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WO1997022386A1 - Destruction d'hydrocarbures halogenes - Google Patents

Destruction d'hydrocarbures halogenes Download PDF

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Publication number
WO1997022386A1
WO1997022386A1 PCT/GB1996/003130 GB9603130W WO9722386A1 WO 1997022386 A1 WO1997022386 A1 WO 1997022386A1 GB 9603130 W GB9603130 W GB 9603130W WO 9722386 A1 WO9722386 A1 WO 9722386A1
Authority
WO
WIPO (PCT)
Prior art keywords
vessel
reaction
sodium
halocarbon
spine
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/GB1996/003130
Other languages
English (en)
Inventor
Ziad Omar El-Koussa
Ronald Eric Banks
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.)
MANCHESTER INSTITUTE OF SCIENCE and TECHNOLOGY, University of
University of Manchester
Original Assignee
MANCHESTER INSTITUTE OF SCIENCE and TECHNOLOGY, University of
University of Manchester
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 MANCHESTER INSTITUTE OF SCIENCE and TECHNOLOGY, University of, University of Manchester filed Critical MANCHESTER INSTITUTE OF SCIENCE and TECHNOLOGY, University of
Priority to AU11845/97A priority Critical patent/AU1184597A/en
Publication of WO1997022386A1 publication Critical patent/WO1997022386A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
    • A62D3/32—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by treatment in molten chemical reagent, e.g. salts or metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B01D53/70—Organic halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/07—Stirrers characterised by their mounting on the shaft
    • B01F27/072—Stirrers characterised by their mounting on the shaft characterised by the disposition of the stirrers with respect to the rotating axis
    • B01F27/0722—Stirrers characterised by their mounting on the shaft characterised by the disposition of the stirrers with respect to the rotating axis perpendicular with respect to the rotating axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
    • B01F27/192—Stirrers with two or more mixing elements mounted in sequence on the same axis with dissimilar elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/20—Organic substances
    • A62D2101/22—Organic substances containing halogen

