hydroxide solution of cathode compartment and air, intermediate chamber leads to sodium hydroxide solution, after leading to direct current between electrode, anode produces chlorine, and the negative electrode oxygen reduction generates hydrogen peroxide, and the concentration of sodium hydroxide solution of intermediate chamber increases; (3) the effusive anolyte in the anolyte compartment external heated reactive tank of flowing through, the chlorine hydrolysis generates hypochlorous acid, homogeneous chemical reaction takes place generate sodium chlorate, and anolyte is recycled electrolyzer anode chamber.The effusive part of intermediate chamber can be used for regulating the pH of anolyte through spissated sodium hydroxide solution.
Method of the present invention is specially:
(1) adopts a kind of electrolyzer, this electrolyzer comprises anode, cationic exchange membrane, anion-exchange membrane and negative electrode, wherein anode and cationic exchange membrane form the anolyte compartment, and cationic exchange membrane and anion-exchange membrane form intermediate chamber, and anion-exchange membrane and negative electrode form cathode compartment.
(2) anode chamber, cathode compartment and intermediate chamber feed electrolytic solution respectively, and wherein, sodium chloride concentration is 0.1-5M in the anolyte, and density of sodium chlorate is 0-5M, and the residence time of anolyte in the anolyte compartment is 10-100s; Cathode compartment feeds sodium hydroxide solution and air, and concentration of sodium hydroxide solution is 0.1-5M, and the residence time is 0.5-10min, and the residence time of air is 0.2-2s; Intermediate chamber feeds the sodium hydroxide solution of 0.1-5M, and the residence time is 0.5-7min.The operating temperature of electrolyzer is 0-100 ℃, and galvanization density is 0.1-6kA/m
2Direct current, anode produces chlorine, the negative electrode oxygen reduction generates hydrogen peroxide, the concentration of sodium hydroxide solution of intermediate chamber increases.
(3) the anolyte external heated reactive tank of flowing through, the chlorine hydrolysis generates hypochlorous acid, homogeneous chemical reaction takes place subsequently generate sodium chlorate, and afterwards, anolyte is recycled electrolyzer anode chamber.By dripping acid, as hypochlorous acid, or suitable alkali, as sodium hydroxide, the pH that comes the Control Circulation anolyte is between 6-7.Regulate sodium hydroxide that pH adopted and can adopt that to come from the electrolyzer intermediate chamber effusive through spissated sodium hydroxide solution.
Anode material among the present invention is the steady electrode of shape (DSA), comprises that titanium is coated with plumbic oxide PbO
2/ Ti, titanium are coated with ruthenium Ru/Ti electrode etc.
Cathode material among the present invention can be selected metals such as stainless steel plate, nickel plate, also can select carbon felt, graphite particle and graphite fibre etc., and negative electrode is preferably the composite graphite particle through carbon black/polytetrafluorethylecoatings coatings among the present invention.
Cationic exchange membrane of the present invention can be selected polyethylene cationic exchange membrane, polyvinyl chloride-type cationic exchange membrane, tetrafluoroethylene conduction cationic exchange membrane or polysulfones sulfonic acid cationic exchange membrane etc. for use.
Anion-exchange membrane of the present invention can be selected polyethylene anion-exchange membrane, butylbenzene quaternary ammonium anion exchange membrane, polysulfones anion-exchange membrane or pyridine quaternary ammonium anion exchange membrane etc. for use.
Electrochemical method of the present invention is two kinds of useful chemical of electrolysis production simultaneously---sodium chlorate and hydrogen peroxide, thus the whole utilising efficiency of raising electric current reduces production costs.In addition, the present invention adopts anode, cationic exchange membrane, anion-exchange membrane and negative electrode putting in order successively, therefore can adopt intermediate chamber effusive, need not use extra sodium hydroxide, thereby can further reduce running cost through spissated sodium hydroxide solution adjusting anolyte pH.
