EP2930232B1 - Cleaning industrial plant components to remove metal halides - Google Patents

Cleaning industrial plant components to remove metal halides Download PDF

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Publication number
EP2930232B1
EP2930232B1 EP15162053.1A EP15162053A EP2930232B1 EP 2930232 B1 EP2930232 B1 EP 2930232B1 EP 15162053 A EP15162053 A EP 15162053A EP 2930232 B1 EP2930232 B1 EP 2930232B1
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Prior art keywords
method comprises
plant components
nitriles
metal halides
halides
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EP15162053.1A
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German (de)
French (fr)
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EP2930232A1 (en
Inventor
Javad MOHSSENI
Konrad Mautner
Peter Nürnberg
Christian Kaltenmarkner
Klaus Kaeppler
Andreas Bockholt
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Wacker Chemie AG
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Wacker Chemie AG
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50—Solvents
    • C11D7/5004—Organic solvents
    • C11D7/5013—Organic solvents containing nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
    • B08B9/027—Cleaning the internal surfaces; Removal of blockages
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50—Solvents
    • C11D7/5004—Organic solvents
    • C11D7/5009—Organic solvents containing phosphorus, sulfur or silicon, e.g. dimethylsulfoxide
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/20—Industrial or commercial equipment, e.g. reactors, tubes or engines

Definitions

  • the invention relates to a method for the purification of technical system parts of metal halides, organometallic halides and silanes with a nitrile.
  • Acetonitrile is described as a solvent for aluminum chloride [ Journal of inorganic and general chemistry. Weinheim: Wiley-VCH, ISSN 0372-7874 Vol. 511 (4, 1984), p. 148 ].
  • US3519458A teaches that fluxes containing inorganic chlorides can be removed from iron surfaces by blends of alkylamine and organic solvents such as butyl diglycol ether.
  • the invention relates to a process for the purification of technical plant parts of impurities selected from metal halides, organometallic halides and silanes and mixtures thereof, in which the plant parts are treated with a liquid nitrile or with a solution of a nitrile in an aprotic solvent.
  • the impurities in particular the metal halides form deposits in the system parts.
  • the impurities can easily be dissolved out of the technical components with nitriles.
  • the linings in the pipes are opened or dissolved and washed out. After cleaning the system parts, they are dried again and put into operation. The residues of the cleaning can be simply rinsed off and professionally e.g. be disposed of by incineration.
  • the impurities are in particular metal halides which are hydrolyzed with water to form acids and organometallic halides, in particular organometallic chlorides.
  • organometallic chlorides and chlorides of iron such as FeCl 2 , FeCl 3 , cobalt, nickel, chromium, titanium, copper, tin, zinc and preferably AlR x Cl 3-x , where R is an organo or organosilane function, in particular methyl and x Values 0, 1 or 2, in particular AlCl 3 .
  • the nitriles used are preferably the nitriles of monocarboxylic or polycarboxylic acids, which preferably contain 2 to 20 carbon atoms, in particular 5 to 12 carbon atoms.
  • nitriles of the aliphatic, saturated monocarboxylic acids such as acetic, propionic, butyric, valeric and caproic acids and the fatty acids having up to 18 carbon atoms.
  • dinitriles of aliphatic, saturated dicarboxylic acids such as malonic, succinic, glutaric, adipic, pimelinic and suberic.
  • Adipodinitrile is an important intermediate for the production of polyamides and therefore easily and inexpensively available.
  • solvents or solvent mixtures having a boiling point or boiling range of up to 120 ° C. at 1013 hPa.
  • solvents such as dioxane, tetrahydrofuran, diethyl ether, di-isopropyl ether, diethylene glycol dimethyl ether; chlorinated hydrocarbons, such as dichloromethane, trichloromethane, carbon tetrachloride, 1,2-dichloroethane, trichlorethylene; Hydrocarbons, such as pentane, n-hexane, hexane isomer mixtures, heptane, octane, benzine, petroleum ether, benzene, toluene, xylenes; Siloxanes, in particular linear dimethylpolysiloxanes having trimethylsilyl end groups with preferably 0 to 6 dimethyl
  • the concentration of the nitriles in the aprotic solvents is preferably at least 1 g / l, particularly preferably at least 5 g / l, in particular at least 10 g / l.
  • the process is preferably carried out at a temperature of 0 ° C to 100 ° C, especially from 15 ° C to 30 ° C.
  • the process is preferably carried out at a pressure of 500 hPa to 2000 hPa, in particular from 900 hPa to 1200 hPa.
  • plant parts are cleaned in which silanes, selected from methylchlorosilanes and chlorosilanes are processed. From these parts of the plant AlR x Cl 3-x , in particular AlCl 3 is removed with high-boiling organochlorosilanes.
  • Acetonitrile is less suitable for these plant components because acetonitrile has a boiling point of 82 ° C at 1013 hPa, and thus a noticeable vapor pressure at room temperature. High vapor pressure makes it difficult to use acetonitrile in pipeline cleaning since acetonitrile is flammable.
  • acetonitrile must not be introduced into silane mixtures of the distillation since the boiling point is very close to chlorosilanes or methylchlorosilanes and then itself would become contaminated.
  • Plant components are nitriles used alone or together with aprotic solvents having a boiling point of at least 120 ° C at 1013 hPa. Particularly preferred is adiponitrile.
  • plant components are pipelines, stirred tanks, tubular reactors, distillation columns and their internals and packings, thin-film evaporators, falling-film evaporators, short-path distillations including their internals such as, for example, Wipers in thin-film evaporators, but also heat exchangers and containers, such as tanks and pistons.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Detergent Compositions (AREA)

