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WO2003018717A1 - Improvements made to the treatment used to reduce sulphur in catalytic gasoline and in intermediate crude distillates by means of silica gel - Google Patents

Improvements made to the treatment used to reduce sulphur in catalytic gasoline and in intermediate crude distillates by means of silica gel Download PDF

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Publication number
WO2003018717A1
WO2003018717A1 PCT/MX2002/000084 MX0200084W WO03018717A1 WO 2003018717 A1 WO2003018717 A1 WO 2003018717A1 MX 0200084 W MX0200084 W MX 0200084W WO 03018717 A1 WO03018717 A1 WO 03018717A1
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WIPO (PCT)
Prior art keywords
silica gel
filter
water
sulfur
regeneration
Prior art date
Application number
PCT/MX2002/000084
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Spanish (es)
French (fr)
Inventor
Israel Quiroz Franco
Mariano FERNÁNDEZ GARCIA
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Fians Capital S.A. De C.V.
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Filing date
Publication date
Application filed by Fians Capital S.A. De C.V. filed Critical Fians Capital S.A. De C.V.
Publication of WO2003018717A1 publication Critical patent/WO2003018717A1/en

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G25/00Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/003Specific sorbent material, not covered by C10G25/02 or C10G25/03
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2400/00Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/02Gasoline

Definitions

  • the present invention is related to production processes of catalytic gasoline and intermediate distillates of crude oil. More particularly, the invention relates to processes for reducing the sulfur content in catalytic gasoline and in petroleum intermediate distillates; and specifically, with the purification of the silica gel filter used in said processes.
  • Said regeneration is necessary since the silica gel is saturated with sulfur and, correspondingly, decreases its effectiveness.
  • the regeneration is carried out by washing with hot air to ensure that the sulfur is oxidized to SO2 and thus removed from the silica gel; for which the filter is isolated, temporarily removing it from the production line, and heated air is injected through it at a temperature of around 450 ° C, until the regeneration of the silica gel is completed, as specified clearly in said patent application.
  • the filter is subsequently cooled and when it reaches the temperature of the refinery's service air, the gel-packed filter is in a position to be reconnected to the production line to be used again in the filtration.
  • the regeneration step which in the Mexican application 99/2593 is carried out with heated air at an elevated temperature, can also be carried out, in an easier, faster and less complicated manner, using a procedure called closed cycle, and that involves the steps of: washing the filter with water at a temperature at least equivalent to the boiling point, until the water comes out clear and without traces of sulfates; dry the filter at 115 ° C; and purify the wash water, to remove traces of sulfur derivatives thereof.
  • the wet water vapor, produced can be reused by drying it previously. This way of regenerating the filter forms the basis for the improvement patent referred to in this description.
  • Figure 1 is a conventional flow chart of the process, in which the situation of two filters packed with silica gel is shown; filters to be regenerated in accordance with the present invention.
  • Figure 2 is a conventional diagram of the assembly for the regeneration of the silica gel contained in the filters of the present invention; Y
  • FIG. 3 is a conventional diagram of the sulfur absorption process in the filter loaded with silica gel, and the subsequent regeneration process thereof.
  • the crude oils are subjected to a series of operations in combined plants, which essentially comprise atmospheric towers, in which products such as primary gasoline, turbosine or naphtha and diesel are obtained; and vacuum distillation towers, in which high vacuum diesel oils are obtained, which are recovered as charges for catalytic plants.
  • catalytic gasoline is obtained as the main product, by means of a catalytic thermal cracking operation of high-vacuum diesel fuels from, among other sources, the vacuum distillation towers referred to in the preceding paragraph. It is in this environment that the invention of the Mexican patent application is used cited above, and where the improvement referred to in this application will apply.
  • the hydrocarbon stream does not substantially lose its sulfur content, so it is normally sent to a desbutanizing tower (not shown), in which, in addition to eliminating light hydrocarbons, such as butane, propane, etc., it is about removing as much sulfur as possible, subjecting the current to a treatment known as "Merox", which is indicated in 3.
  • a treatment known as "Merox" which is indicated in 3.
  • the reduction of sulfur in treatment 3 is limited.
  • the aforementioned Mexican application taught the installation of two filters 4 and 5, loaded with silica gel, at the exit of catalytic gasoline from the chemical treatment Merox 3.
  • the purpose of these filters is to absorb the non-eliminated sulfur in treatment 3, by passing the gasoline through silica gel.
  • the pair of filters 4 and 5 works alternately; that is, one of them (4) is put into operation until the silica gel is close to the saturation point with sulfur, at which point the other filter 5 is connected, while the filter 4 is regenerated by hot air. It is necessary to note that, although only two filters 4 and 5 have been illustrated, each of them can be replaced by a train of filters, so their number could be greater.
  • the number 7 represents the line through which the regeneration means of the filters 4 and 5 are passed countercurrently, when that operation should be performed; while the number 9 identifies the upper filter regeneration valve that, through line 8, connects with a sulfur plant (not shown).
  • FIG. 3 is a flow chart, much more detailed, illustrating the regeneration system referred to in the present improvement.
  • the dry hot steam inlet (without moisture) has been identified with “A”; with “B”, the sulfur-containing water outlet to the bitter water recovery plant; and with “C” the entrance of virgin demineralized water.
  • filters 4 and 5 are arranged in the same relation with respect to the towers 1 , 2 and 3 also defined in said previous application.
  • the improvement of the invention lies is in the way of regenerating filters 4 and 5.
  • one of the filters 4, 5 (which can be representative of a train of filters) is put into operation.
  • the silica gel contained in the filter retains the sulfur contained in the stream of filtration, is saturated with the result that the sulfur content in the product is increasing.
  • the filter is removed from the line, replacing it with the other (5, 4) (which can also be representative of a filter train). While this other filter is in operation, the filter removed from the line is subjected to the regeneration steps.
  • the filter to be regenerated is first subjected to a washing step, as shown with the dotted lines, until the moment the outlet water is clean and clear, without yellow color. At that time it will be free of sulfur. The absence of sulfates is checked visually or (preferred) by a test commonly used with cadmium acetate. If it is verified that the water is clear and clear, the water will be used again for regeneration, in a closed cycle.
  • the water used will be at an elevated temperature, preferably equivalent to at least the boiling point. This will produce, as usual, wet steam, which can be used repeatedly, drying it. Preferably, the steam is reheated. Once the silica gel has been washed with the water at a temperature at least equivalent to the boiling point, as stated above, it is dried, preferably at a temperature of about
  • the filter is able to be used again in the filtration of gasoline or other sulfur-containing product.
  • the regeneration step allows the silica silica to be reused practically without limits; as long as the practice of regenerating it is observed every time it is saturated.
  • the results will invariably remain within the scale of indicated reductions, always below 0.1%.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The invention relates to an improvement made to the chemical treatment used to reduce the sulphur content of catalytic gasoline and intermediate crude distillates using at least one filter filled with silica gel. Said improvement consists in regenerating the silica gel by washing same with water at a temperature that is at least equal to the boiling temperature.

