WO1998033753A1 - Procede de retraitement du 1,2-dichloroethane produit lors de l'oxychloration - Google Patents

Procede de retraitement du 1,2-dichloroethane produit lors de l'oxychloration Download PDF

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Publication number
WO1998033753A1
WO1998033753A1 PCT/EP1998/000462 EP9800462W WO9833753A1 WO 1998033753 A1 WO1998033753 A1 WO 1998033753A1 EP 9800462 W EP9800462 W EP 9800462W WO 9833753 A1 WO9833753 A1 WO 9833753A1
Authority
WO
WIPO (PCT)
Prior art keywords
zone
washing
oxychlorination
edc
catalyst
Prior art date
Application number
PCT/EP1998/000462
Other languages
German (de)
English (en)
Inventor
Peter Schwarzmaier
Ingolf Mielke
Original Assignee
Vinnolit Monomer Gmbh & Co. Kg
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 Vinnolit Monomer Gmbh & Co. Kg filed Critical Vinnolit Monomer Gmbh & Co. Kg
Priority to AU62142/98A priority Critical patent/AU6214298A/en
Publication of WO1998033753A1 publication Critical patent/WO1998033753A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
    • C07C17/15—Preparation of halogenated hydrocarbons by replacement by halogens with oxygen as auxiliary reagent, e.g. oxychlorination
    • C07C17/152—Preparation of halogenated hydrocarbons by replacement by halogens with oxygen as auxiliary reagent, e.g. oxychlorination of hydrocarbons
    • C07C17/156—Preparation of halogenated hydrocarbons by replacement by halogens with oxygen as auxiliary reagent, e.g. oxychlorination of hydrocarbons of unsaturated hydrocarbons