Description

Die Erfindung betrifft ein Verfahren zur Reinigung von technischen Anlagenteilen von Metallhalogeniden, Organometallhalogeniden und Silanen mit einem Nitril.The invention relates to a method for the purification of technical system parts of metal halides, organometallic halides and silanes with a nitrile.

Viele industrielle Rohprodukte und Mischungen, wie die Methylchlorsilane und Chlorsilane enthaltenden Mischungen aus der Direktsynthese (Müller-Rochow-Synthese) oder die Chlorsilanmischungen aus der Hydrochlorierung von metallurgischem Silizium können Metallhalogenide, Organometallhalogenide und Silane, insbesondere AlCl3 enthalten. Die Silane in den Rohsilanen werden mittels Destillation in mehreren Stufen in Reinsilane getrennt. Diese Verunreinigungen der Rohsilane setzen sich in den Rohrleitungen ab und führen zu Problemen bis hin zu Verstopfung der Leitungen. Daher müssen die Leitungen in regelmäßigen Zeitabständen demontiert und z.B. mit Wasser gereinigt werden. Die genannte Reinigungsmethode hat zwei Nachteile: Erster Nachteil ist der Aufwand. Demontage-Reinigung-Montage von Leitungen nimmt viel Zeit in Anspruch und ist kostenintensiv. Zweiter Nachteil der Reinigung mit Wasser, ist die Bildung von Salzsäure durch Hydrolyse von Chlorsilanresten und Metallchloriden und/oder Organometallhalogeniden und/oder Mischungen aus Metallhalogeniden/Organometallhalogeniden, welche die Rohrleitungen angreift.Many industrial raw products and mixtures, such as the methylchlorosilane and chlorosilane-containing mixtures of the direct synthesis (Müller-Rochow synthesis) or the chlorosilane mixtures from the hydrochlorination of metallurgical silicon may contain metal halides, organometallic halides and silanes, in particular AlCl 3 . The silanes in the crude silanes are separated by distillation in several stages in pure silanes. These impurities of the raw silanes settle in the pipelines and lead to problems up to clogging of the pipes. Therefore, the pipes must be dismantled at regular intervals and, for example, cleaned with water. The mentioned cleaning method has two disadvantages: First disadvantage is the effort. Disassembly-cleaning-installation of pipes takes a lot of time and is costly. The second disadvantage of water purification is the formation of hydrochloric acid by hydrolysis of chlorosilane radicals and metal chlorides and / or organometallic halides and / or mixtures of metal halides / organometallic halides which attack the pipelines.

