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WO2008002197A1 - Procédé de production de chlore - Google Patents

Procédé de production de chlore Download PDF

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Publication number
WO2008002197A1
WO2008002197A1 PCT/RU2007/000336 RU2007000336W WO2008002197A1 WO 2008002197 A1 WO2008002197 A1 WO 2008002197A1 RU 2007000336 W RU2007000336 W RU 2007000336W WO 2008002197 A1 WO2008002197 A1 WO 2008002197A1
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WO
WIPO (PCT)
Prior art keywords
pulse
gaseous mixture
discharge
hydrogen chloride
less
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.)
Ceased
Application number
PCT/RU2007/000336
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English (en)
Russian (ru)
Inventor
Alexandr Borisovich Beilin
Mikhail Borisovich Beilin
Anjelika Sergeevna Karpova
Sergei Jurievich Sokovnin
Alexandr Mikhailovich Efremov
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Obschestvo S Ogranichennoi Otvetstvennostju 'ksm-Engineering'
Original Assignee
Obschestvo S Ogranichennoi Otvetstvennostju 'ksm-Engineering'
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Obschestvo S Ogranichennoi Otvetstvennostju 'ksm-Engineering' filed Critical Obschestvo S Ogranichennoi Otvetstvennostju 'ksm-Engineering'
Publication of WO2008002197A1 publication Critical patent/WO2008002197A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/03—Preparation from chlorides
    • C01B7/04—Preparation of chlorine from hydrogen chloride

