WO2004103513A1 - Method for the in situ distillation of volatile organic compounds (voc) by means of water vapour injection and hot nitrogen stripping, comprising treatment of the emission gases by condensation and cryocondensation - Google Patents

Method for the in situ distillation of volatile organic compounds (voc) by means of water vapour injection and hot nitrogen stripping, comprising treatment of the emission gases by condensation and cryocondensation Download PDF

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Publication number
WO2004103513A1
WO2004103513A1 PCT/ES2004/000095 ES2004000095W WO2004103513A1 WO 2004103513 A1 WO2004103513 A1 WO 2004103513A1 ES 2004000095 W ES2004000095 W ES 2004000095W WO 2004103513 A1 WO2004103513 A1 WO 2004103513A1
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treatment
vocs
distillation
stripper
condensation
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PCT/ES2004/000095
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Spanish (es)
French (fr)
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Evaristo Fontecha Cuetos
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Evaristo Fontecha Cuetos
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38—Steam distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/343—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances the substance being a gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation

Definitions

  • the present invention describes a distillation process that has the following applications:
  • VOCs Water and sludge treatment contaminated by VOCs. Recycling of solvents and other contaminated VOCs. Treatment of containers with substances contaminated by VOCs. The procedure includes operations concerning Safety and Environment (inertization of vessels and circuits with nitrogen, emission control by cryoprespiration, recovery and confinement of the VOCs contaminants, etc.), which make it especially suitable for treating those VOCs that have a high Explosive risk or potentially causing irreversible effects on people and the environment.
  • Safety and Environment inertization of vessels and circuits with nitrogen, emission control by cryoprespiration, recovery and confinement of the VOCs contaminants, etc.
  • VOCs not admitted to incinerator plants (high concentration in halogens, sulfur, etc.) and also not admitted to distillation plants (self-ignition temperatures in vacuum pumps, cryogenic condensation temperatures, etc.).
  • An example of VOC with these characteristics is carbon sulfide.
  • the method of the patent allows recycling contaminated carbon sulfide and also enables the distillation of water and sludge contaminated with carbon disulphide, in all cases a completely secure and recovering a carbon disulfide total purity.
  • the process object of this patent of invention for precise application of the following elements: a vessel or stripper treatment; a heating source with its electronic regulation unit; a condenser with cooling system; one criocondensador VOC with liquid nitrogen tank; and a collector with nitrogen heater.
  • the treatment vessel or stripper must have the following components: water vapor diffusers and nitrogen; a temperature probe; a stirrer; a safety valve; and various tubing for the emission gas, water vapor, nitrogen and drainage lines of the stripper.
  • the process object of the present invention patent comprises the following operations:
  • the distillation temperature is determined by the boiling point of VOCs and the cooling capacity of the condensing system.
  • the installed cooling capacity must be sufficient to counteract the specific and latent heats of the gas stream generated in the stripper (nitrogen, water vapor and VOCs).
  • the nitrogen flow rate of stripping is to be limited, since the condensable be, is cooled to cryogenic temperatures as it passes through the criocondensador and consumes some of the cooling capacity installed.
  • the treatment vessel or stripper -1- has water vapor diffusers -2- a nitrogen diffuser network -3- an agitator -4- and a temperature probe -5-.
  • the temperature probe sends the signal to an electronic unit -6- that regulates the steam provided by the steam source -7-.
  • the emission gases -8- are conducted to a condenser -9- connected to a glycol water cooler -10-.
  • the non-condensed gases pass to a VOC cryo-condenser -11- fed by a source of liquid nitrogen -12-.
  • the temperature parameters are entered in the cryo condenser control panel -13- depending on the emission limits of VOCs in the treated gases -14-.
  • the gas nitrogen line at its outlet of the cryoprestrainer -15- is connected to a collector with a nitrogen heater -16- for reuse of nitrogen as a source of stripping -17-.
  • a representative case of application of the procedure is presented in the treatment of water and sludge contaminated by solvent.