Acetonitril wird als Lösungsmittel für Aluminiumchlorid beschrieben [ Zeitschrift für anorganische und allgemeine Chemie. Weinheim : Wiley-VCH, ISSN 0372-7874 Vol. 511 (4. 1984), S. 148 ].Acetonitrile is described as a solvent for aluminum chloride [ Journal of inorganic and general chemistry. Weinheim: Wiley-VCH, ISSN 0372-7874 Vol. 511 (4, 1984), p. 148 ].

US4221674A beschreibt den Einsatz von organischen Nitrilen im Gemisch mit organischem Lösungsmittel bei der Reinigung metallischer Oberflächen zur Entfernung polymerer organischer Verbindungen US4221674A describes the use of organic nitriles mixed with organic solvent in the cleaning of metallic surfaces to remove polymeric organic compounds

US3519458A lehrt, dass Flussmittel, die anorganische Chloride enthalten, von Eisenoberflächen entfernt werden können durch Gemische aus Alkylamin und organischem Lösungsmittel, wie Butyldiglykolether. US3519458A teaches that fluxes containing inorganic chlorides can be removed from iron surfaces by blends of alkylamine and organic solvents such as butyl diglycol ether.

Gegenstand der Erfindung ist ein Verfahren zur Reinigung von technischen Anlagenteilen von Verunreinigungen, die ausgewählt werden aus Metallhalogeniden, Organometallhalogeniden und Silanen und Mischungen davon, bei dem die Anlagenteile mit einem flüssigen Nitril oder mit einer Lösung eines Nitrils in einem aprotischen Lösungsmittel behandelt werden.The invention relates to a process for the purification of technical plant parts of impurities selected from metal halides, organometallic halides and silanes and mixtures thereof, in which the plant parts are treated with a liquid nitrile or with a solution of a nitrile in an aprotic solvent.

Die Verunreinigungen, insbesondere die Metallhalogenide bilden Beläge in den Anlagenteilen. Die Verunreinigungen lassen sich mit Nitrilen leicht aus den technischen Anlagenteilen herauslösen. Die Beläge in den Leitungen werden an- oder aufgelöst und ausgewaschen. Nach der Reinigung der Anlagenteile werden diese wieder getrocknet und in Betrieb genommen. Die Rückstände der Reinigung können einfach ausgespült und fachgerecht z.B. durch Verbrennung entsorgt werden.The impurities, in particular the metal halides form deposits in the system parts. The impurities can easily be dissolved out of the technical components with nitriles. The linings in the pipes are opened or dissolved and washed out. After cleaning the system parts, they are dried again and put into operation. The residues of the cleaning can be simply rinsed off and professionally e.g. be disposed of by incineration.

Durch Reinigung von Anlagenteilen mit Nitrilen werden die zeit- und kostenintensive Demontage und Reinigung mit Wasser eingespart. Da die Leitungen nicht mehr mit saurem Wasser in Kontakt kommen, wird die Lebensdauer der Anlagenteile verlängert.By cleaning parts of the system with nitriles, time- and cost-intensive dismantling and cleaning with water are saved. As the pipes no longer come into contact with acidic water, the service life of the system components is extended.

