ES2220215A1 - 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

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Publication number
ES2220215A1
ES2220215A1 ES200301196A ES200301196A ES2220215A1 ES 2220215 A1 ES2220215 A1 ES 2220215A1 ES 200301196 A ES200301196 A ES 200301196A ES 200301196 A ES200301196 A ES 200301196A ES 2220215 A1 ES2220215 A1 ES 2220215A1
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Prior art keywords
vocs
treatment
distillation
condensation
cryocondensation
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Granted
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ES200301196A
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Spanish (es)
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ES2220215B1 (en
Inventor
Evaristo Fontecha Cuetos
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Priority to ES200301196A priority Critical patent/ES2220215B1/en
Priority to PCT/ES2004/000095 priority patent/WO2004103513A1/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38Steam distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/343Distillation 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • B01D5/006Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation

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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

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.Procedure of distillation " in situ " of volatile organic compounds (VOCs) 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 process of distillation presenting the following applications:

- Tratamiento de aguas y lodos contaminados por COV's.- Treatment of water and sludge contaminated by VOCs.

- Reciclado de disolventes y otros COV's contaminados.- Recycling of solvents and other VOCs contaminated

- Tratamiento de recipientes con sustancias contaminadas por COV's.- Treatment of containers with substances contaminated by VOCs.

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.The procedure includes operations concerning Safety and Environment (inertization of vessels and circuits with nitrogen, emission control by cryopreservation, recovery and confinement of VOCs contaminants, etc.), which make it especially suitable for treating those VOCs that present a high explosive risk or that are 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 art

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 Treatment of substances with VOC content, is in Incineration plants and distillation plants. The Biological treatment plants and procedures stabilization, are not feasible for substance treatment containing 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 plants incinerators (high concentration of halogens, sulfur, etc.) and also not admitted to distillation plants (temperatures of autoignition in vacuum pumps, cryogenic temperatures of condensation, etc.) An example of VOC with these characteristics It 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 procedure object of the patent allows recycle contaminated carbon sulfide and also allows distillation of contaminated water and sludge of carbon sulfide, in all cases completely safe and with recovery of a carbon puride of 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 procedure object of this patent of precise invention for its application of the following elements: a treatment vessel or stripper; a heating source with its electronic regulation unit; a capacitor with its refrigeration system; a VOC cryoprodenser with its tank of liquid nitrogen; and a manifold with heater nitrogen.

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.The treatment vessel or stripper must dispose of the following components: water vapor diffusers and nitrogen; a temperature probe; a stirrer; a valve security; and various tubing for the gas lines of emission, water vapor, nitrogen and stripper drainage.

El procedimiento objeto de la presente patente de invención comprende las operaciones siguientes:The procedure object of the present patent of The invention comprises the following operations:

--
Llenado de la vasija de tratamiento o stripper con la carga de COV's a destilar.Filling the vessel of treatment or stripper with the load of VOCs to distill.

--
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 control unit steam. The distillation temperature will be determined by the boiling temperature of VOCs and the cooling capacity of  condensation system The installed cooling capacity must be sufficient to counteract specific heats and latent 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 control panel of the cryopredenser parameters cryocondensation circuit temperature, depending on the melting temperature and emission limits of 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 in the stripper The nitrogen flow rate of stripping must be limited, since being untiring, it is cooled to cryogenic temperatures as it passes through the cryo condenser and consumes part of the power Refrigerator installed.

--
Conducción de los gases de emisión del stripper al condensador, con condensación de vapor de agua y en menor medida de COV's.Driving the emission gases from the stripper to the condenser, with condensation of water vapor and to a lesser extent VOCs.

--
Conducción de los gases no condensados al criocondensador, con condensación de los COV's contaminantes.Driving the gases not condensed to the cryopredenser, with condensation of the VOCs contaminants.

--
Disposición en un colector del nitrógeno gasificado en el criocondensador para su calentamiento y posterior inyección al stripper.Provision in a Nitrogen collector gasified in the cryo condenser for its heating and subsequent injection to 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 COV's y por tanto demanda de potencia frigorífica, se puede incrementar la temperatura de destilación.Finish the distillation when the absence of solvent in the condensates of the cryopredenser In the final distillation phase, at  there is a lower vaporization of VOCs and therefore demand for cooling capacity, the temperature of distillation.

El stripping con nitrógeno caliente aporta cualidades al procedimiento en los aspectos siguientes:Hot nitrogen stripping provides qualities of the procedure in the following aspects:

1.one.
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.Reduce the boiling temperature of VOCs. In accordance with the Law of Dalton the total steam tension will be the sum of the tensions partial, so VOCs behave as in a distillation under reduced pressure.

2.two.
Inertiza la corriente de gases, evitando así la formación de atmósferas inflamables o explosivas.Inertizes the gas flow, thus preventing the formation of atmospheres flammable or explosive

3.3.
Actúa como agente portador de los COV's desde la vasija de tratamiento hasta el criocondensador, haciendo innecesario el uso de extractores.Act as agent VOC carrier from the treatment vessel to the Cryo condenser, making the use of extractors

4.Four.
Actúa como coadyuvante o incluso como sustituto del agitador de la carga durante la destilación.Act like adjuvant or even as a substitute for the load agitator during distillation.