Definitions

  • EDC 2-dichloroethane
  • This method has been known for a long time and is used on a large scale and in several variants in technology.
  • DE-C 43 03 086 describes a process for the production of pure EDC by oxychlorination of ethylene with hydrogen chloride and oxygen at temperatures from 190 to 250 ° C. and pressures from 2 to 6 bar in the presence of a copper (II) -chloride on a supported catalyst in a fluidized bed fluidized by recycle gas known as a reaction zone, which is characterized in that a) over a first
  • wash sodium hydroxide solution metered in and returned to the washing zone e) takes another part of sodium hydroxide solution from the residence zone, feeds this part to a stripping zone, from which the stripped liquid phase is discharged as waste water from the process and the condensed gauges are returned to the separation zone of stage g); f) the washed reaction gas from the washing zone in a condensation zone into uncondensed recycle gas, which is returned to the reaction zone, and the liquid phase is separated; g) the liquid phase in a separation zone in water, which is returned to the washing zone, and raw EDC separates; h) the crude EDC is purified in a distillation zone by adding sodium hydroxide solution to the top product mixture of water and low boilers, recycling the resulting aqueous sodium hydroxide solution to the washing zone and removing the condensed low boilers from the process and the pure EDC as the bottom product of the distillation zone takes.
  • the oxygen required for the oxychlorination can also be supplied in the form of air.
  • the gases containing oxygen in the air cause the fluidization of the catalyst bed and leave the reactor practically unchanged.
  • the entrained catalyst can be removed by the process described in DE-A-41 32 030, ie in a dry operated cleaning zone from the raw EDC gas stream.
  • the method according to the invention brings - in addition to the already mentioned prevention of disruptive deposits in the systems - a number of further advantages:
  • the reaction gases are washed in one
  • Wash tower with four to twenty floors.
  • Aqueous sodium hydroxide solution with a concentration of 5 to 25% by weight is metered into the washing medium, which is expediently carried out in countercurrent, in such an amount that the washing water running off has a pH of 10 to 12.
  • the washed reaction gases pass into a condensation zone and then into a separation zone in which phase separation takes place.
  • the aqueous phase is returned to the wash tower and the organic
  • Another aspect of the invention relates to analytical monitoring of the reaction. It has been found that the composition of the process gases advantageously takes place immediately after the catalyst has been separated off. For this purpose, a partial stream is branched off after the catalyst has been removed and passed through a condensation zone in which the EDC is separated off. The uncondensed portions are monitored for the content of carbon monoxide / carbon dioxide, hydrogen chloride and ethylene. In this way, process values can be obtained that allow direct control of the hydrogen chloride and / or ethylene supply. Furthermore, the oxygen content is monitored, which is expediently kept below about 0.5% by volume in order to conduct the process safely and well below the explosion limit.
  • the process according to the invention can be mastered well and can be carried out, for example, in such a way that the hydrogen chloride is completely converted.
  • the invention further relates to a device which is suitable for carrying out the method according to the invention.
  • the figure schematically represents a preferred embodiment of the invention.
  • This device consists essentially of a reactor 1, the gas discharge 2 with a
  • Catalyst separator 3 is connected, from which the process gases pass via line 4 into a washing zone 5, from which they are led via line 6 into a condensation stage 7, from which the condensate via line 8 into a separation zone 9 arrives, from which the EDC formed is removed via line 10.
  • 11 is the supply for ethylene and 12 and 13 respectively designate the supply for hydrogen chloride and oxygen or the oxygen-containing gas.
  • the reactor 1 advantageously contains a mixing device 14, for example a static mixer or a device with a similar effect, which ensures intensive mixing of the reaction participants.
  • a mixing device 14 for example a static mixer or a device with a similar effect, which ensures intensive mixing of the reaction participants.
  • Washing towers and columns are suitable as washing zone 5.
  • 16 a circuit line for the washing medium. A portion of the washing medium can be removed via line 17. 18 denotes a line for feeding the aqueous phase from the separation zone 9 into the circuit line 16.
  • Condensation stage 23 are passed to the analytical measuring devices 24.
  • the circuit line 16 advantageously contains one or more measuring devices (not shown in the drawing) for measuring the metering of the sodium hydroxide solution via the line 15. This control can be carried out, for example, via the pH value or via the electrical conductivity, as described, for example, in German patent application 196 31 382.1 of August 2, 1996 was proposed.
  • the design of the method according to the invention also allows EDC of different purity levels from other sources to be fed into the device at a suitable point. If this EDC contains acidic components, these are also reliably removed.
  • the method and the device according to the present invention allow perfect control of the method and enable rapid control if there are deviations from the specified values.
  • Separate devices for the separation of carbon dioxide, for example from the low-boiling fractions, are not required.
  • the washed EDC passes via line 6 into the condensation stage 7, from which the condensed EDC passes via line 8 into the separation zone 9, from which it is removed via line 10.
  • EDC contains no detectable amounts of carbon dioxide and chloral.
  • Condensation stage 19 from which, on the one hand, residual condensed EDC is passed via line 20 into the separation zone 9 and, on the other hand, the gases are returned to the reactor 1 via line 21.
  • the analytical monitoring of the reaction takes place via branch line 22 from line 4, which leads to measuring devices 24 via a condensation stage 23.
  • the ratio of carbon monoxide to carbon dioxide and the proportions of unused reactants are measured.
  • the supply of the reactants is regulated so that the analytical monitoring gives the following values:

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

On peut retraiter plus facilement les composants gazeux qui se dégagent lors de la production de 1,2-dichloroéthane par oxychloration en faisant passer les composants gazeux à travers un catalyseur qui provoque leur précipitation dans une zone de lavage dans laquelle les éléments constitutifs acides sont séparés au moyen d'une solution alcaline de lavage.
PCT/EP1998/000462 1997-02-03 1998-01-29 Procede de retraitement du 1,2-dichloroethane produit lors de l'oxychloration WO1998033753A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU62142/98A AU6214298A (en) 1997-02-03 1998-01-29 Process for recycling 1,2-dichloroethane from oxychlorination

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19703857.3 1997-02-03
DE1997103857 DE19703857A1 (de) 1997-02-03 1997-02-03 Verfahren zur Aufarbeitung von 1,2-Dichlorethan aus Oxichlorierung