Description of drawings
Fig. 1 is the electrochemical method synoptic diagram of the present invention's while electrolysis production sodium chlorate and alkaline hydrogen peroxide.
Embodiment
Below in conjunction with specific embodiment electrochemical method of the present invention is further described.
Fig. 1 has provided electrochemical method testing apparatus of the present invention and technical process.As shown in Figure 1, a kind of electrolyzer that the present invention adopts comprises anode, cationic exchange membrane, anion-exchange membrane and negative electrode, wherein anode and cationic exchange membrane form the anolyte compartment, and cationic exchange membrane and anion-exchange membrane form intermediate chamber, and anion-exchange membrane and negative electrode form cathode compartment.Logical sodium-chlor in anolyte compartment and sodium chlorate solution, cathode compartment feeds sodium hydroxide solution and air, and intermediate chamber leads to sodium hydroxide solution.
When electric tank working, the hydroxide ion that electrolysis produces in the cathode compartment enters intermediate chamber by anion-exchange membrane, with the sodium ion formation sodium hydroxide from anolyte.Adopt intermediate chamber effusive, need not use extra sodium hydroxide, thereby can reduce running cost through spissated sodium hydroxide solution adjusting anolyte pH.Intermediate chamber flows out sodium hydroxide solution, and a part is used to regulate anolyte pH, and a part is back to former sodium hydroxide solution storage tank.
When the logical direct current in electrode two ends, negative electrode produces hydrogen peroxide, and anode produces chlorine, and the chlorine hydrolysis generates hypochlorous acid, homogeneous chemical reaction takes place in the reacting by heating groove externally generate sodium chlorate.When the sodium chlorate in the anolyte reaches finite concentration, segment anode liquid can be discharged, and additional sodium chloride solution.Also can in circulating anode liquid, add or drainage water, to keep water balance.In the present invention, porous cathode can adopt the trickle bed mode to carry out electrolysis, and sodium hydroxide solution and air pass through cathode compartment from top to bottom in the same way.The electrolytic solution of anolyte compartment and intermediate chamber flows into from bottom to top.The effusive sodium hydroxide solution of intermediate chamber, part is used to regulate anolyte pH, is partly refluxed to the reservoir of former NaOH solution.
The feasibility of electrochemical method of the present invention tested verify.Continous way electrochemical reaction process as shown in Figure 1, sodium hydroxide solution and air (catholyte) and sodium chloride solution (anolyte) are pumped into respectively in the electrolyzer of the present invention.The catholyte one way is passed through electrolyzer.And anolyte loops back electrolyzer behind the external heated reactive tank, and reacting by heating groove having heaters is used for controlling the temperature of anolyte.The pH of circulating anode liquid is controlled between 6-7 automatically by dripping hypochlorous acid or sodium hydroxide, and it is effusive through spissated sodium hydroxide solution that the adjusting sodium hydroxide that pH adopted comes from the electrolyzer intermediate chamber.
Embodiment 1
Adopt electrochemical process testing apparatus as shown in Figure 1, with preparation alkaline hydrogen peroxide and sodium chlorate.Concrete test conditions is as follows: cathode material is carbon black/polytetrafluorethylecoatings coatings composite graphite particle, and nickel cathode plate (80*70mm), anode are that titanium is coated with plumbic oxide DSA electrode (80*70mm), and the electrode apparent area is 30cm
2, anion-exchange membrane is the polyethylene heterogeneous membrane, cationic exchange membrane is the polyethylene heterogeneous membrane.Anolyte is 3.8MNaCl, and a residence time in the anolyte compartment is 21s; Catholyte is 2M NaOH, and the residence time is 7min, and air feeds cathode compartment behind alkali cleaning bottle and washing bottle, and the residence time is 1s; Intermediate chamber NaOH strength of solution is 1M, and the residence time is 100s.Anode temperature is 30 ℃ in the electrolyzer, and catholyte is 35 ℃.Current density is 1.2kA/m
2The time, average terminal voltage is 4.3V.The temperature of reacting by heating groove is 70 ℃, and the pH of anolyte is controlled at 6.5 in the reacting by heating groove, and the volume of anolyte is 1L in the reacting by heating groove.After the electrolysis 3 hours, H
2O
2Concentration is 0.161M, NaClO
3Be 0.04M, current efficiency is respectively 86.3% and 59.6%.