Definitions

  • the present invention relates to the destruction of unwanted halocarbons
  • halocarbon refers to compounds which contain at least one carbon-halogen bond and which may contain atoms of other elements in addition to carbon and halogen
  • halocarbon covers (but is not limited to) CFCs (chlorofluorocarbons), Halons (bromofluoro- or bromochlorofluoro-carbons) and HCFCs (hydrochlorofluorocarbons)
  • Halocarbons have been used in numerous applications tor many years, e.g as refrigerants, solvents, fire extinguishants, foam blowing agents, aerosol propellants etc
  • halocarbons have proved to be useful chemical compounds, it is now well established that volatile members of this class containing chlorine and/or bromine deplete stratospheric ozone hence their dispersive use is now being phased out under the terms of the "Montreal Protocol on Substances that Deplete the Ozone Layer"
  • halocarbons e g in storage or inco ⁇ orated in equipment such as refrigerators
  • a halocarbon destruction method using molten sodium is disclosed in O-A-94/03237 (EA Technology and MANWEB) and comprises bubbling halocarbon vapours through molten sodium, the reaction being effected at atmospheric pressure
  • O-A-94/03237 EA Technology and MANWEB
  • the reaction can only be controlled satisfactorily if the halocarbon flow rate is very low and hot spots are avoided, since these lead to sparking, flames, and the formation of red hot glowing regions in the magma-like reaction mixture.
  • the flow rate of the halocarbon is increased, the reaction becomes more exothermic and sparking becomes more frequent especially since normal methods of stirring are inadequate; hence uncontrolled burning of the carbon produced is a common occurrence.
  • step (b) above means that the halocarbon is introduced into the headspace without firstly being bubbled or otherwise passed through the molten sodium or molten sodium dispersed with the inert soiid reaction products
  • the method of the invention is effected in an essentially air free environment and provides a number ot advantages
  • the reduced pressure allows the reaction between the molten sodium and halocarbon to proceed immediately without the induction pe ⁇ od encountered at atmospheric pressure
  • the reaction then proceeds smoothly without sparking or combustion and may easily be controlled simply by controlling the pressure of the reaction, as described more fully below
  • the time taken for complete reaction of the sodium is approximately one fifth of the time taken for reaction at atmospheric pressure and the other disadvantages of operating at atmospheric pressure (e g poor control of reaction) are avoided
  • the pressure of gaseous or vapou ⁇ sed halocarbon in the vessel at the start of the reaction should not exceed 20 mm (2 66 kPa) of mercury and more preferably does not exceed 10 mm ( 1 33 kPa) of mercurv
  • the initial pressure in the vessel containing the molten sodium (prior to introduction of the halocarbon) is less than 1 m (0 133 kPa) of mercury
  • an inert gas e.g. nitrogen
  • the molten sodium is initially at a temperature of 100 °C to 150 °C, ideally about 1 10 °C .
  • Halocarbon is then introduced directly into the reduced pressure headspace of the reaction vessel above the molten sodium and as a result an exothermic reaction is immediately initiated.
  • the pressure and temperature may be increased. Ideally however the pressure should not be allowed to increase above 0.6 atmospheres (61 kPa) [more preferably not above 0.5 atmospheres (51 kPa)] and the wall temperature of the vessel should preferably not exceed 350 °C (more preferably 300 °C) although may be higher if required (e.g. 350°C-400°C).
  • the halocarbon is one having a boiling point (at atmospheric pressure) of up to about 100 °C so as to be a gas or vapour at the low pressures at which it is supplied to the vessel. It is possible to employ the method of the invention to destroy higher boiling liquids, low-melting solids or sublimable solids but these will generally need to be heated to appropriate temperatures in separate vessels and the vapours produced then fed to the reaction vessel.
  • reaction is complete when further increase in pressure of the halocarbon is not matched by a rise in temperature of the reactor's contents. At this stage, substantially all of the sodium will have been consumed but, as a precaution, it is preferred (after terminating the halocarbon feed and removing to storage any unreacted halocarbon from the reactor, then cooling the vessel and returning it to atmospheric pressure) to introduce a lower alkanol (preferably methanol) into the reactor vessel so as to destroy any remaining sodium.
  • a lower alkanol preferably methanol
  • the reaction vessel may be washed at least one more time with alkanol then dried by evacuation before being recharged with sodium to effect a further reaction.
  • the method of the invention may be effected in a reaction vessel (e.g. of mild or stainless steel) equipped with a halocarbon inlet connected yja a three-way valve to a manometer and a vacuum system.