  • the solvents to be distilled must have a boiling point or azeotropic point with water below 100 ° C and a melting temperature below -20 ° C.
  • the cryo condenser has a "defrosting" heating system that is used to remove the ice plugs, so sometimes the condenser and its glycol water cooler can be dispensed with.
  • cryocondenser outlet nitrogen in a collector for heating and subsequent injection into the stripper.
  • the manifold has a valve which allows release to the atmosphere or other facility nitrogen not demanded by the stripper.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention relates to a method for the in situ distillation of volatile organic compounds (VOCs) by means of water vapour injection and hot nitrogen stripping, comprising treatment of the emission gases by condensation and cryocondensation. The inventive method comprises the following operations consisting in: loading the treatment tank or stripper; programming the distillation and cryocondensation temperatures; injecting water vapour and stripping with hot nitrogen; conveying the emission gases from the stripper to the condensation system; controlling the emissions, and recovering the pollutant VOCs by means of condensation and cryocondensation. According to the invention, the distillation process is terminated upon verification of the absence of VOCs in the condensates from the cryocondenser. The invention can be used for: treatment of VOC-contaminated water and sludge, recycling of solvents and other contaminated VOCs, and treatment of containers housing VOC-contaminated substances.

Description

DESCRIPCIÓN Procedimiento de destilación "in situ" de compuestos orgánicos volátiles (COV's) mediante inyección de vapor de agua y stripping con nitrógeno caliente, con tratamiento de los gases de emisión por condensación y criocondensación.DESCRIPTION Procedure of distillation "in situ" of volatile organic compounds (VOC ' s) by injection of water vapor and stripping with hot nitrogen, with treatment of the emission gases by condensation and cryocondensation.
OBJETO DE LA INVENCIÓNOBJECT OF THE INVENTION
La presente invención describe un procedimiento de destilación que presenta las aplicaciones siguientes:The present invention describes a distillation process that has the following applications:
Tratamiento de aguas y lodos contaminados por COV's. Reciclado de disolventes y otros COV's contaminados. Tratamiento de recipientes con sustancias contaminadas por COV's. El procedimiento comprende operaciones concernientes a Seguridad y Medio Ambiente (inertización de recipientes y circuitos con nitrógeno, control de emisiones por criocondensación, recuperación y confinamiento de los COV's contaminantes, etc.), que lo hacen especialmente apto para tratar aquellos COV's que presenten un alto riesgo de explosividad o que sean potencialmente causantes de efectos irreversibles en las personas y el medio ambiente.Water and sludge treatment contaminated by VOCs. Recycling of solvents and other contaminated VOCs. Treatment of containers with substances contaminated by VOCs. The procedure includes operations concerning Safety and Environment (inertization of vessels and circuits with nitrogen, emission control by cryoprespiration, recovery and confinement of the VOCs contaminants, etc.), which make it especially suitable for treating those VOCs that have a high Explosive risk or potentially causing irreversible effects on people and the environment.
Una ventaja inherente a este procedimiento de destilación "in situ", reside en que los COV's contaminantes son recuperados como materia prima y no han de ser gestionados como residuos peligrosos.An inherent advantage of this "in situ" distillation procedure is that the contaminant VOCs are recovered as raw material and should not be managed as hazardous waste.
ESTADO DE LA TÉCNICASTATE OF THE TECHNIQUE
La alternativa al presente procedimiento para el tratamiento de sustancias con contenido en COV's, se encuentra en las plantas de incineración y en las plantas de destilación. Las plantas de tratamiento biológico y los procedimientos de estabilización, no son factibles para el tratamiento de sustancias que contengan cantidades apreciables de COV's.The alternative to the present procedure for the treatment of substances with VOC content is found in the incineration plants and in the plants of distillation. Biological treatment plants and stabilization procedures are not feasible for the treatment of substances that contain appreciable amounts of VOCs.
