EP1283281B1 - Verfahren zur elektrochemischen Herstellung von Chlor aus wässrigen Lösungen von Chlorwasserstoff - Google Patents

Verfahren zur elektrochemischen Herstellung von Chlor aus wässrigen Lösungen von Chlorwasserstoff Download PDF

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Publication number
EP1283281B1
EP1283281B1 EP02016239A EP02016239A EP1283281B1 EP 1283281 B1 EP1283281 B1 EP 1283281B1 EP 02016239 A EP02016239 A EP 02016239A EP 02016239 A EP02016239 A EP 02016239A EP 1283281 B1 EP1283281 B1 EP 1283281B1
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EP
European Patent Office
Prior art keywords
cathode
chamber
oxygen
pressure
anode
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP02016239A
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German (de)
English (en)
French (fr)
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EP1283281A2 (de
EP1283281A3 (de
Inventor
Andreas Bulan
Fritz Dr. Gestermann
Hans-Dieter Pinter
Gerd Speer
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Bayer Intellectual Property GmbH
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Bayer MaterialScience AG
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Publication of EP1283281A3 publication Critical patent/EP1283281A3/de
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/26—Chlorine; Compounds thereof

Definitions

  • the invention relates to a method for the electrochemical production of chlorine from aqueous solutions of hydrogen chloride in an electrolytic cell.
  • aqueous solutions of hydrogen chloride are by-produced in the production of organic chlorine compounds by chlorination with elemental chlorine. Many of these organic chlorine compounds are intermediates for the large-scale production of plastics.
  • the resulting aqueous solutions of hydrogen chloride must be recycled. The recovery preferably takes place in such a way that chlorine is again produced from the aqueous solutions of hydrogen chloride, which can then be used, for example, for further chlorinations.
  • the conversion to chlorine can be carried out, for example, by electrolysis of the aqueous solutions of hydrogen chloride on a gas diffusion cathode.
  • a corresponding procedure is off US-A-5,770,035 and US-A-6149782 known.
  • the electrolysis takes place according to US-A-5,770,035 in an electrolytic cell with an anode compartment, with a suitable anode, for example a noble metal-coated or -doped titanium electrode, which is filled with the aqueous solution of hydrogen chloride.
  • the chlorine formed at the anode escapes from the anode compartment and is fed to a suitable treatment.
  • the anode compartment is separated from a cathode compartment by a commercially available cation exchange membrane.
  • a gas diffusion electrode is located on the cation exchange membrane. Behind the gas diffusion electrode is a power distributor. In the cathode space usually an oxygen-containing gas or pure oxygen is introduced.
  • the anode compartment is maintained at a higher pressure than the cathode compartment.
  • the adjustment of the pressure can be done, for example, by a liquid immersion, through which the chlorine gas formed in the anode chamber is passed.
  • the end US-A-5,770,035 known method has the disadvantage that at high current densities, which in particular current densities greater than 4000 A / m 2 are to be understood, a comparatively high amount of hydrogen is formed on the gas diffusion cathode.
  • high current densities are necessary in the technical implementation of the method for economic reasons.
  • US 6 149 782 A discloses a process for the electrochemical production of chlorine from aqueous solutions of hydrogen chloride in an electrolytic cell comprising an anode chamber and a cathode chamber.
  • the anode compartment is separated from the cathode compartment by a cation exchange membrane, Nafion 324.
  • the anode chamber contains an anode and the cathode chamber contains an oxygen-consuming cathode containing a rhodium compound catalyst.
  • An aqueous solution of hydrogen chloride is introduced into the anode chamber, and oxygen is introduced into the cathode chamber.
  • the partial pressure of the oxygen is 45-50 mbar, so the pressure in the cathode chamber is above 1.05 bar.