  • the vessel will be provided with a stirrer (for which constructions are described more fully below) and is preferably also equipped, at the base thereof, with a discharge facility to permit ready discharge of its contents, e.g. a plug or gate vaive.
  • the vessel is preferably also provided with means for heating the contents of the vessel and/or removing heat therefrom.
  • the stirring and grinding of the reactant/product mixture is preferably effected simultaneously by means of an appropriately designed stirrer assembly which is of relatively low surface area to prevent material sticking thereto.
  • the grinding is effected at a lower region of the stirrer assembly between a grinding element thereof and the wall of the vessel (which will generally be cylindrical)
  • the stirrer assembly is configured so as to move mate ⁇ al downwardly to the base for the material to be subjected to a grinding operation
  • the stirrer assembly is provided with vessel wall clearing means which sweep around the inner walls ofthe vessel to prevent/remove material adhering thereto
  • stirrer is magnetically d ⁇ ven for ease of maintaining a trouble- free, leakproof seal It is however possible to use other types of stirrer drive which are able to provide such seals
  • the stirrer is rotated in a direction such that material in the vessel is pushed by the spokes towards the base of the vessel for grinding to be effected
  • the stirrer is additionally provided with vessel wall dealing means which may comp ⁇ se generally U-shaped loops attached by their limbs (which may be provided by said spokes) to the spine of the assembly and arranged such that the "bases" of the loops sweep around the inner surface of the vessel
  • vessel wall dealing means may comp ⁇ se generally U-shaped loops attached by their limbs (which may be provided by said spokes) to the spine of the assembly and arranged such that the "bases" of the loops sweep around the inner surface of the vessel
  • CFCs chlorofluorocarbons
  • Halons bromofluoro- or bromochlorofluoro-carbons
  • CF 3 Br CF 2 ClBr
  • CF 2 BrCF 2 Br bromochlorofluoro-carbons
  • the invention may also be apphed to cyclic compounds and to compounds contaimng atoms other than those of carbon and the halogens
  • the invention may be applied to sulphur containing compounds such as CF j SCl, CF 3 SF 5 and (CF 3 ) 2 S as well as nitrogen containing compounds such as (CF 3 ) 3 N, CF 3 NF 2 , perfluoro-N-fluoropipe ⁇ dine and pentafluoropy ⁇ dine
  • Useful mate ⁇ als may be obtained from the product ot the reaction
  • the product of the destruction reaction comprises carbon, sodium fluoride and sodium bromide
  • the supernatant liquid obtained by filtration of the product/methanol slurry comp ⁇ ses sodium bromide dissolved in methanol Evaporation of the methanol leaves sodium bromide
  • the remaining "insoluble" residue in the slurry comprises carbon and sodium fluoride
  • This residue may be heated at 600 C - 700 °C in air (e in a muffle furnace) to burn off the carbon and leave sodium fluoride which is pure enough to be considered as a feedstock in the fluorochemicals industry
  • Fig 1 illustrates one embodiment of a stirrer assembly which mav be used in the method of the invention
  • Fig. 2 illustrates one embodiment of apparatus for effecting destruction of halocarbons using the method ofthe invention
  • the illustrated stirrer assembly 1 (see Fig 1 ) which is attached in conventional removable fashion to the drive shaft of a magnetic or other type of mechanical stirrer comprises a central spine 2 on which are arranged a plurality ot parallel spokes 3 which are spaced along the length ot spine 2 and which extend transversely to the axis thereof. As clearly shown in Fig. 1 , the spokes 3 are arranged in helical fashion around the spine 2.
  • the spine 2 needs to be robust and purely by way of example we have found that a 1 cm diameter spine in a 7.6 cm diameter reactor is suitable.
  • the spine 2 At its base the spine 2 has a grinding arrangement comprised of two diametrically opposite arms 4 each having, at their ends remote from the spine 2, an upstanding grinding element 5.
  • a further feature of the illustrated stirrer assembly is that certain spokes designated as 3a provide limbs of U-shaped loops having a "base " 6 joining the limbs 3a.
  • the illustrated stirrer assembly is intended for location in a vessel 7 as represented by dashed lines.
  • the grinding elements 5 are closely spaced from the inner wall of the vessel as are the '" bases" 6 of the U- shaped loops which provide vessel wall clearing means.
  • the stirrer In use, the stirrer is rotated in a direction such that the spokes 3 push material within the vessel 7 towards the base thereof so that a grinding operation may be effected by the grinding elements 5.
  • the "bases" 6 of the U-shaped loops act as brushes and sweep around the inner walls of the vessel 7 so as to prevent material sticking thereto.
  • the relatively narrow cross section of the spokes 3 ensures that material does not adhere thereto.
  • spokes 3 and "bases" 6 are shown as being of circular section they could be made of generally rectangular plate, although it may be desirable for the brushes 6 to have rounded edges.
  • the illustrated apparatus comprises a stainless-steel cylindrical reactor 20 capable of use under vacuum.