Embodiment 2
Adopt electrochemical process testing apparatus as shown in Figure 1, with preparation alkaline hydrogen peroxide and sodium chlorate.Concrete test conditions is as follows: cathode material is carbon black/polytetrafluorethylecoatings coatings composite graphite particle, and stainless steel cathode plate (80*70mm), anode are that titanium is coated with plumbic oxide DSA electrode (80*70mm), and the electrode apparent area is 30cm
2, anion-exchange membrane is the polysulfones heterogeneous membrane, cationic exchange membrane is a perfluoro sulfonic acid membrane.Anolyte is 2.8MNaCl and 2.42M NaClO
3, be 8s in a residence time of anolyte compartment; Catholyte is 2M NaOH, and the residence time is 84s, and air feeds cathode compartment behind alkali cleaning bottle and washing bottle, and the residence time is 1s; Intermediate chamber NaOH strength of solution is 2M, and the residence time is 10s.Anode temperature is 30 ℃ in the electrolyzer, and catholyte is 35 ℃.Current density is 1.2kA/m
2The time, average terminal voltage is 4.1V.The temperature of reacting by heating groove is 70 ℃, and the pH of anolyte is controlled at 6.5 in the reacting by heating groove, and the volume of anolyte is 1L in the reacting by heating groove.After the electrolysis 3 hours, H
2O
2Concentration is 0.036M, NaClO
3Increase to 2.47M, current efficiency is respectively 96.5% and 74.4%.
Embodiment 3
Adopt electrochemical process testing apparatus as shown in Figure 1, with preparation alkaline hydrogen peroxide and sodium chlorate.Concrete test conditions is as follows: cathode material is the carbon felt, and stainless steel cathode plate (80*70mm), anode are that titanium is coated with ruthenium Ru/Ti electrode (80*70mm), and the electrode apparent area is 30cm
2, anion-exchange membrane is the polysulfones heterogeneous membrane, cationic exchange membrane is a perfluoro sulfonic acid membrane.Anolyte is 3.8M NaCl and 0.25M NaClO
3, be 42s in a residence time of anolyte compartment; Catholyte is 4M NaOH, and the residence time is 42s, and air feeds cathode compartment behind alkali cleaning bottle and washing bottle, and the residence time is 0.2s; Intermediate chamber NaOH strength of solution is 2M, and the residence time is 5s.Anode temperature is 50 ℃ in the electrolyzer, and catholyte is 50 ℃.Current density is 3kA/m
2The time, average terminal voltage is 6V.The temperature of reacting by heating groove is 70 ℃, and the pH of anolyte is controlled at 6.5 in the reacting by heating groove, and the volume of anolyte is 2L in the reacting by heating groove.After the electrolysis 6 hours, H
2O
2Concentration is 0.037M, NaClO
3Increase to 0.37M, current efficiency is respectively 79.3% and 71.5%.