  • the object of the invention is to provide a method for the electrochemical production of chlorine from aqueous solutions of hydrogen chloride, wherein even when working with high current densities as little as possible hydrogen is formed and sets the lowest possible voltage.
  • the invention relates to a method according to claim 1 for the electrochemical production of chlorine from aqueous solutions of hydrogen chloride in an electrolytic cell, comprising at least one anode chamber and a cathode chamber, wherein the anode chamber is separated by a cation exchange membrane from the cathode chamber, the anode chamber an anode and the cathode chamber contains an oxygen-consuming cathode, and in the anode chamber, the aqueous solution of hydrogen chloride and in the cathode chamber, an oxygen-containing gas is introduced, wherein the absolute pressure in the cathode chamber is at least 1.05 bar.
  • oxygen-containing gas for example, pure oxygen, a mixture of oxygen and inert gases, in particular nitrogen, or air can be used. Pure oxygen, in particular a purity of at least 99% by volume, is preferably used as the oxygen-containing gas.
  • the indication of the pressure in the cathode chamber are absolute values.
  • the pressure in the cathode chamber is preferably 1.05 to 1.5 bar, particularly preferably 1.05 to 1.3 bar.
  • the adjustment of the pressure in the cathode chamber to the value according to the invention of at least 1.05 bar can be effected, for example, by accumulating the oxygen-containing gas supplied to the cathode chamber by means of a pressure-retaining device.
  • a suitable pressure-holding device is, for example, a liquid compression, by which the cathode space is shut off. Throttling via valves is also a suitable method for adjusting the pressure in the cathode compartment.
  • a pressure is set in the anode chamber, which is 200 to 500 mbar higher than the pressure in the cathode chamber.
  • the inventive method is operated at a current density of at least 5000 A / m 2 .
  • the temperature of the supplied aqueous solution of hydrogen chloride is preferably from 30 to 80 ° C, particularly preferably from 50 to 70 ° C.
  • the concentration of hydrochloric acid in the electrolyzer in carrying out the process according to the invention is 5 to 20 wt .-%, particularly preferably 10 to 15 wt .-%.
  • the consumed hydrochloric acid in the electrolyzer can be supplemented by a hydrochloric acid supplied to the electrolyzer in the concentration range from 8 to 36% by weight.
  • the oxygen-containing gas is preferably supplied in an amount such that oxygen is present in excess relative to the theoretically required amount. Particularly preferred is a 1.2 to 1.5-fold excess of oxygen.
  • the process according to the invention is carried out in an electrochemical cell (electrolysis cell) whose anode chamber is separated from the cathode chamber by a cation exchange membrane, the cathode chamber containing an oxygen-consuming cathode.
  • electrochemical cell electrolysis cell
  • the electrolytic cell used may, for example, comprise the following components: an anode in an anode chamber, a cation exchange membrane which is hydrostatically pressed onto an oxygen-consuming cathode (SVK), which in turn is supported on a cathode-side current distributor and thus electrically contacted, and a cathode-side gas space (cathode chamber) ,
  • the aqueous solution of hydrogen chloride is introduced into the anode chamber, the oxygen-containing gas in the cathode chamber.
  • oxygen-consuming cathode is not critical.
  • the known and partly commercially available oxygen-consuming cathodes can be used.
  • oxygen-consuming cathodes are used which contain a catalyst of the platinum group, preferably platinum or rhodium.
  • Suitable cation exchange membranes are those made of perfluoroethylene, which contain sulfonic acid groups as active centers. Both single-layer membranes having sulfonic acid groups of equal equivalent weights on both sides and membranes having sulfonic acid groups of different equivalent weights on both sides are suitable. Also membranes with carboxyl groups on the cathode side are conceivable.