Description

MEJORAS EN TRATAMIENTO PARA REDUCCIÓN DE AZUFRE EN GASOLINAS CATALÍTICAS Y EN DESTILADOS INTERMEDIOS DE CRUDO, CON SÍLICA GELIMPROVEMENTS IN TREATMENT FOR REDUCTION OF SULFUR IN CATALYTIC GASOLINES AND IN INTERMEDIATE CRUDE DISTILLATES, WITH GEL SILICA
CAMPO TÉCNICOTECHNICAL FIELD
La presente invención está relacionada con procesos de producción de gasolina catalítica y destilados intermedios de crudo de petróleo. Más en particular, la invención se relaciona con procesos para reducir el contenido de azufre en gasolinas catalíticas y en los destilados de productos intermedios de petróleo; y específicamente, con la purificación del filtro de sílica gel usado en dichos procesos.The present invention is related to production processes of catalytic gasoline and intermediate distillates of crude oil. More particularly, the invention relates to processes for reducing the sulfur content in catalytic gasoline and in petroleum intermediate distillates; and specifically, with the purification of the silica gel filter used in said processes.
ANTECEDENTES DE LA INVENCIÓN En la solicitud de patente mexicana No. 99/2593, presentada el 18 de marzo deBACKGROUND OF THE INVENTION In Mexican patent application No. 99/2593, filed on March 18,
1999, a nombre de los inventores de la presente, se describe un tratamiento químico para reducir el contenido de azufre de gasolinas catalíticas y destilados intermedios de crudo. En dicho tratamiento se absorbe el azufre en al menos un filtro empacado con gel de sílice, que opera a la presión de salida de los procesos de producción de gasolinas catalíticas y de destilación de crudos intermedios. Un paso de importancia capital en el tratamiento a que se refiere dicha solicitud de patente en trámite es la regeneración de la sílica gel empleada para el paso de filtrado.1999, in the name of the inventors herein, a chemical treatment is described to reduce the sulfur content of catalytic gasoline and intermediate crude distillates. In said treatment the sulfur is absorbed in at least one filter packed with silica gel, which operates at the outlet pressure of the processes of production of catalytic gasolines and distillation of intermediate crudes. A step of capital importance in the treatment referred to in said pending patent application is the regeneration of the silica gel used for the filtering step.
Dicha regeneración, como se especifica claramente en la citada solicitud de patente mexicana, es necesaria puesto que la sílica gel, se va saturando con el azufre y, correspondientemente, va disminuyendo su efectividad. La regeneración es efectuada mediante un lavado con aire caliente para lograr que el azufre se oxide a SO2 y sea sacado así de la sílica gel; para lo cual se aisla el filtro, sacándolo temporalmente de la línea de producción, y se inyecta a través de él aire calentado a una temperatura de alrededor de 450° C, hasta que se complete la regeneración de la sílica gel, tal como se especifica claramente en dicha solicitud de patente. Posteriormente se enfría el filtro y cuando alcanza la temperatura del aire de servicio de la refinería, el filtro empacado con sílica gel está en condiciones de ser reconectado a la línea de producción para ser utilizado de nuevo en la filtración.Said regeneration, as clearly specified in the aforementioned Mexican patent application, is necessary since the silica gel is saturated with sulfur and, correspondingly, decreases its effectiveness. The regeneration is carried out by washing with hot air to ensure that the sulfur is oxidized to SO2 and thus removed from the silica gel; for which the filter is isolated, temporarily removing it from the production line, and heated air is injected through it at a temperature of around 450 ° C, until the regeneration of the silica gel is completed, as specified clearly in said patent application. The filter is subsequently cooled and when it reaches the temperature of the refinery's service air, the gel-packed filter is in a position to be reconnected to the production line to be used again in the filtration.
OBJETIVO DE LA INVENCIÓNOBJECTIVE OF THE INVENTION
