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EP1330308A2 - Procede de dissolution de sels dans 1,2-dichloroethane par ultrasons et dispositif de mise en oeuvre de ce procede - Google Patents

Procede de dissolution de sels dans 1,2-dichloroethane par ultrasons et dispositif de mise en oeuvre de ce procede

Info

Publication number
EP1330308A2
EP1330308A2 EP01986621A EP01986621A EP1330308A2 EP 1330308 A2 EP1330308 A2 EP 1330308A2 EP 01986621 A EP01986621 A EP 01986621A EP 01986621 A EP01986621 A EP 01986621A EP 1330308 A2 EP1330308 A2 EP 1330308A2
Authority
EP
European Patent Office
Prior art keywords
ultrasound
edc
salt
sodium chloride
dissolving
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.)
Withdrawn
Application number
EP01986621A
Other languages
German (de)
English (en)
Inventor
Michael Benje
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.)
ThyssenKrupp Industrial Solutions AG
Original Assignee
Uhde GmbH
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 Uhde GmbH filed Critical Uhde GmbH
Publication of EP1330308A2 publication Critical patent/EP1330308A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F21/00—Dissolving
    • B01F21/02—Methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • B01F31/84—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations for material continuously moving through a tube, e.g. by deforming the tube
    • B01F31/841—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations for material continuously moving through a tube, e.g. by deforming the tube with a vibrating element inside the tube
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/013—Preparation of halogenated hydrocarbons by addition of halogens
    • C07C17/02—Preparation of halogenated hydrocarbons by addition of halogens to unsaturated hydrocarbons