  • Suitable anodes are, for example, titanium anodes, in particular with an acid-resistant, chlorine-developing coating.
  • the cathode-side power distributor can consist, for example, of expanded titanium metal or noble metal-coated titanium.
  • FIG Fig. 1 A suitable electrolytic cell for carrying out the method according to the invention is shown schematically in FIG Fig. 1 shown.
  • the electrolysis cell 1 is divided by a cation exchange membrane 6 into a cathode chamber 2 with an oxygen-consuming cathode 5 and an anode chamber 3 with an anode 4 .
  • the oxygen-consuming cathode 5 is located on the cathode side on the cation exchange membrane 6 .
  • Behind the Sauerstoffverzehrkathode 5 is a power distributor. 7 Due to the higher pressure in the anode chamber 3 , the cation exchange membrane 6 is pressed onto the oxygen-consuming cathode 5 and this in turn onto the current distributor 7 . In this way, the Sauerstoffverzehrkathode 5 is sufficiently electrically contacted and supplied with power.
  • a pressure maintenance 8 The adjustment of the pressure in the cathode chamber 2 and anode chamber 3 takes place respectively via a pressure maintenance 8.
  • a pressure maintenance 8 Via an HCl inlet 12 , an aqueous solution of hydrogen chloride is introduced into the anode chamber 3 , wherein formed at the anode 4 chlorine, which flows through the pressure maintenance 8 and discharged via the Cl 2 outlet 13 from the anode chamber 3 becomes.
  • an O 2 inlet 9 oxygen-containing gas is introduced into the cathode chamber 2 , where it reacts with the oxygen-consuming cathode 5 to form water with protons, which diffuse out of the anode chamber 3 into the oxygen-consuming cathode 5 .
  • the water formed is removed together with the excess oxygen-containing gas via the pressure maintenance 8 from the cathode chamber 2 , wherein the water formed via a H 2 O outlet 11 and the oxygen-containing gas via an O 2 outlet 10 is removed. It is also possible that the oxygen supply is from below and / or that the removal of water formed and oxygen-containing gas is carried out separately via a separate pressure maintenance.
  • the electrolysis was carried out in an electrolytic cell 1 divided into a cathode chamber 2 and an anode chamber 3 as shown in FIG Fig. 1 shown schematically and explained in more detail above.
  • An activated titanium anode with a size of 10 cm ⁇ 10 cm was used as anode 4 .
  • the anode chamber 3 was supplied with an aqueous solution of hydrogen chloride.
  • the temperature of the aqueous solution of hydrogen chloride was 60 ° C, the concentration 12-15 wt .-%.
  • a gas diffusion electrode of the company E-TEK, type ELAT which was directly on a power distributor 7 in the form of an activated expanded titanium metal.
  • Cathode chamber 2 and anode chamber 3 were separated from a cation exchange membrane 6 from DuPont, type Nafion® 324.
  • pure oxygen having a content of greater than 99 vol .-% was introduced at a temperature of 20 ° C.
  • the electrolysis was at a pressure in the anode chamber 3 of 1 , 4 bar, abs. and a pressure in the cathode chamber 2 of 1 bar, abs., A voltage of 1.67 V and a current density of 6000 A / m 2 operated.
  • the excess oxygen-containing gas was removed from the cathode chamber 2 together with the water formed.
  • the concentration of hydrogen in this gas was determined by gas chromatography. The hydrogen concentration was 700 ppm after an electrolysis time of 10 minutes, increased steadily during the electrolysis and was 1600 ppm after an electrolysis time of 3 hours.
  • Example 1 An electrolysis of an aqueous solution of hydrogen chloride was carried out as described in Example 1.
  • the pressure in the anode chamber 3 was 1.4 bar, abs.,
  • the pressure in the cathode chamber 2 1 bar, abs.,
  • the voltage 1.82 V and the current density 7000 A / m 2 were measured.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
EP02016239A 2001-08-03 2002-07-22 Verfahren zur elektrochemischen Herstellung von Chlor aus wässrigen Lösungen von Chlorwasserstoff Expired - Lifetime EP1283281B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10138215 2001-08-03
DE10138215A DE10138215A1 (de) 2001-08-03 2001-08-03 Verfahren zur elektrochemischen Herstellung von Chlor aus wässrigen Lösungen von Chlorwasserstoff