Se ha descubierto ahora que el paso de regeneración, que en la solicitud mexicana 99/2593 es efectuado con aire calentado a una temperatura elevada, puede ser efectuado también, de manera más fácil, más rápida y menos complicada, utilizando un procedimiento que se denomina de ciclo cerrado, y que implica los pasos de: lavar el filtro con agua a una temperatura por lo menos equivalente al punto de ebullición, hasta que el agua salga clara y sin rastros de sulfatos; secar el filtro a 115° C; y purificar el agua de lavado, para eliminar los vestigios de derivados de azufre de la misma. El vapor de agua húmedo, producido, podrá volver a ser usado secándolo previamente. Esta manera de regenerar el filtro constituye la base para la patente de mejoras a que se refiere esta descripción.It has now been discovered that the regeneration step, which in the Mexican application 99/2593 is carried out with heated air at an elevated temperature, can also be carried out, in an easier, faster and less complicated manner, using a procedure called closed cycle, and that involves the steps of: washing the filter with water at a temperature at least equivalent to the boiling point, until the water comes out clear and without traces of sulfates; dry the filter at 115 ° C; and purify the wash water, to remove traces of sulfur derivatives thereof. The wet water vapor, produced, can be reused by drying it previously. This way of regenerating the filter forms the basis for the improvement patent referred to in this description.
BREVE DESCRIPCIÓN DE LOS DIBUJOSBRIEF DESCRIPTION OF THE DRAWINGS
A fin de que se pueda comprender mejor las mejoras de la invención, y su conexión con la solicitud de patente 99/2593, presentada el 18 de marzo de 1999, se dará una descripción pormenorizada de los aspectos novedosos incluidos en estas mejoras, y para el efecto se hará referencia en ella a los dibujos anexos, en los que están ilustradas. En dichos dibujos:In order to better understand the improvements of the invention, and its connection with patent application 99/2593, filed on March 18, 1999, a detailed description of the novel aspects included in these improvements will be given, and for this purpose reference will be made thereto to the attached drawings, in which they are illustrated. In these drawings:
La figura 1 es un diagrama de flujo convencional del proceso, en la que se muestra la situación de dos filtros empacados con sílica gel; filtros que habrán de ser regenerados conforme a la presente invención. La figura 2 es un diagrama convencional del ensamble para la regeneración de la sílica gel contenida en los filtros de la presente invención; yFigure 1 is a conventional flow chart of the process, in which the situation of two filters packed with silica gel is shown; filters to be regenerated in accordance with the present invention. Figure 2 is a conventional diagram of the assembly for the regeneration of the silica gel contained in the filters of the present invention; Y
La figura 3 es un diagrama convencional del proceso de absorción del azufre en el filtro cargado con sílica gel, y del subsecuente proceso de regeneración de la misma. DESCRIPCIÓN PORMENORIZADA DE LA INVENCIÓNFigure 3 is a conventional diagram of the sulfur absorption process in the filter loaded with silica gel, and the subsequent regeneration process thereof. PORMENORIZED DESCRIPTION OF THE INVENTION
Tal como se hizo constar en la solicitud de patente mexicana anteriormente citada, y cuyo contenido total se incorpora en la presente como referencia, los crudos de petróleo son sometidos a una serie de operaciones en plantas combinadas, que fundamentalmente comprenden torres atmosféricas, en las que se obtienen productos tales como gasolina primaria, turbosina o nafta y diesel; y torres de destilación al vacío, en las que se obtienen gasóleos de alto vacío, los cuales son recuperados como cargas para plantas catalíticas.As stated in the aforementioned Mexican patent application, and whose total content is incorporated herein by reference, the crude oils are subjected to a series of operations in combined plants, which essentially comprise atmospheric towers, in which products such as primary gasoline, turbosine or naphtha and diesel are obtained; and vacuum distillation towers, in which high vacuum diesel oils are obtained, which are recovered as charges for catalytic plants.