Die Verunreinigungen sind insbesondere mit Wasser zu Säuren hydrolysierende Metallhalogenide und Organometallhalogenide, insbesondere Organometallchloride. Beispiele sind Organometallchloride und Chloride von Eisen, wie FeCl2, FeCl3, Kobalt, Nickel, Chrom, Titan, Kupfer, Zinn, Zink und bevorzugt AlRxCl3-x, wobei R eine Organo- oder Organosilanfunktion, insbesondere Methyl und x die Werte 0, 1 oder 2 bedeuten, insbesondere AlCl3.The impurities are in particular metal halides which are hydrolyzed with water to form acids and organometallic halides, in particular organometallic chlorides. Examples are organometallic chlorides and chlorides of iron, such as FeCl 2 , FeCl 3 , cobalt, nickel, chromium, titanium, copper, tin, zinc and preferably AlR x Cl 3-x , where R is an organo or organosilane function, in particular methyl and x Values 0, 1 or 2, in particular AlCl 3 .

Als Nitrile werden vorzugsweise eingesetzt die Nitrile von Mono- oder Polycarbonsäuren, die vorzugsweise 2 bis 20 Kohlenstoffatome, insbesondere 5 bis 12 Kohlenstoffatome enthalten.The nitriles used are preferably the nitriles of monocarboxylic or polycarboxylic acids, which preferably contain 2 to 20 carbon atoms, in particular 5 to 12 carbon atoms.

Bevorzugt sind die Nitrile der aliphatischen, gesättigten Monocarbonsäuren, wie Essig-, Propion-, Butter-, Valerian- und Capronsäure und der Fettsäuren mit bis zu 18 Kohlenstoffatomen.Preference is given to the nitriles of the aliphatic, saturated monocarboxylic acids, such as acetic, propionic, butyric, valeric and caproic acids and the fatty acids having up to 18 carbon atoms.

Bevorzugt sind auch die Dinitrile der aliphatischen, gesättigten Dicarbonsäuren, wie Malon-, Bernstein-, Glutar-, Adipin-, Pimelin- und Suberinsäure.Also preferred are the dinitriles of aliphatic, saturated dicarboxylic acids, such as malonic, succinic, glutaric, adipic, pimelinic and suberic.

Bevorzugt sind Nitrile mit einem Siedepunkt von mindestens 120°C bei 1013 hPa, insbesondere mindestens 150°C bei 1013 hPa.Preference is given to nitriles having a boiling point of at least 120 ° C. at 1013 hPa, in particular at least 150 ° C. at 1013 hPa.

Insbesondere bevorzugt ist Adipodinitril, welches bei 295°C bei 1013 hPa siedet und aufgrund seiner zwei Nitrilgruppen im Molekül eine starke komplexierende Wirkung auf Metallionen aufweist. Adipodinitril ist ein wichtiges Intermediate zur Herstellung von Polyamiden und daher leicht und kostengünstig verfügbar.Particularly preferred is adiponitrile, which boils at 295 ° C at 1013 hPa and has a strong complexing effect on metal ions due to its two nitrile groups in the molecule. Adipodinitrile is an important intermediate for the production of polyamides and therefore easily and inexpensively available.