Definitions

  • the claimed invention relates to a method for producing chlorine in the gas-phase oxidation of hydrogen chloride.
  • a known method of producing chlorine in the absence of a catalyst in the process of gas-phase oxidation of hydrogen chloride by atmospheric oxygen by continuously supplying a gaseous mixture containing hydrogen chloride and oxygen to the flowing reaction zone.
  • the process of oxidation of hydrogen chloride with oxygen with the formation of the target product is carried out in the zone of electrical impulse discharges created at a voltage of 10-40 kV (RU, 1801943 Al, valid 15.03.1993, IPC: COlB 7/04).
  • the specified method allows the oxidation process in the absence of a catalyst.
  • the basis of the claimed invention is the task of creating conditions for a stable and continuous process of oxidation of hydrogen chloride to create such a method for producing chlorine, which would increase the degree of conversion of hydrogen chloride with high technological stability of the feasibility of the method.
  • This problem is solved when creating a method for producing chlorine by continuously supplying a gaseous mixture containing hydrogen chloride and oxygen to a flowing reaction zone and oxidizing hydrogen chloride with oxygen to form the target product, in which, according to the invention, a gaseous mixture is supplied at a pressure of 1.1 to 5.0 bar and transfer the gaseous mixture to a state of low-temperature plasma by exposure to pulsed electric discharge and is carried out in an environment formed by a low-temperature LASMA oxidation of hydrogen chloride with oxygen, after which the gaseous mixture containing the oxidation product is withdrawn from the reaction zone is condensed and separated the desired product from the condensed water.
  • a microsecond streamer discharge as a pulsed electric discharge, generated at an accelerating voltage of at least 150 kV, pulse energy of at least 1.25 J, pulse repetition rate of not more than 10 kHz, pulse duration of not more than 10 microseconds, discharge current at least 80 A, or use a flash corona discharge generated at an accelerating voltage of 10 kV to 150 kV, an energy per pulse of at least 1.25 J, a pulse repetition rate of not more than 10 kHz, a pulse duration of not more e 10 microseconds, a discharge current is not less than 10 mA, or as a pulsed electric discharge by using a discharge forming unfocused an electron beam with an accelerating voltage of 150 kV, an energy per pulse of 1.75 J, and a pulse repetition rate of not more than 25 kHz.
  • the method of producing chlorine is based on the use of gaseous hydrogen chloride as a chlorine-containing raw material for the recovery of chlorine.
  • the inventive method for producing chlorine is that a gaseous mixture containing hydrogen chloride and oxygen is continuously fed at a pressure of from 1.1 to 5.0 bar into the flowing reaction zone.
  • the gaseous mixture is partially or completely converted to ionized gas, that is, it is converted to a low-temperature plasma by exposure to a pulsed electric discharge, for example, a microsecond streamer discharge, a discharge forming an unfocused electron beam, a flash corona discharge, a surface-barrier discharge, and smoldering discharge of atmospheric pressure.
  • a pulsed electric discharge for example, a microsecond streamer discharge, a discharge forming an unfocused electron beam, a flash corona discharge, a surface-barrier discharge, and smoldering discharge of atmospheric pressure.
  • an electric accelerating voltage of 10 kV to 200 kV is performed, the pulse energy is not less than 1.25 J, the pulse repetition rate is not more than 100 kHz, the pulse duration is not less than 100 nanoseconds, the discharge current is not less than 10 mA.
  • a microsecond streamer discharge generated at an accelerating voltage of at least 150 kV, pulse energy of at least 1.25 J, pulse repetition rate of not more than 10 kHz, pulse duration of not less than 100 nanoseconds, discharge current of not less than 80 A.
  • a flash corona discharge formed at accelerating voltage from 10 kV to 150 kV, pulse energy not less than 1.25 J, pulse repetition rate not more than 10 kHz, pulse duration not more than 10 microseconds, discharge current not less than 10 mA.
  • a surface-barrier discharge generated at an accelerating voltage of at least 150 kV, pulse energy of at least 1, 25 J, pulse repetition rate of not more than 10 kHz, pulse duration of not less than 100 nanoseconds, discharge current of not less than 80 A. It is also advisable to use a glow discharge of atmospheric pressure generated at an accelerating voltage of 10 kV to 50 kV, an energy per pulse of at least 1.25 J, a pulse repetition rate of not more than 10 kHz, a pulse duration of not more than 10 microseconds, and a discharge current of at least 10 mA.