Una aportación fundamental del procedimiento resulta de su aplicación a COV's no admitidos en plantas incineradoras (alta concentración en halógenos, azufre, etc.) y tampoco admitidos en plantas de destilación (temperaturas de autoignición en bombas de vacío, temperaturas criogénicas de condensación, etc.). Un ejemplo de COV con dichas características es el sulfuro de carbono.A fundamental contribution of the procedure results from its application to VOCs not admitted to incinerator plants (high concentration in halogens, sulfur, etc.) and also not admitted to distillation plants (self-ignition temperatures in vacuum pumps, cryogenic condensation temperatures, etc.). ). An example of VOC with these characteristics is carbon sulfide.
El procedimiento objeto de la patente permite reciclar sulfuro de carbono contaminado e igualmente permite la destilación de aguas y lodos contaminados de sulfuro de carbono, en todos los casos de forma totalmente segura y con recuperación de un sulfuro de carbono de total pureza.The method of the patent allows recycling contaminated carbon sulfide and also enables the distillation of water and sludge contaminated with carbon disulphide, in all cases a completely secure and recovering a carbon disulfide total purity.
DESCRIPCIÓN DE LA INVENCIÓNDESCRIPTION OF THE INVENTION
El procedimiento objeto de esta patente de invención precisa para su aplicación de los elementos siguientes: una vasija de tratamiento o stripper; una fuente de calentamiento con su unidad electrónica de regulación; un condensador con su sistema de refrigeración; un criocondensador de COV's con su tanque de nitrógeno líquido; y un colector con calentador de nitrógeno.The process object of this patent of invention for precise application of the following elements: a vessel or stripper treatment; a heating source with its electronic regulation unit; a condenser with cooling system; one criocondensador VOC with liquid nitrogen tank; and a collector with nitrogen heater.
La vasija de tratamiento o stripper ha de disponer de los siguientes componentes: difusores de vapor de agua y nitrógeno; una sonda de temperatura; un agitador; una válvula de seguridad; y tubuladuras diversas para las líneas de gases de emisión, vapor de agua, nitrógeno y drenaje del stripper. El procedimiento objeto de la presente patente de invención comprende las operaciones siguientes:The treatment vessel or stripper must have the following components: water vapor diffusers and nitrogen; a temperature probe; a stirrer; a safety valve; and various tubing for the emission gas, water vapor, nitrogen and drainage lines of the stripper. The process object of the present invention patent comprises the following operations:
Llenado de la vasija de tratamiento o stripper con la carga de COV's a destilar.Filling the treatment vessel or stripper with the load of VOCs to be distilled.
Programación de la temperatura de destilación en la unidad electrónica de regulación de vapor. La temperatura de destilación vendrá determinada por la temperatura de ebullición de los COV's y la potencia frigorífica del sistema de condensación. La potencia frigorífica instalada ha de ser suficiente para contrarrestar los calores específicos y latentes de la corriente de gases generados en el stripper (nitrógeno, vapor de agua y COV's).Programming of the distillation temperature in the electronic steam control unit. The distillation temperature is determined by the boiling point of VOCs and the cooling capacity of the condensing system. The installed cooling capacity must be sufficient to counteract the specific and latent heats of the gas stream generated in the stripper (nitrogen, water vapor and VOCs).
Programación en el panel de control del criocondensador de los parámetros de temperatura del circuito de criocondensación, en función de la temperatura de fusión y límites de emisión de los COV's.Programming in the cryo condenser control panel of the cryocondensation circuit temperature parameters, depending on the melting temperature and emission limits of the VOCs.
Inyección de vapor, stripping con nitrógeno caliente y agitación de la carga en el stripper. El caudal de nitrógeno de stripping ha de estar limitado, ya que al ser incondensable, es enfriado a temperaturas criogénicas a su paso por el criocondensador y consume parte de la potencia frigorífica instalada.Steam injection, stripping with hot nitrogen and stirring the load on the stripper. The nitrogen flow rate of stripping is to be limited, since the condensable be, is cooled to cryogenic temperatures as it passes through the criocondensador and consumes some of the cooling capacity installed.