Falls Lösungen von Nitrilen in aprotischen Lösungsmitteln verwendet werden, sind Lösungsmittel oder Lösungsmittelgemische mit einem Siedepunkt bzw. Siedebereich von bis zu 120°C bei 1013 hPa bevorzugt. Beispiele für solche Lösungsmittel sind Ether, wie Dioxan, Tetrahydrofuran, Diethylether, Di-isopropylether, Diethylenglycoldimethylether; chlorierte Kohlenwasserstoffe, wie Dichlormethan, Trichlormethan, Tetrachlormethan, 1,2-Dichlorethan, Trichlorethylen; Kohlenwasserstoffe, wie Pentan, n-Hexan, Hexan-Isomerengemische, Heptan, Oktan, Waschbenzin, Petrolether, Benzol, Toluol, Xylole; Siloxane, insbesondere lineare Dimethylpolysiloxane mit Trimethylsilylendgruppen mit bevorzugt 0 bis 6 Dimethylsiloxaneinheiten, oder cyclische Dimethylpolysiloxane mit bevorzugt 4 bis 7 Dimethylsiloxaneinheiten, beispielsweise Hexamethyldisiloxan, Octamethyltrisiloxan, Octamethylcyclotetrasiloxan und Decamethylcyclopentasiloxan;
Ketone, wie Aceton, Methylethylketon, Di-isopropylketon, Methyl-isobutylketon (MIBK); Ester, wie Ethylacetat, Butylacetat, Propylpropionat, Ethylbutyrat, Ethyl-isobutyrat; Schwefelkohlenstoff und Nitrobenzol, oder Gemische dieser Lösungsmittel.If solutions of nitriles in aprotic solvents are used, preference is given to solvents or solvent mixtures having a boiling point or boiling range of up to 120 ° C. at 1013 hPa. Examples of such solvents are ethers, such as dioxane, tetrahydrofuran, diethyl ether, di-isopropyl ether, diethylene glycol dimethyl ether; chlorinated hydrocarbons, such as dichloromethane, trichloromethane, carbon tetrachloride, 1,2-dichloroethane, trichlorethylene; Hydrocarbons, such as pentane, n-hexane, hexane isomer mixtures, heptane, octane, benzine, petroleum ether, benzene, toluene, xylenes; Siloxanes, in particular linear dimethylpolysiloxanes having trimethylsilyl end groups with preferably 0 to 6 dimethylsiloxane units, or cyclic Dimethylpolysiloxanes having preferably 4 to 7 dimethylsiloxane units, for example, hexamethyldisiloxane, octamethyltrisiloxane, octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane;
Ketones such as acetone, methyl ethyl ketone, diisopropyl ketone, methyl isobutyl ketone (MIBK); Esters such as ethyl acetate, butyl acetate, propyl propionate, ethyl butyrate, ethyl isobutyrate; Carbon disulfide and nitrobenzene, or mixtures of these solvents.

Die Konzentration der Nitrile in den aprotischen Lösungsmitteln beträgt vorzugsweise mindestens 1 g/l, besonders bevorzugt mindestens 5 g/l, insbesondere mindestens 10 g/l.The concentration of the nitriles in the aprotic solvents is preferably at least 1 g / l, particularly preferably at least 5 g / l, in particular at least 10 g / l.

Das Verfahren wird vorzugsweise bei einer Temperatur von 0°C bis 100°C, insbesondere von 15°C bis 30°C durchgeführt.The process is preferably carried out at a temperature of 0 ° C to 100 ° C, especially from 15 ° C to 30 ° C.

Das Verfahren wird vorzugsweise bei einem Druck von 500 hPa bis 2000 hPa, insbesondere von 900 hPa bis 1200 hPa durchgeführt.The process is preferably carried out at a pressure of 500 hPa to 2000 hPa, in particular from 900 hPa to 1200 hPa.

In einer besonderen Ausführungsform werden Anlagenteile gereinigt, in welchen Silane, ausgewählt aus Methylchlorsilanen und Chlorsilanen verarbeitet werden. Aus diesen Anlagenteilen wird AlRxCl3-x, insbesondere AlCl3 mit hochsiedenden Organochlorosilanen entfernt. Für diese Anlagenteile ist Acetonitril weniger geeignet, denn Acetonitril hat einen Siedepunkt von 82°C bei 1013 hPa, und damit einen merklichen Dampfdruck bei Raumtemperatur. Hoher Dampfdruck erschwert die Verwendung von Acetonitril in der Reinigung von Rohrleitungen, da Acetonitril brennbar ist. Acetonitril darf auch nicht in Silangemische der Destillation eingeschleppt werden, da der Siedepunkt sehr nah bei Chlorsilanen oder Methylchlorsilanen liegt und dann selbst zur Verunreinigung würde. Für diese Anlagenteile werden Nitrile alleine oder zusammen mit aprotischen Lösungsmitteln mit einem Siedepunkt von mindestens 120°C bei 1013 hPa eingesetzt. Insbesondere bevorzugt ist Adipodinitril.In a particular embodiment, plant parts are cleaned in which silanes, selected from methylchlorosilanes and chlorosilanes are processed. From these parts of the plant AlR x Cl 3-x , in particular AlCl 3 is removed with high-boiling organochlorosilanes. Acetonitrile is less suitable for these plant components because acetonitrile has a boiling point of 82 ° C at 1013 hPa, and thus a noticeable vapor pressure at room temperature. High vapor pressure makes it difficult to use acetonitrile in pipeline cleaning since acetonitrile is flammable. Also, acetonitrile must not be introduced into silane mixtures of the distillation since the boiling point is very close to chlorosilanes or methylchlorosilanes and then itself would become contaminated. For this Plant components are nitriles used alone or together with aprotic solvents having a boiling point of at least 120 ° C at 1013 hPa. Particularly preferred is adiponitrile.