Publications (1)

Publication Number Publication Date
WO1998033753A1 true WO1998033753A1 (fr) 1998-08-06

Family

ID=7819072

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1998/000462 WO1998033753A1 (fr) 1997-02-03 1998-01-29 Procede de retraitement du 1,2-dichloroethane produit lors de l'oxychloration

Country Status (4)

Country Link
AU (1) AU6214298A (fr)
CO (1) CO4990993A1 (fr)
DE (1) DE19703857A1 (fr)
WO (1) WO1998033753A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19753165B4 (de) 1997-12-01 2006-10-19 Vinnolit Monomer Gmbh & Co. Kg Verfahren zur Herstellung von 1,2-Dichlorethan durch Oxichlorierung
DE10059229A1 (de) * 2000-11-29 2002-06-13 Vinnolit Technologie Gmbh & Co Verfahren zur Herstellung von mit Bezug auch Chloral sehr reinem 1,2-Dichlorethan (EDC), das durch Oxichlorierung hergestellt worden ist
EP1228023B1 (fr) * 2000-11-29 2004-04-28 Vinnolit GmbH & Co. KG Procede de fabrication de 1,2-dichloroethane
DE102011108211A1 (de) 2011-07-21 2013-01-24 Thyssenkrupp Uhde Gmbh Verfahren zum Konzentrieren wässriger Lauge und dafür geeignete Vorrichtung

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1518931A1 (de) * 1965-05-24 1969-07-10 Goodrich Co B F Verfahren zur Herstellung von 1,2-Dichloraethan
GB1189815A (en) * 1967-05-22 1970-04-29 Mitsui Toatsu Chemicals Catalytic Chlorination of Ethylene
US3996300A (en) * 1976-03-18 1976-12-07 The Dow Chemical Company Removal of chloral from effluent gas of 1,2-dichloroethane synthesis
FR2314907A1 (fr) * 1975-06-17 1977-01-14 Allied Chem Procede cyclique d'oxychlorhydratation d'ethylene avec emissions d'hydrocarbures reduites et dichlorure d'ethylene ainsi obtenu
US4042640A (en) * 1975-11-06 1977-08-16 The Lummus Company Oxychlorination of hydrocarbons
DE4132030A1 (de) * 1991-09-26 1993-04-01 Hoechst Ag Verfahren zur entfernung des katalysatorabriebs aus 1,2-dichlorethan
DE4303086A1 (de) * 1993-02-04 1994-08-18 Hoechst Ag Verfahren zur Herstellung von reinem 1,2-Dichlorethan durch Oxichlorierung

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1518931A1 (de) * 1965-05-24 1969-07-10 Goodrich Co B F Verfahren zur Herstellung von 1,2-Dichloraethan
GB1189815A (en) * 1967-05-22 1970-04-29 Mitsui Toatsu Chemicals Catalytic Chlorination of Ethylene
FR2314907A1 (fr) * 1975-06-17 1977-01-14 Allied Chem Procede cyclique d'oxychlorhydratation d'ethylene avec emissions d'hydrocarbures reduites et dichlorure d'ethylene ainsi obtenu
US4042640A (en) * 1975-11-06 1977-08-16 The Lummus Company Oxychlorination of hydrocarbons
US3996300A (en) * 1976-03-18 1976-12-07 The Dow Chemical Company Removal of chloral from effluent gas of 1,2-dichloroethane synthesis
DE4132030A1 (de) * 1991-09-26 1993-04-01 Hoechst Ag Verfahren zur entfernung des katalysatorabriebs aus 1,2-dichlorethan
DE4303086A1 (de) * 1993-02-04 1994-08-18 Hoechst Ag Verfahren zur Herstellung von reinem 1,2-Dichlorethan durch Oxichlorierung

Also Published As

Publication number Publication date
DE19703857A1 (de) 1998-08-06
AU6214298A (en) 1998-08-25
CO4990993A1 (es) 2000-12-26

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