Conducción de los gases de emisión del stripper al condensador, con condensación de vapor de agua y en menor medida de COV's.Conduction emission gases to the stripper condenser, condensing water vapor and less VOC.
Conducción de los gases no condensados al criocondensador, con condensación de los COV's contaminantes.Conduction of non-condensed gases to the cryopredenser, with condensation of the polluting VOCs.
Disposición en un colector del nitrógeno gasificado en el criocondensador para su calentamiento y posterior inyección al stripper. Finaliza la destilación cuando se verifique la ausencia de disolvente en los condensados del criocondensador. En la fase final de destilación, al producirse una menor vaporización de COV's y por tanto demanda de potencia frigorífica, se puede incrementar la temperatura de destilación. El stripping con nitrógeno caliente aporta cualidades al procedimiento en los aspectos siguientes:Arrangement in a collector of the gasified nitrogen in the cryo condenser for heating and subsequent injection into the stripper. Ends distillation when the absence of solvent in the criocondensador condensates is verified. In the final phase of distillation, when there is a lower vaporization of VOCs and therefore demand for cooling power, the distillation temperature can be increased. The hot stripping with nitrogen adds to the qualities the following procedure:
1. Reduce la temperatura de ebullición de los COV's. De acuerdo con la Ley de Dalton la tensión total del vapor será la suma de las tensiones parciales, por lo que los COV's se comportan como en una destilación a presión reducida.1. Reduce the boiling temperature of VOCs. According to Dalton's Law, the total vapor tension will be the sum of the partial tensions, so the VOCs behave as in a distillation under reduced pressure.
2. Inertiza la corriente de gases, evitando así la formación de atmósferas inflamables o explosivas.2. Inertizes the gas stream, thus preventing the formation of flammable or explosive atmospheres.
3. Actúa como agente portador de los COV's desde la vasija de tratamiento hasta el criocondensador, haciendo innecesario el uso de extractores.3. Acts as carrier agent VOCs from the treatment vessel to criocondensador, making it unnecessary to use extractors.
4. Actúa como coadyuvante o incluso como sustituto del agitador de la carga durante la destilación.4. It acts as an adjuvant or even as a substitute for the agitator of the load during distillation.
5. Actúa como fuente localizada de calor mejorando la eficiencia del stripping.5. It acts as a localized source of heat improving stripping efficiency.
DESCRIPCIÓN DE LA FIGURA ADJUNTADESCRIPTION OF THE ATTACHED FIGURE
Para facilitar la explicación se acompaña la descripción de una figura en la que se representa, a título de ejemplo ilustrativo y no limitativo, la disposición del equipamiento para un ejemplo de tratamiento de una carga con COV's contaminantes.To facilitate the explanation, the description of a figure is included in which, by way of illustrative and non-limiting example, the arrangement of the equipment for an example of treatment of a load with contaminating VOCs is represented.
Los elementos designados con números en la Ωgura 1 corresponden a las partes que se indican a continuación: La vasija de tratamiento o stripper -1- dispone de difusores de vapor de agua -2- una red difusora de nitrógeno -3- un agitador -4- y una sonda de temperatura -5-. La sonda de temperatura envía la señal a una unidad electrónica -6- que regula el vapor aportado por la fuente de vapor -7-. Los gases de emisión -8- son conducidos a un condensador -9- conectado a un refrigerador de agua glicolada -10-. Los gases no condensados pasan a un criocondensador de COV's -11- alimentado por una fuente de nitrógeno líquido -12-. Se introducen los parámetros de temperatura en el panel de control del criocondensador -13- en función de los límites de emisión de COV's en los gases tratados -14-. La línea de nitrógeno gas a su salida del criocondensador -15- va conectada a un colector con calentador de nitrógeno -16- para reutilización del nitrógeno como fuente de stripping -17-.The elements designated with numbers in the Ωgura 1 correspond to the parts indicated below: The treatment vessel or stripper -1- has water vapor diffusers -2- a nitrogen diffuser network -3- an agitator -4- and a temperature probe -5-. The temperature probe sends the signal to an electronic unit -6- that regulates the steam provided by the steam source -7-. The emission gases -8- are conducted to a condenser -9- connected to a glycol water cooler -10-. The non-condensed gases pass to a VOC cryo-condenser -11- fed by a source of liquid nitrogen -12-. The temperature parameters are entered in the cryo condenser control panel -13- depending on the emission limits of VOCs in the treated gases -14-. The gas nitrogen line at its outlet of the cryoprestrainer -15- is connected to a collector with a nitrogen heater -16- for reuse of nitrogen as a source of stripping -17-.