Beispiele für Anlagenteile sind Rohrleitungen, Rührkessel, Rohrreaktoren, Destillationskolonnen und deren Einbauten und Packungen, Dünnschichtverdampfer, Fallfilmverdampfer, Kurzwegdestillationen inklusive deren Einbauten wie z.B. Wischer in Dünnschichtverdampfern, aber auch Wärmetauscher und Behälter, wie Tanks und Kolben.Examples of plant components are pipelines, stirred tanks, tubular reactors, distillation columns and their internals and packings, thin-film evaporators, falling-film evaporators, short-path distillations including their internals such as, for example, Wipers in thin-film evaporators, but also heat exchangers and containers, such as tanks and pistons.

Claims (7)

  1. Method of cleaning industrial plant components to remove contaminants selected from silanes, metal halides, organometallic halides and mixtures thereof wherein said method comprises treating the plant components with a liquid nitrile or with a solution of a nitrile in an aprotic solvent.
  2. Method according to Claim 1 wherein the metal halides and organometallic halides are selected from chlorides and organometallic chlorides of iron, cobalt, nickel, chromium, titanium, copper, tin, zinc and aluminum.
  3. Method according to one or more of the preceding claims wherein said method comprises employing nitriles of mono- or polycarboxylic acids comprising from 2 to 20 carbon atoms.
  4. Method according to one or more of the preceding claims wherein said method comprises employing a solution of nitriles in an aprotic solvent selected from ethers, chlorinated hydrocarbons, hydrocarbons, siloxanes, ketones, esters, carbon disulfide and nitrobenzene and mixtures thereof.
  5. Method according to one or more of the preceding claims wherein said method comprises cleaning plant components in which silanes selected from chlorosilanes and methylchlorosilanes are processed wherein said method comprises removing AlCl3 and employing nitriles and optionally aprotic solvents having a boiling point of at least 120°C at 1013 hPa.
  6. Method according to one or more of the preceding claims wherein said method comprises employing adiponitrile.
  7. Method according to one or more of the preceding claims wherein the plant components are selected from pipes, stirred tanks, tubular reactors, distillation columns and internals and packings thereof, thin film evaporators, falling film evaporators, short path distillation apparatuses including internals thereof, heat exchangers and vessels.
EP15162053.1A 2014-04-09 2015-03-31 Cleaning industrial plant components to remove metal halides Active EP2930232B1 (en)

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DE102016206090A1 (en) * 2016-04-12 2017-10-12 Wacker Chemie Ag Process for the separation of aluminum chloride from silanes
JP7389977B2 (en) 2018-03-29 2023-12-01 国立研究開発法人宇宙航空研究開発機構 power control system

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DE102014206875A1 (en) 2015-10-15
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CN104971918B (en) 2018-03-13
CN104971918A (en) 2015-10-14
KR20150117207A (en) 2015-10-19
US9994802B2 (en) 2018-06-12
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EP2930232A1 (en) 2015-10-14
US20150291920A1 (en) 2015-10-15

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