Definitions

  • the invention is directed to a process for dissolving salts, in particular catalytically active sodium chloride NaCl and iron (III) chloride FeCl 3 , in liquid 1, 2-dichloroethane, hereinafter referred to as EDC, which is predominantly an intermediate
  • EDC monomeric vinyl chloride
  • PVC polyvinyl chloride
  • EDC hydrogen chloride HCI is produced.
  • EDC is therefore preferably produced from ethene C 2 H 4 and chlorine Cl 2 in such a way that a balanced balance is achieved according to the following reaction equations with regard to the hydrogen chloride HCl generated and consumed during the reactions:
  • reaction (1) which is also referred to as direct chlorination
  • the implementation of the reaction (1) is usually done as a gas-liquid interface reaction in a loop reactor, for which different embodiments are known, the resolution of the ethene C 2 H 4 being the rate-determining step or in the liquid phase.
  • the EDC itself is used as the solvent for the reactants. It has been shown for many years that the purity of the EDC produced in terms of economy and the product purity that can ultimately be achieved in relation to the reaction (2) and thus the overall process is of paramount importance. Therefore, many attempts have been made in the past to suppress the side reactions of reaction (1); this also includes the development of powerful catalyst systems.
  • the reaction (1) is of the type "addition reaction” and is generally by
  • the object of the invention is therefore to salt, in particular sodium chloride NaCl and iron (III) chloride FeCI 3 , in such an advantageous manner and amount.
  • the inventive method therefore achieves the object in that a suspension of solid, granular sodium chloride NaCl in liquid EDC, which contains iron (III) chloride FeCI 3 in dissolved form, is subjected to ultrasound and the suspension is then filtered ,
  • iron (III) chloride FeCl 3 and sodium chloride NaCl are suspended together in EDC.
  • the iron (III) chloride FeCI 3 first goes into solution, and as soon as enough iron (III) chloride FeCI 3 has gone into solution, the sodium chloride NaCl in the EDC, which is now iron, also becomes Contains (III) chloride FeCI 3 in dissolved form, dissolved by ultrasound.
  • the clear solution obtained whose molar ratio of iron (III) chloride FeCl 3 to sodium chloride NaCl can optionally be up to 1: 1, is mixed into the reaction medium.
  • the method according to the invention can be operated in the secondary flow while the system is in operation, or can be designed as a batch operation.
  • the addition of sodium chloride NaCl in EDC and its dissolution by means of ultrasound can be carried out either in separate devices or in a common device.
  • Fig. 1 shows schematically an embodiment of the method according to the invention.
  • Fig. 2 shows the schematic view of a preferred device for performing the method
  • a dissolving device 1 for sodium chloride in conjunction with a loop reactor 11.
  • the sodium chloride suspension 2 is added to the dissolving device 1.
  • sodium chloride NaCl can also be added as a bed through an opening or a sluice device in the dissolving device 1, but it must then be ensured that no vaporous EDC can escape, since EDC is very toxic.
  • Liquid EDC 3 is supplied to the dissolving device 1 as the solvent.
  • the ultrasound transducer hereinafter referred to as sonotrode 4, which is connected to the ultrasound transmitter 5, is located in the opening device 1.
  • the sonotrode 4 introduces the ultrasound into the suspension.
  • the solution 6 leaves the dissolving device 1 after it has previously been filtered by a filter device 7.
  • Solution 6 is injected, for example, directly into the loop reactor 11, but it is possible, without departing from the inventive concept, to use an addition point at another, more favorable point in the EDC circuit.
  • the loop reactor H consists of the chlorine addition 8, chlorine dissolving section 9, the riser pipe 10, the down pipe 12, the ethene addition 13 and the evaporation tank 14.
  • EDC produced can be drawn off either as EDC vapor 15 or as liquid EDC 16.
  • a partial stream of the EDC produced can be used again for dissolving sodium chloride NaCl in the dissolving device 1, although it is possible to use any other EDC partial stream from the EDC circuit without departing from the inventive concept.
  • FIG. 2 shows a preferred device with a dissolving chamber 17, a cylindrical sonotrode 18 and a filtration device 19.
  • the entire device can be used both in batch operation and in continuous operation.
  • a feed lock for salts can be attached to the filling flange 20.
  • the solvent EDC is fed to the dissolving chamber 17, the outlet for the solution is the discharge line 23.
  • the filled salt is also in suspension in the dissolving chamber 17, which is at least up to the level of
  • the discharge line is filled with liquid EDC and is rendered inert in the gas space above.
  • the salt particles in the dissolving chamber 17 are conveyed by the flow against the filtration device 19, where they are retained in the filter cake that forms.
  • this filter cake is subjected to ultrasound from the submerged sonotrode, as a result of which passive layers forming on the salt crystals are continuously removed and the sparingly soluble salt dissolves. It is advantageous to arrange the filtration device in such a way that a large surface enveloping the sonotrode is formed. On the one hand, the distance between the filtration device and the sonotrode must be large enough to accommodate the filter cake and not impair the flow, on the other hand, the distance Do not exceed a few centimeters so that the ultrasonic waves can reach the filter cake without weakening.
  • FIG. 2 also shows a generally closed emptying device 24 and the ultrasound transmitter 5 required for the operation of the cylindrical sonotrode 18.
  • Shut-off devices, inerting devices and measures against explosion risk that are necessary in the field are not shown the EDC manufacturing specialist will of course undertake.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé et un dispositif de dissolution de sel difficilement soluble, en particulier de chlorure de sodium, et d'autres sels difficilement solubles dans 1,2-dichloroéthane, ladite dissolution trouvant notamment son application dans des dispositifs de chloration directe pour la fabrication de 1,2-dichloroéthane. A cet effet, une sonde à ultrasons (sonotrode) est disposée et exploitée dans une chambre de dissolution contenant une suspension de sels cristallins et de 1,2-dichloroéthane. Cette suspension est filtrée après le processus de dissolution.
EP01986621A 2000-10-10 2001-09-27 Procede de dissolution de sels dans 1,2-dichloroethane par ultrasons et dispositif de mise en oeuvre de ce procede Withdrawn EP1330308A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10050315A DE10050315C2 (de) 2000-10-10 2000-10-10 Verfahren zur Auflösung von Salzen in 1,2-Dichlorethan mittels Ultraschall und Vorrichtung zur Durchführung des Verfahrens
DE10050315 2000-10-10
PCT/EP2001/011188 WO2002030563A2 (fr) 2000-10-10 2001-09-27 Procede de dissolution de sels dans 1,2-dichloroethane par ultrasons et dispositif de mise en oeuvre de ce procede

Publications (1)

Publication Number Publication Date
EP1330308A2 true EP1330308A2 (fr) 2003-07-30

Family

ID=7659388

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01986621A Withdrawn EP1330308A2 (fr) 2000-10-10 2001-09-27 Procede de dissolution de sels dans 1,2-dichloroethane par ultrasons et dispositif de mise en oeuvre de ce procede

Country Status (7)

Country Link
US (1) US6956143B2 (fr)
EP (1) EP1330308A2 (fr)
JP (1) JP2004510576A (fr)
AU (1) AU2002215908A1 (fr)
DE (1) DE10050315C2 (fr)
NO (1) NO20031633D0 (fr)
WO (1) WO2002030563A2 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004025836B3 (de) * 2004-05-24 2005-12-22 Dr. Hielscher Gmbh Verfahren und Vorrichtung zum Einbringen von Ultraschall in ein fließfähiges Medium
US7846341B2 (en) 2006-12-04 2010-12-07 Bacoustics, Llc Method of ultrasonically treating a continuous flow of fluid
CN105311857A (zh) * 2015-12-02 2016-02-10 上海矩源自动化科技有限公司 超声波逆流循环反应器及物料提取浓缩系统

Family Cites Families (22)