  • the formation of the target product occurs, in accordance with the inventive method, from a gaseous mixture in a state of low temperature plasma.
  • the gaseous mixture containing the oxidation product is continuously withdrawn from the reaction zone, condensed and the desired product is isolated from condensed water.
  • pulsed electrical discharges it is possible to use well-known equipment.
  • a plasma-chemical reactor a generator of high-voltage pulses from nanosecond to microsecond duration, and a frequency electron accelerator can be used to output an unfocused electron beam into the gas medium.
  • the claimed method a high percentage conversion of the mixture to chlorine and water vapor is achieved.
  • the gas-vapor mixture is subjected to cooling in a condenser to 2-3 degrees. C.
  • the bulk of the water is separated.
  • the inventive method is feasible in the absence of catalysts, does not require the use of high temperatures - feasible at ambient temperature, has high reliability and consistently good technological performance.
  • Example 1 For a better understanding of the present invention, the following examples of its specific implementation. Example 1
  • Hydrogen chloride in an amount of 5.15 kg / h and oxygen in an amount of 1.13 kg / h are sent to the preliminary mixing chamber at a temperature of 20 degrees C, after which it is continuously fed at a pressure of 1.2 bar into the reaction zone of the plasma chemical reactor.
  • an unfocused electron beam from the electron frequency accelerator assembled according to the thyratron-pulse transformer-semiconductor current chopper scheme is formed.
  • the gaseous mixture At a pressure of 1.2 bar, under the influence of an unfocused electron beam, the gaseous mixture completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • composition of the reaction products chlorine - 5.0 kg / h, water - 1.27 kg / h.
  • Hydrogen chloride in an amount of 10.3 kg / h and oxygen in an amount of 2.26 kg / h are sent to the preliminary mixing chamber at a temperature of 20 degrees C, after which they are fed into the streamer discharge zone created in the generator of high-voltage pulses of nanosecond duration - operating voltage generator no less than 150 kV, pulse duration 500 nanoseconds.
  • the gaseous mixture Under the influence of the indicated streamer discharge, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zones are subjected to condensation in a capacitor-phase separator and the target product is isolated from condensed water.
  • composition of the reaction products chlorine - 10.0 kg / h, water - 2.54 kg / h.
  • Hydrogen chloride in an amount of 5.15 kg / h and oxygen in an amount of 1.13 kg / h are fed into the pre-mixing chamber at a temperature of 20 degrees C.
  • the formed reaction gaseous mixture is then continuously directed at a pressure of 1.2 bar through the annular collector to the reaction zone of the plasma chemical reactor into the zone of streamer discharges created by the high-voltage pulse generator at a discharge current of 80 A, voltage of 150 kV, pulse energy of 1.75 J, and repetition rate pulses up to 10 kHz.
  • the gaseous mixture In a flowing reaction zone at a pressure of 1.2 bar, the gaseous mixture is partially or completely converted to ionized gas, that is, the gaseous mixture is transferred to a low-temperature plasma state. Under the influence of the indicated streamer discharges, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • composition of the reaction products chlorine - 5.0 kg / h, water - 1.27 kg / h.
  • Hydrogen chloride in an amount of 52.425 kg / h and oxygen in an amount of 11.475 kg / h are fed into the preliminary mixing chamber at a temperature of 20 degrees C.
  • the resulting reaction gas mixture is then continuously fed through a ring manifold to a reaction zone at a pressure of 1.6 bar.
  • the gaseous mixture In a flowing reaction zone at a pressure of 1.6 bar, the gaseous mixture is partially or completely converted to ionized gas, that is, the gaseous mixture is transferred to a low-temperature plasma state.
  • the gaseous mixture Under the influence of these flare corona discharges, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • the composition of the reaction products chlorine - 49.96 kg / h, water - 12.62 kg / h.
  • Hydrogen chloride in an amount of 52.425 kg / h and oxygen in an amount of 11.475 kg / h are fed into the preliminary mixing chamber at a temperature of 20 degrees C.
  • the formed reaction gaseous mixture is then continuously directed through a ring collector to a reaction zone of a plasma chemical reactor into a flash corona discharge zone created by a high-voltage pulse generator with a discharge current of 12 mA, voltage of 150 kV, and a pulse repetition rate of up to lkHz.
  • the gaseous mixture In a flowing reaction zone at a pressure of 4.8 bar, the gaseous mixture is completely converted to ionized gas, that is, the gaseous mixture is transferred to a low-temperature plasma state.