5.5.
Actúa como fuente localizada de calor mejorando la eficiencia del stripping.Acts as a source localized 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 in which it is represented, by way of illustrative and non-limiting example, the provision of equipment for an example of treatment of a load with VOCs pollutants

Los elementos designados con números en la figura 1 corresponden a las partes que se indican a continuación:The elements designated with numbers in the figure 1 correspond to the parts indicated below:

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 treatment vessel or stripper (1) has of water vapor diffusers (2) a nitrogen diffuser network (3) a stirrer (4) and a temperature probe (5). The probe of temperature sends the signal to an electronic unit (6) that regulates the steam provided by the steam source (7). Emission gases (8) are conducted to a capacitor (9) connected to a glycol water cooler (10). Non-condensed gases pass to a VOC cryoprodenser (11) powered by a source of liquid nitrogen (12). The temperature parameters are entered in the control panel of the cryoprunner (13) depending on the VOC emission limits in treated gases (14). The line Nitrogen gas at the outlet of the cryo condenser (15) is connected to a collector with nitrogen heater (16) for reuse of nitrogen as a source of stripping; (17).

Modo preferente de realización de la invenciónPreferred 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 procedure is presented in the treatment of water and sludge contaminated by solvent. The solvents to be distilled must have a boiling temperature 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, la secuencia operacional es la siguiente:In view of Figure 1 and according to the description of the procedure, the operational sequence is the next:

--
Instalación de equipos y carga del stripper con las aguas y lodos contaminados de disolvente.Installation of equipment and loading of the stripper with the water and sludge contaminated 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.Programming of the distillation temperature in the electronic control unit of steam, in accordance with the available cooling capacity. Programming in the cryocondenser control panel of the temperature parameters of the cryocondensation circuit, in function of melting temperature and emission limits of solvent

--
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.).Steam injection, stripping with hot nitrogen and stirring the load in the stripper The steam injection can be replaced by another heating system (electrical resistors, exchangers of heat, 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.Driving the emission gases from the stripper to the condenser, with condensation of water vapor and to a lesser extent solvent vapor. The condenser, connected to a glycol water cooler, prevents the formation of ice plugs in the cryopredenser and allows Reduce 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 the gases not condensed to the cryopredenser, with steam condensation of solvent. The cryo condenser has a system of "defrosting" heating used to remove the plugs of ice, so sometimes you can do without condenser and its glycol water cooler.

--
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 Exit nitrogen from the cryopredenser in a collector for its heating and subsequent injection to the stripper. The collector has of a discharge valve, which allows the atmosphere to be released another facility the 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.Finish the distillation when the absence of solvent in the condensates of the cryopredenser. In the final distillation phase, at  there is less solvent vaporization and therefore demand of cooling capacity, the temperature of distillation.

Claims (2)

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 (VOCs) 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;Vessel load of treatment 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 control unit water vapor;
--
Programación en el panel de control del criocondensador de los parámetros de temperatura del circuito de criocondensación;Programming in the control panel of the cryopredenser parameters cryocondensation circuit temperature;
--
Inyección de vapor, stripping con nitrógeno caliente y agitación de la carga;Steam injection, stripping with hot nitrogen and stirring the load;
--
Conducción de los gases de emisión del stripper al condensador, con condensación de vapor de agua y en menor medida de COV's;Driving the emission gases from the stripper to the condenser, with condensation of water vapor and to a lesser extent VOCs;
--
Conducción de los gases no condensados al criocondensador, con condensación de los COV's contaminantes;Driving the gases not condensed to the cryopredenser, with condensation of the VOCs contaminants;
--
Disposición del nitrógeno de salida del criocondensador en un colector para su calentamiento y posterior inyección al stripper;Disposition of Exit nitrogen from the cryopredenser in a collector for its heating and subsequent injection to the stripper;
Manteniéndose la secuencia de destilación hasta que la ausencia de COV's en los condensados del criocondensador determine la finalización del tratamiento.Maintaining the distillation sequence until that the absence of VOCs in the condensates of the cryo condenser Determine the end 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. Procedure " in situ " treatment 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;Adaptation of own container to be treated as a stripper;
--
Tratamiento del recipiente y destilación de los COV's contaminantes, según la secuencia de operaciones descrita en la reivindicación 1.Treatment of container and distillation of polluting VOCs, according to the sequence of operations described in claim 1.
ES200301196A 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. Expired - Fee Related ES2220215B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
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.
PCT/ES2004/000095 WO2004103513A1 (en) 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

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
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.

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ES2220215A1 true ES2220215A1 (en) 2004-12-01
ES2220215B1 ES2220215B1 (en) 2006-02-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107715486A (en) * 2017-11-22 2018-02-23 广东银洋环保新材料有限公司 A kind of emulsion VOC release units

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2010082A6 (en) * 1988-01-14 1989-10-16 Chemical Waste Management Process and apparatus for separating organic contaminants from contaminated inert materials.
EP1167905A2 (en) * 2000-06-20 2002-01-02 Air Products And Chemicals, Inc. Process and apparatus for removal of volatile compounds from process gases

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2010082A6 (en) * 1988-01-14 1989-10-16 Chemical Waste Management Process and apparatus for separating organic contaminants from contaminated inert materials.
EP1167905A2 (en) * 2000-06-20 2002-01-02 Air Products And Chemicals, Inc. Process and apparatus for removal of volatile compounds from process gases

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107715486A (en) * 2017-11-22 2018-02-23 广东银洋环保新材料有限公司 A kind of emulsion VOC release units
CN107715486B (en) * 2017-11-22 2023-09-12 广东银洋环保新材料有限公司 Emulsion VOC breaks away from device

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ES2220215B1 (en) 2006-02-16
WO2004103513A1 (en) 2004-12-02

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