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DE813706C (de) 1948-10-02 1952-01-07 Atlas Werke Ag Verfahren zum Extrahieren von Stoffen, insbesondere fuer pharmazeutische Zwecke
NL6901398A (fr) 1969-01-29 1969-11-25
US3729543A (en) * 1971-01-21 1973-04-24 Dunn Inc Wendell E Process for preparing alkali-metal tetra-chloroferrate
IT1012014B (it) 1971-06-01 1977-03-10 Zaccheroni V E C Di Apparecchio dosatore e miscelatore ad ultrasuoni particolarmente adat to per la preparazione di bevande da prodotti liofilizzati e metodo di fabbricazione e funzionale di tale apparecchio
DE2540291C3 (de) 1975-09-10 1984-02-23 Hoechst Ag, 6230 Frankfurt Verfahren zur kontinuierlichen Herstellung von 1,2-Dichloräthan und Katalysatorbehälter als Bestandteil einer Vorrichtung zur Durchführung des genannten Verfahrens
DE2803285C3 (de) * 1978-01-26 1980-10-23 Wacker-Chemie Gmbh, 8000 Muenchen Verfahren zur kontinuierlichen Chlorierung von Olefinen in flüssiger Phase sowie Meßanordnung zur Durchführung dieses Verfahrens
DE3137513A1 (de) * 1981-09-21 1983-04-07 Hoechst Ag, 6230 Frankfurt Verfahren zur herstellung von 1,2-dichlorethan
EP0075742B1 (fr) 1981-09-21 1984-11-07 Hoechst Aktiengesellschaft Procédé pour la préparation de 1,2-dichloroéthane
DE3148450A1 (de) 1981-12-08 1983-06-16 Hoechst Ag, 6230 Frankfurt Katalysatorgemisch und verfahren zur herstellung von 1,2-dichlorethan
CH665629A5 (en) 1985-02-05 1988-05-31 Nicolas Szekasy Dr Tri:alkoxyphenyl-haloalkyl ketone prodn. from tri:alkoxybenzene - and halo:alkanoyl halide, in presence of ferric chloride; are intermediates for vasodilating aminoalkyl analogues
JPH02103496A (ja) 1988-10-12 1990-04-16 Power Reactor & Nuclear Fuel Dev Corp 超音波を利用した使用済み核燃料等の溶解方法
DE3902665A1 (de) 1989-01-30 1990-08-02 Harald Garbe Verfahren zur veredelung von anorganisch nichtmetallischen fasern insbesondere keramikfasern sowie vorrichtung zur durchfuehrung dieses verfahrens
DE4103281A1 (de) 1991-02-04 1992-08-06 Buna Ag Verfahren zur herstellung von 1,2-dichlorethan
DE4133810A1 (de) 1991-10-12 1993-04-15 Hoechst Ag Verfahren zur reaktionsenthalpie-nutzung bei der herstellung von 1,2-dichlorethan
FR2691168B1 (fr) * 1992-05-18 1995-01-20 Atochem Elf Sa Procédé de dégraissage d'une pluralité d'objets.
DE4318609A1 (de) 1993-01-27 1994-07-28 Hoechst Ag Verfahren und Vorrichtung zur Herstellung von 1,2-Dichlorethan durch Direktchlorierung
ES2108423T3 (es) * 1993-01-27 1997-12-16 Hoechst Ag Procedimiento y dispositivo para la preparacion de 1,2-dicloroetano por cloracion directa.
DE4425872A1 (de) 1994-07-21 1996-01-25 Hoechst Ag Verfahren und Vorrichtung zur Herstellung von 1,2-Dichlorethan durch Direktchlorierung unter Abgasrückführung
DE19524712C2 (de) * 1995-07-11 1997-07-03 Metallgesellschaft Ag Vorrichtung zur Durchführung chemischer Reaktionen
CN1157310A (zh) 1995-11-22 1997-08-20 琳得科株式会社 粘合剂组合物和粘合片
FR2742352B1 (fr) 1995-12-18 1998-02-27 Ixtlan Ag Procede et appareil pour filtrer des substances liquides ou pateuses et/ou pour separer des composants inclus dans ces substances
DE19641562A1 (de) * 1996-07-04 1998-01-08 Hoechst Ag Verfahren zur Herstellung von 1,2-Dichlorethan durch Direktchlorierung

Non-Patent Citations (1)

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Title
See references of WO0230563A2 *

Also Published As

Publication number Publication date
AU2002215908A1 (en) 2002-04-22
WO2002030563A3 (fr) 2002-06-27
WO2002030563A2 (fr) 2002-04-18
NO20031633L (no) 2003-04-09
DE10050315A1 (de) 2002-04-18
DE10050315C2 (de) 2003-08-21
US6956143B2 (en) 2005-10-18
NO20031633D0 (no) 2003-04-09
US20030183798A1 (en) 2003-10-02
JP2004510576A (ja) 2004-04-08

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