MODO PREFERENTE DE REALIZACIÓN DE LA INVENCIÓNPREFERRED MODE OF EMBODIMENT OF THE INVENTION
Un caso representativo de aplicación del procedimiento se presenta en el tratamiento de aguas y lodos contaminados por disolvente. Los disolventes a destilar han de tener una temperatura de ebullición o punto azeotrópico con el agua inferior a 100 °C y una temperatura de fusión inferior a -20°C.A representative case of application of the procedure is presented in the treatment of water and sludge contaminated by solvent. The solvents to be distilled must have a boiling point or azeotropic point with water below 100 ° C and a melting temperature below -20 ° C.
A la vista de la figura 1 y de acuerdo con la descripción del procedimiento, laIn view of Figure 1 and according to the description of the procedure, the
secuencia operacional es la siguiente:Operational sequence is as follows:
Instalación de equipos y carga del stripper con las aguas y lodos contaminados de disolvente.Equipment installation and loading of the stripper with contaminated water and sludge of solvent.
Programación de la temperatura de destilación en la unidad electrónica de regulación de vapor, en concordancia con la potencia frigorífica disponible. Programación en el panel de control del criocondensador de los parámetros de temperatura del circuito de criocondensación, en función de la temperatura de fusión y límites de emisión del disolvente. Inyección de vapor, stripping con nitrógeno caliente y agitación de la carga en el stripper. La inyección de vapor puede ser sustituida por otro sistema de calentamiento (resistencias eléctricas, intercambiadores de calor, etc.). Conducción de los gases de emisión del stripper al condensador, con condensación de vapor de agua y en menor medida de vapor de disolvente. El condensador, conectado a un refrigerador de agua glicolada, previene la formación de tapones de hielo en el criocondensador y permite reducir el consumo de nitrógeno líquido.Programming of the distillation temperature in the electronic steam regulation unit, in accordance with the available cooling capacity. Programming of the cryocondenser circuit temperature parameters in the control panel, depending on the melting temperature and solvent emission limits. Steam injection, hot stripping with nitrogen and stirring the load on the stripper. The steam injection can be replaced by another heating system (electrical resistors, heat exchangers, etc.). Conduction of the emission gases from the stripper to the condenser, with condensation of water vapor and to a lesser extent of solvent vapor. The condenser, connected to a glycol water cooler, prevents the formation of ice plugs in the cryo condenser and reduces the consumption of liquid nitrogen.
Conducción de los gases no condensados al criocondensador, con condensación del vapor de disolvente. El criocondensador dispone de un sistema de calentamiento "defrosting" que sirve para eliminar los tapones de hielo, por lo que en ocasiones se puede prescindir del condensador y su refrigerador de agua glicolada.Driving uncondensed gases to the criocondensador, with condensation of the solvent vapor. The cryo condenser has a "defrosting" heating system that is used to remove the ice plugs, so sometimes the condenser and its glycol water cooler can be dispensed with.
Disposición del nitrógeno de salida del criocondensador en un colector para su calentamiento y posterior inyección al stripper. El colector dispone de una válvula de descarga, que permite liberar a la atmósfera u otra instalación el nitrógeno no demandado por el stripper.Disposition of the cryocondenser outlet nitrogen in a collector for heating and subsequent injection into the stripper. The manifold has a valve which allows release to the atmosphere or other facility nitrogen not demanded by the stripper.