  • the reactor is equipped with a magnetically-driven spiral-spoke stirrer assembly 1 (of the type described with reference to Fig. 1 ), a heater unit 21, thermocouple points 22 and 23, a bolt-on lid 24 carrying inlet lines 25 and 26. a vacuum/pressure gauge 27, and the stirrer motor unit 28.
  • a plug valve 29 is fixed to the base of the reactor 20 to allow removal of solid products.
  • Halocarbon to be destroyed is supplied from a reservoir 30 which is positioned on a weighing mechanism 31.
  • a line 32 connects reservoir 30 to line 26 via a valve 33 and a fine control valve 34.
  • a T' valve 35 Provided in the line 32 is a T' valve 35, the leg 36 of which communicates with (i) a vacuum hne 37 via a valve 38. and (n) a standard mercury manometer 39 via a valve 40.
  • the mercury manometer enables headspace pressures (hence rate of consumption of halocarbons) to be determined accurately
  • a line 41 is connected to inlet line 26 via a valve 42 and serves for the supply of mtrogen
  • the invention is further illustrated by the following non-limiting Examples which were effected using an apparatus as illustrated in Fig 2.
  • the volume of the reactor vessel 20 being 1 litre
  • the reactor described above was charged with sodium (200 g), evacuated and heated to 250 °C The heater was then turned off and sti ⁇ er activated (c ⁇ 300 rpm) before the valves isolating the reactor from the halocarbon storage vessel were opened to allow bromotrifluoromethane (Halon 1301, b p -57 °C) to bleed slowly from the storage cylinder into the headspace of the evacuated reactoi Throughout this operation, the reactor headspace pressure and temperature. the reactor wall temperature and the rate mineralisation of the halocarbon were monitored regularly (see Table 1).
  • total CF 3 Br destroyed 315 g, determined by change in weight of the stock cylinder, which was connected to the reactor via a flexible tube
  • the storage cylinder was closed, and bromotrifluoromethane remaining in the reactor and the connecting line was pumped out for recovery before the vessel was allowed to cool to room temperature, the vacuum broken by admitting dry nitrogen, and methanol (3 x 400 cm ) introduced to act as quenching agent for any unreacted sodium and to create a siurry which was removed via the reactor ' s plug valve.
  • Example 1 was repeated, using 100 g of sodium to destroy 158 g of bromotrifluoromethane (99 8% utilisation of sodium) over 310 minutes, du ⁇ ng which time the pressure of this halocarbon in the headspace of the reactor was increased from 10 mmHg to 300 mmHg
  • the wall temperature of the reactor rose gradually as the pressure increased from 250 °C (the initial temperature above the molten sodium was 1 10 °C) to 284 °C and was maintained in that range during the remainder of the run by adjusting the feed-rate (hence the pressure) of CF 3 Br (see Table 2)
  • the decomposition product (a 257 g of free-flowing black powder, Found C. 5 0%, H, none detected, Br.
  • CFC-1 1 (18.3 g; b.p. 23.8 °C) was decomposed with molten sodium (12.2 g) at 265-280 °C (reactor wall temperature) over 15 minutes, during which time the reactor head-space pressure of the feedstock was increased gradually from 10 mmHg to 290 mmHg. determination of the alkalinity of the methanol used to wash the black solid product showed that >99% utilisation of the sodium had been achieved.
  • perfluoro-N-fluoropiperidine 13.9 g, b.p. 49.5 °C
  • molten sodium 12.4 g
  • the product was a fine free-flowing black powder and >99% utilisation of sodium was achieved.
  • the fine black powder was shown by combustion analysis to contain 1 1.1 % of carbon and 2.3% of nitrogen (calculated for 4 C + 1 1 NaF + NaCN: C, 10.7% and N. 2.5%).
  • perfluoropropane 13.62 g, b.p. -37°C was destroyed with molten sodium (13.4 g) at 390-400 ⁇ C (reactor wall temperature) during 15 minutes (the headspace pressure was increased from 1 to 450 mmHg during the course of the process).
  • the product was a free-flowing black powder.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Business, Economics & Management (AREA)
  • Toxicology (AREA)
  • Emergency Management (AREA)
  • General Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Ce procédé de destruction d'hydrocarbures halogénés comprend les étapes qui consistent (a) à introduire du sodium fondu pur dans une cuve à pression réduite, la quantité de sodium étant telle qu'il existe un espace libre au-dessus du sodium dans la cuve, (b) à introduire l'hydrocarbure halogéné gazeux ou vaporisé directement dans ledit espace libre tout en maintenant une pression réduite au sein de ladite cuve et (c) à remuer et à broyer le contenu de la cuve de manière à ce qu'il n'y ait pas de dépôt du produit de réaction solide sur les surfaces internes de la cuve, que l'encapsulation de sodium fondu par des produits de réaction solides ne puisse pas avoir lieu et que ledit produit de réaction soit un matériau particulaire.
PCT/GB1996/003130 1995-12-19 1996-12-18 Destruction d'hydrocarbures halogenes Ceased WO1997022386A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU11845/97A AU1184597A (en) 1995-12-19 1996-12-18 Destruction of halocarbons