Publications (3)

Publication Number Publication Date
EP1283281A2 EP1283281A2 (de) 2003-02-12
EP1283281A3 EP1283281A3 (de) 2003-05-28
EP1283281B1 true EP1283281B1 (de) 2012-11-14

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EP02016239A Expired - Lifetime EP1283281B1 (de) 2001-08-03 2002-07-22 Verfahren zur elektrochemischen Herstellung von Chlor aus wässrigen Lösungen von Chlorwasserstoff

Country Status (7)

Country Link
US (1) US6790339B2 (es)
EP (1) EP1283281B1 (es)
CN (1) CN1247818C (es)
DE (1) DE10138215A1 (es)
ES (1) ES2397508T3 (es)
HK (1) HK1054575A1 (es)
PT (1) PT1283281E (es)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
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CA2445578C (en) 2001-04-27 2012-08-28 Johns Hopkins University Biological pacemaker comprising dominant-negative kir2.1aaa
DE10152275A1 (de) * 2001-10-23 2003-04-30 Bayer Ag Verfahren zur Elektrolyse von wässrigen Lösungen aus Chlorwasserstoff
ES2533254T3 (es) * 2002-11-27 2015-04-08 Asahi Kasei Chemicals Corporation Célula electrolítica bipolar, sin intersticios
DE10342148A1 (de) 2003-09-12 2005-04-07 Bayer Materialscience Ag Verfahren zur Elektrolyse einer wässrigen Lösung von Chlorwasserstoff oder Alkalichlorid
DE102006023261A1 (de) 2006-05-18 2007-11-22 Bayer Materialscience Ag Verfahren zur Herstellung von Chlor aus Chlorwasserstoff und Sauerstoff
JP5041769B2 (ja) * 2006-09-06 2012-10-03 住友化学株式会社 スタートアップ方法
DE102008015901A1 (de) * 2008-03-27 2009-10-01 Bayer Technology Services Gmbh Elektrolysezelle zur Chlorwasserstoffelektrolyse
WO2010119918A1 (ja) 2009-04-16 2010-10-21 クロリンエンジニアズ株式会社 ガス拡散電極を有する２室法イオン交換膜食塩電解槽を用いる電解方法
DE102009023539B4 (de) * 2009-05-30 2012-07-19 Bayer Materialscience Aktiengesellschaft Verfahren und Vorrichtung zur Elektrolyse einer wässerigen Lösung von Chlorwasserstoff oder Alkalichlorid in einer Elektrolysezelle
ES2643234T3 (es) 2010-03-30 2017-11-21 Covestro Deutschland Ag Procedimiento para la preparación de carbonatos de diarilo y policarbonatos
US9175135B2 (en) 2010-03-30 2015-11-03 Bayer Materialscience Ag Process for preparing diaryl carbonates and polycarbonates
US8562810B2 (en) 2011-07-26 2013-10-22 Ecolab Usa Inc. On site generation of alkalinity boost for ware washing applications
KR101585995B1 (ko) * 2012-01-10 2016-01-22 이시후꾸 긴조꾸 고오교 가부시끼가이샤 살균수 생성장치
SI2867388T1 (sl) * 2012-06-29 2019-08-30 Australian Biorefining Pty Ltd Postopek in naprava za proizvodnjo ali ponovno pridobivanje klorovodikove soli iz raztopin kovinskih soli

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Publication number Priority date Publication date Assignee Title
JPS534796A (en) * 1976-07-05 1978-01-17 Asahi Chem Ind Co Ltd Electrolysis of pressurized alkali halide
US4311568A (en) * 1980-04-02 1982-01-19 General Electric Co. Anode for reducing oxygen generation in the electrolysis of hydrogen chloride
IT1282367B1 (it) * 1996-01-19 1998-03-20 De Nora Spa Migliorato metodo per l'elettrolisi di soluzioni acquose di acido cloridrico
US6149782A (en) * 1999-05-27 2000-11-21 De Nora S.P.A Rhodium electrocatalyst and method of preparation
US6135331A (en) * 1999-08-13 2000-10-24 Davis; Richard Maurice Snow ski boot remover

Also Published As

Publication number Publication date
DE10138215A1 (de) 2003-02-20
JP2003049290A (ja) 2003-02-21
HK1054575A1 (zh) 2003-12-05
US6790339B2 (en) 2004-09-14
CN1405357A (zh) 2003-03-26
CN1247818C (zh) 2006-03-29
ES2397508T3 (es) 2013-03-07
EP1283281A2 (de) 2003-02-12
PT1283281E (pt) 2013-01-24
EP1283281A3 (de) 2003-05-28
US20030024824A1 (en) 2003-02-06
JP4251432B2 (ja) 2009-04-08

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