Finaliza la destilación cuando se verifique la ausencia de disolvente en los condensados del criocondensador. En la fase final de destilación, al producirse una menor vaporización de disolvente y por tanto demanda de potencia frigorífica, se puede incrementar la temperatura de destilación. The distillation ends when the absence of solvent in the condensates of the cryo condenser is verified. In the final distillation stage, to the vaporization occur less solvent and therefore demand for cooling capacity, it can increase the distillation temperature.

Claims

REIVINDICACIONES
1.- Procedimiento de destilación "in situ" de compuestos orgánicos volátiles (COV's) mediante inyección de vapor de agua y stripping con nitrógeno caliente, con tratamiento de los gases de emisión por condensación y criocondensación, caracterizado por comprender las operaciones siguientes:1.- Procedure of distillation "in situ" of volatile organic compounds (VOC ' s) by injection of water vapor and stripping with hot nitrogen, with treatment of the emission gases by condensation and cryocondensation, characterized by comprising the following operations:
Carga de la vasija de tratamiento o stripper con los COV's a destilar;Loading of the treatment vessel or stripper with the VOCs to be distilled;
Programación de la temperatura de destilación en la unidad electrónica de regulación de vapor de agua;Programming of the distillation temperature in the electronic water vapor control unit;
Programación en el panel de control del criocondensador de los parámetros de temperatura del circuito de criocondensación;Programming of the cryo condenser circuit temperature parameters in the control panel;
Inyección de vapor, stripping con nitrógeno caliente y agitación de la carga;Steam injection, hot nitrogen stripping and load agitation;
Conducción de los gases de emisión del stripper al condensador, con condensación de vapor de agua y en menor medida de COV's;Conduction emission gases to the stripper condenser, condensing water vapor and less VOC;
Conducción de los gases no condensados al criocondensador, con condensación de los COV's contaminantes;Conduction of non-condensed gases to the cryopredenser, with condensation of the polluting VOCs;
Disposición del nitrógeno de salida del criocondensador en un colector para su calentamiento y posterior inyección al stripper; Manteniéndose la secuencia de destilación hasta que la ausencia de COV's en los condensados del criocondensador determine la finalización del tratamiento.Disposal of the cryocondenser outlet nitrogen in a collector for heating and subsequent injection into the stripper; Maintaining the distillation sequence until the absence of VOCs in condensed criocondensador determine the completion of treatment.
2.- Procedimiento de tratamiento "in situ" de recipientes con sustancias contaminadas por COV's, según la reivindicación 1, caracterizado por comprender las operaciones siguientes:2. Method of treatment "in situ" of containers with substances contaminated by VOCs, according to claim 1, characterized by comprising the following operations:
Adaptación del propio recipiente a tratar como stripper; Tratamiento del recipiente y destilación de los COV's contaminantes, según la secuencia de operaciones descrita en la reivindicación 1. Adaptation of the container to be treated as a stripper; Treatment of the container and distillation of the contaminating VOCs, according to the sequence of operations described in claim 1.
PCT/ES2004/000095 2003-05-22 2004-03-01 Method for the in situ distillation of volatile organic compounds (voc) by means of water vapour injection and hot nitrogen stripping, comprising treatment of the emission gases by condensation and cryocondensation WO2004103513A1 (en)

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ES200301196A ES2220215B1 (en) 2003-05-22 2003-05-22 DISPOSAL PROCEDURE "IN SITU" OF VOLATILE ORGANIC COMPOUNDS "COV'S) THROUGH INJECTION OF WATER VAPOR AND STRIPPING WITH HOT NITROGEN, WITH TREATMENT OF GASES OF EMISSION BY CONDENSATION AND CRIOCONDENSATION.
ESP200301196 2003-05-22

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ITAN20120143A1 (en) * 2012-11-06 2014-05-07 Polaris S P A DEVICE AND PROCEDURE FOR THE REMOVAL OF ORGNIC VOLATILE COMPOUNDS FROM THE WATER
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