  • the gaseous mixture Under the influence of these flare corona discharges, the gaseous mixture is completely converted into ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • the composition of the reaction products chlorine - 48.76 kg / h, water - 11.22 kg / h.
  • Hydrogen chloride in an amount of 5.15 kg / h and oxygen in an amount of 1.13 kg / h are sent to the preliminary mixing chamber at a temperature of 20 degrees. C, after which it is continuously fed at a pressure of 5.0 bar to the reaction zone of the plasma chemical reactor.
  • an unfocused electron beam from an electron frequency accelerator assembled according to the thyratron-pulse transformer-semiconductor current chopper scheme is formed.
  • the gaseous mixture At a pressure of 5.0 bar, under the influence of an unfocused electron beam, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • composition of the reaction products chlorine - 5.0 kg / h, water - 1.27 kg / h.
  • Hydrogen chloride in the amount of 10.3 kg / h and oxygen in the amount of 2.26 kg / h are sent to the preliminary mixing chamber at a temperature of 20 degrees C, after which it is supplied at a speed of 100 m / s to the glow discharge zone created by the high-voltage pulse generator nanosecond duration - the operating voltage of the generator is at least 30 kV, the pulse duration is 500 nanoseconds.
  • the gaseous mixture Under the influence of the indicated glow discharge, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • composition of the reaction products chlorine - 10.0 kg / h, water - 2.54 kg / h.
  • Hydrogen chloride in an amount of 5.15 kg / h and oxygen in an amount of 1.13 kg / h are fed into the pre-mixing chamber at a temperature of 20 degrees C.
  • the formed reaction gaseous mixture is then continuously directed at a pressure of 1.2 bar through the annular collector into the reaction zone of the plasma chemical reactor to the surface-barrier discharge zone created by the high-voltage pulse generator at a discharge current of 80 A, voltage of 50 kV, pulse energy of 1.75 J, pulse repetition rate up to 10 Hz.
  • the gaseous mixture In a flowing reaction zone at a pressure of 1.2 bar, the gaseous mixture is partially or completely converted to ionized gas, that is, the gaseous mixture is transferred to a low-temperature plasma state. Under the influence of the indicated surface-barrier discharge, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • Hydrogen chloride in an amount of 52.425 kg / h and oxygen in an amount of 11.475 kg / h are fed into the preliminary mixing chamber at a temperature of 20 degrees C.
  • the formed reaction gaseous mixture is then continuously directed through a ring collector to a reaction zone of a plasma chemical reactor at a pressure of 1.6 bar into a zone of surface-barrier discharge created by a high-voltage pulse generator at a discharge current of 100 A, voltage of 50 kV, pulse repetition rate up to 10 Hz, pulse duration no less than 100 nanoseconds.
  • the gaseous mixture In a flowing reaction zone at a pressure of 1.6 bar, the gaseous mixture is partially or completely converted to ionized gas, that is, the gaseous mixture is transferred to a low-temperature plasma state.
  • the gaseous mixture Under the influence of the indicated surface-barrier discharge, the gaseous mixture partially or completely turns into an ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • the composition of the reaction products chlorine - 49.96 kg / h, water - 12.62 kg / h.
  • Hydrogen chloride in an amount of 52.425 kg / h and oxygen in an amount of 11.475 kg / h are fed into the preliminary mixing chamber at a temperature of 20 degrees C.
  • the formed reaction gaseous mixture is then continuously fed at a pressure of 4.8 bar at a speed of 200 m / s into the reaction zone of the plasma chemical reactor into the atmospheric pressure glow discharge zone created by the high-voltage pulse generator at a discharge current of 12 mA, voltage of 50 kV, and pulse repetition rate up to lkHz .
  • the gaseous mixture is completely converted to ionized gas, that is, the gaseous mixture is transferred to a low-temperature plasma state.
  • the gaseous mixture Under the influence of these flare corona discharges, the gaseous mixture is completely converted into ionized gas and acquires the state of a low-temperature plasma.
  • hydrogen chloride is oxidized with oxygen, after which the gaseous mixture containing the oxidation product is removed from the reaction zone, condensed in a condenser-phase separator, and the target product is isolated from condensed water.
  • the composition of the reaction products chlorine - 48.76 kg / h, water - 11.22 kg / h.
  • the invention will find application, in particular, in the disposal of abhase hydrogen chloride formed in organochlorine synthesis processes.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)