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9525894.3 1995-12-19
GBGB9525894.3A GB9525894D0 (en) 1995-12-19 1995-12-19 Destruction of halocarbons

Publications (1)

Publication Number Publication Date
WO1997022386A1 true WO1997022386A1 (fr) 1997-06-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1996/003130 Ceased WO1997022386A1 (fr) 1995-12-19 1996-12-18 Destruction d'hydrocarbures halogenes

Country Status (3)

Country Link
AU (1) AU1184597A (fr)
GB (1) GB9525894D0 (fr)
WO (1) WO1997022386A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104857898A (zh) * 2015-05-21 2015-08-26 新疆美克化工股份有限公司 一种反应器

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2255096A1 (en) * 1973-12-19 1975-07-18 Gen Electric High speed rotary turbulence mixer with improved vanes - for blending and compounding thermoplastic granules and various additives
DE3334811A1 (de) * 1982-09-29 1984-03-29 CIBA-GEIGY AG, 4002 Basel Ruehrvorrichtung und ihre verwendung
US4465590A (en) * 1983-08-17 1984-08-14 American Mobile Oil Purification Co., Inc. Process for eliminating polychlorinated bi-phenyls from oils
WO1989000614A1 (fr) * 1987-07-09 1989-01-26 Dural Aluminum Composites Corporation Preparation de materiaux composites
DE4127873A1 (de) * 1991-08-22 1993-02-25 Reimelt Dietrich Kg Kneteinrichtung fuer eine zu knetende masse
WO1994003237A1 (fr) * 1992-08-06 1994-02-17 Ea Technology Limited Procede de destruction d'halocarbones
US5338115A (en) * 1992-12-11 1994-08-16 The United States Of America As Represented By The United States Department Of Energy Mixing device for materials with large density differences
GB2299080A (en) * 1995-03-24 1996-09-25 Ea Tech Ltd Process for the destruction of halocarbons

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2255096A1 (en) * 1973-12-19 1975-07-18 Gen Electric High speed rotary turbulence mixer with improved vanes - for blending and compounding thermoplastic granules and various additives
DE3334811A1 (de) * 1982-09-29 1984-03-29 CIBA-GEIGY AG, 4002 Basel Ruehrvorrichtung und ihre verwendung
US4465590A (en) * 1983-08-17 1984-08-14 American Mobile Oil Purification Co., Inc. Process for eliminating polychlorinated bi-phenyls from oils
WO1989000614A1 (fr) * 1987-07-09 1989-01-26 Dural Aluminum Composites Corporation Preparation de materiaux composites
DE4127873A1 (de) * 1991-08-22 1993-02-25 Reimelt Dietrich Kg Kneteinrichtung fuer eine zu knetende masse
WO1994003237A1 (fr) * 1992-08-06 1994-02-17 Ea Technology Limited Procede de destruction d'halocarbones
US5338115A (en) * 1992-12-11 1994-08-16 The United States Of America As Represented By The United States Department Of Energy Mixing device for materials with large density differences
GB2299080A (en) * 1995-03-24 1996-09-25 Ea Tech Ltd Process for the destruction of halocarbons

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104857898A (zh) * 2015-05-21 2015-08-26 新疆美克化工股份有限公司 一种反应器

Also Published As

Publication number Publication date
AU1184597A (en) 1997-07-14
GB9525894D0 (en) 1996-02-21

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