Embodiment 4
Adopt electrochemical process as shown in Figure 1 to test, with preparation alkaline hydrogen peroxide and sodium chlorate.Concrete test conditions is as follows: cathode material is the carbon felt, and stainless steel cathode plate (80*70mm), anode are that titanium is coated with ruthenium Ru/Ti electrode (80*70mm), and the electrode apparent area is 30cm
2, anion-exchange membrane is a butylbenzene quaternary ammonium film, cationic exchange membrane is the polysulfones sulfonate film.Anolyte is 2.8M NaCl and 2.89M NaClO
3Mixing solutions, a residence time in the anolyte compartment is 14s; Catholyte is 1M NaOH, and the residence time is 42s, and air feeds cathode compartment behind alkali cleaning bottle and washing bottle, and the residence time is 0.4s; Intermediate chamber NaOH strength of solution is 2M, and the residence time is 5s.Anode temperature is 30 ℃ in the electrolyzer, and catholyte is 35 ℃.Current density is 2.4kA/m
2The time, average terminal voltage is 5.7V.The temperature of reacting by heating groove is 70 ℃, and the pH of anolyte is controlled at 6.5 in the reacting by heating groove, and the volume of anolyte is 1L in the reacting by heating groove.After the electrolysis 3 hours, H
2O
2Concentration is 0.295M, NaClO
3Increase to 3.00M, current efficiency is respectively 79.1% and 81.9%.
Claims (5)
1, the electrochemical method of a kind of production sodium chlorate simultaneously and alkaline hydrogen peroxide is characterized in that comprising the steps:
(1) adopts a kind of electrolyzer of forming by anode, cationic exchange membrane, anion-exchange membrane and negative electrode, wherein anode and cationic exchange membrane form the anolyte compartment, cationic exchange membrane and anion-exchange membrane form intermediate chamber, and anion-exchange membrane and negative electrode form cathode compartment;
(2) anode chamber, cathode compartment and intermediate chamber feed electrolytic solution respectively; Wherein, sodium chloride concentration is 0.1-5M in the anolyte, and density of sodium chlorate is 0-5M, and the residence time of anolyte in the anolyte compartment is 10-100s; Cathode compartment feeds sodium hydroxide solution and air, and concentration of sodium hydroxide solution is 0.1-5M, and the residence time is 0.5-10min, and the residence time of air is 0.2-2s; Intermediate chamber feeds the sodium hydroxide solution of 0.1-5M, and the residence time is 0.5-7min; The operating temperature of electrolyzer is 0-100 ℃, and galvanization density is 0.1-6kA/m
2Direct current, anode produces chlorine, the negative electrode oxygen reduction generates hydrogen peroxide, the concentration of sodium hydroxide solution of intermediate chamber increases;
(3) the anolyte external heated reactive tank of flowing through, the chlorine hydrolysis generates hypochlorous acid, homogeneous chemical reaction takes place generate sodium chlorate, and anolyte is recycled electrolyzer anode chamber; By dripping acid or alkali, the pH of regulation and control circulating anode liquid is between 6-7.
2, the electrochemical method of production sodium chlorate and alkaline hydrogen peroxide in the time of according to claim 1, the acid that it is characterized in that regulating and control the pH employing of circulating anode liquid is hypochlorous acid, and the alkali of employing is effusive through spissated sodium hydroxide solution for coming from the electrolyzer intermediate chamber.
3, the electrochemical method of production sodium chlorate and alkaline hydrogen peroxide in the time of according to claim 1, it is characterized in that described anodic material is that titanium is coated with plumbic oxide or titanium is coated with ruthenium, the material of described negative electrode is selected stainless steel plate, nickel plate, carbon felt, graphite particle, graphite fibre or through the composite graphite particle of carbon black or polytetrafluorethylecoatings coatings.
4, the electrochemical method of production sodium chlorate and alkaline hydrogen peroxide in the time of according to claim 1 is characterized in that described cationic exchange membrane selects polyethylene cationic exchange membrane, polyvinyl chloride-type cationic exchange membrane, tetrafluoroethylene conduction cationic exchange membrane or polysulfones sulfonic acid cationic exchange membrane for use.
5, the electrochemical method of production sodium chlorate and alkaline hydrogen peroxide in the time of according to claim 1 is characterized in that described anion-exchange membrane selects polyethylene anion-exchange membrane, butylbenzene quaternary ammonium anion exchange membrane, polysulfones anion-exchange membrane or pyridine quaternary ammonium anion exchange membrane for use.
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