Abstract

La présente invention concerne un procédé de production de chlore consistant à introduire en continu un mélange gazeux contenant du chlorure d'hydrogène et de l'oxygène à une pression comprise entre 1,1 et 5,0 bar; à faire passer ce mélange gazeux à l'état de plasma basse température dans une zone de réaction à écoulement sous l'action d'une décharge électrique par impulsion; à oxyder le chlorure d'hydrogène à l'aide d'oxygène dans le plasma basse température ainsi formé, puis à retirer le mélange gazeux contenant le produit d'oxydation de la zone de réaction et à condenser le mélange et à extraire le produit cible de l'eau ainsi condensée.
PCT/RU2007/000336 2006-06-20 2007-06-20 Procédé de production de chlore Ceased WO2008002197A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2006121532/15A RU2320534C1 (ru) 2006-06-20 2006-06-20 Способ получения хлора
RU2006121532 2006-06-20

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WO2008002197A1 true WO2008002197A1 (fr) 2008-01-03

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WO (1) WO2008002197A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105502293A (zh) * 2016-01-25 2016-04-20 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种低温等离子体制备氯气的方法
CN106082130A (zh) * 2016-08-12 2016-11-09 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种等离子体法盐酸制备氯气的方法
CN106335878A (zh) * 2016-08-12 2017-01-18 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种盐酸制备氯气的方法
US10272020B2 (en) 2013-12-23 2019-04-30 Imertech Sas Personal cleansing compositions comprising spherical perlite microspheres
CN111392692A (zh) * 2019-04-26 2020-07-10 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种高气压低温等离子体氯化氢氧化制备氯气的方法及装置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104591090B (zh) * 2014-12-22 2016-09-07 上海方纶新材料科技有限公司 一种氯化氢催化氧化制备氯气的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1801943A1 (ru) * 1991-03-19 1993-03-15 Волгоградский Политехнический Институт Способ получения хлора из хлористого водорода 2
RU2088565C1 (ru) * 1995-11-27 1997-08-27 Институт сильноточной электроники СО РАН Способ неполного окисления низших углеводородов в электрическом разряде и устройство для его осуществления
US5908607A (en) * 1996-08-08 1999-06-01 Sumitomo Chemical Co., Ltd. Process for producing chlorine
US5935390A (en) * 1996-02-29 1999-08-10 E. I. Du Pont De Nemours And Company Producing chlorine and hydrogen from hydrogen chloride by plasma process
RU2253607C1 (ru) * 2004-02-19 2005-06-10 ООО "КСМ-Инжиниринг" Способ получения хлора из газообразного хлористого водорода

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU331649A1 (ru) * 1970-09-22 1976-11-05 Способ получени хлора
SU487018A1 (ru) * 1973-02-16 1975-10-05 Сумгаитский Филиал Ордена Трудового Красного Знамени Институт Нефтехимических Процессов Им.Академика Ю.Г.Мамедалиева Ан Азерб.Сср Способ получени хлора окислением хлористого водорода воздухом на катализаторах

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1801943A1 (ru) * 1991-03-19 1993-03-15 Волгоградский Политехнический Институт Способ получения хлора из хлористого водорода 2
RU2088565C1 (ru) * 1995-11-27 1997-08-27 Институт сильноточной электроники СО РАН Способ неполного окисления низших углеводородов в электрическом разряде и устройство для его осуществления
US5935390A (en) * 1996-02-29 1999-08-10 E. I. Du Pont De Nemours And Company Producing chlorine and hydrogen from hydrogen chloride by plasma process
US5908607A (en) * 1996-08-08 1999-06-01 Sumitomo Chemical Co., Ltd. Process for producing chlorine
RU2253607C1 (ru) * 2004-02-19 2005-06-10 ООО "КСМ-Инжиниринг" Способ получения хлора из газообразного хлористого водорода

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10272020B2 (en) 2013-12-23 2019-04-30 Imertech Sas Personal cleansing compositions comprising spherical perlite microspheres
US10342746B2 (en) 2013-12-23 2019-07-09 Imertech Sas Cleansing compositions
US10583071B2 (en) 2013-12-23 2020-03-10 Imertech Sas Personal cleansing compositions comprising expanded perlite microspheres
CN105502293A (zh) * 2016-01-25 2016-04-20 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种低温等离子体制备氯气的方法
CN106082130A (zh) * 2016-08-12 2016-11-09 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种等离子体法盐酸制备氯气的方法
CN106335878A (zh) * 2016-08-12 2017-01-18 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种盐酸制备氯气的方法
CN111392692A (zh) * 2019-04-26 2020-07-10 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) 一种高气压低温等离子体氯化氢氧化制备氯气的方法及装置

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RU2320534C1 (ru) 2008-03-27

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