En los reactores de las plantas catalíticas se obtiene como producto principal gasolina catalítica, por medio de una operación de craqueo térmico catalítico de los gasóleos de alto vacío procedentes, entre otras fuentes, de las torres de destilación al vacío a que se hizo referencia en el párrafo precedente. Es en este entorno en el que se utiliza la invención de la solicitud de patente mexicana citada con anterioridad, y donde tendrá aplicación la mejora a que se refiere la presente solicitud.In catalytic plant reactors, catalytic gasoline is obtained as the main product, by means of a catalytic thermal cracking operation of high-vacuum diesel fuels from, among other sources, the vacuum distillation towers referred to in the preceding paragraph. It is in this environment that the invention of the Mexican patent application is used cited above, and where the improvement referred to in this application will apply.
Haciendo referencia primeramente a la figura 1 , el crudo de los campos petrolíferos, con alto contenido de azufre, es enviado a una torre fraccionadoraReferring first to Figure 1, oil from the oil fields, with high sulfur content, is sent to a fractional tower
1 , de donde pasa a la torre catalítica 2.1, from where it passes to the catalytic tower 2.
En las operaciones efectuadas en ellas, la corriente de hidrocarburo no pierde sustancialmente su contenido de azufre, por lo que normalmente es enviada a una torre desbutanizadora (no mostrada), en la que, además de eliminar los hidrocarburos ligeros, como butano, propano, etc., se trata de eliminar la mayor cantidad posible de azufre, sometiendo la corriente a un tratamiento conocido como "Merox", que está indicado en 3. Sin embargo, la reducción de azufre en el tratamiento 3 es limitada.In the operations carried out in them, the hydrocarbon stream does not substantially lose its sulfur content, so it is normally sent to a desbutanizing tower (not shown), in which, in addition to eliminating light hydrocarbons, such as butane, propane, etc., it is about removing as much sulfur as possible, subjecting the current to a treatment known as "Merox", which is indicated in 3. However, the reduction of sulfur in treatment 3 is limited.
Estos contenidos elevados de azufre en las gasolinas catalíticas que salen por la línea 6, limitan la producción. Por este concepto, las pérdidas de producción de gasolina catalítica son actualmente de alrededor de 10%. Sin embargo, conforme transcurre el tiempo, esa pérdida de producción se incrementa dado que los crudos que se están procesando en la actualidad son cada vez más pesados y contienen mayor porcentaje de azufre.These high sulfur contents in the catalytic gasolines that leave on line 6 limit production. For this concept, the losses of catalytic gasoline production are currently around 10%. However, as time goes by, this loss of production increases since the crude oils that are currently being processed are becoming heavier and contain a higher percentage of sulfur.
Para obviar estos inconvenientes, la solicitud mexicana anteriormente citada enseñó la instalación de dos filtros 4 y 5, cargados con sílica gel, a la salida de gasolina catalítica del tratamiento químico Merox 3. La finalidad de estos filtros es la de absorber el azufre no eliminado en el tratamiento 3, haciendo pasar la gasolina a través de sílica gel. La pareja de filtros 4 y 5 trabaja alternativamente; es decir, uno de ellos (4) se pone en función hasta que la sílica gel queda cercana al punto de saturación con azufre, momento en el que se conecta el otro filtro 5, mientras el filtro 4 se somete a regeneración mediante aire caliente. Es necesario advertir que, si bien se ha ilustrado únicamente dos filtros 4 y 5, cada uno de ellos puede ser reemplazado por un tren de filtros, por lo que su número podría ser mayor.To obviate these inconveniences, the aforementioned Mexican application taught the installation of two filters 4 and 5, loaded with silica gel, at the exit of catalytic gasoline from the chemical treatment Merox 3. The purpose of these filters is to absorb the non-eliminated sulfur in treatment 3, by passing the gasoline through silica gel. The pair of filters 4 and 5 works alternately; that is, one of them (4) is put into operation until the silica gel is close to the saturation point with sulfur, at which point the other filter 5 is connected, while the filter 4 is regenerated by hot air. It is necessary to note that, although only two filters 4 and 5 have been illustrated, each of them can be replaced by a train of filters, so their number could be greater.
Con referencia a la figura 2, el número 7 representa la línea a través de la cual se hace pasar a contracorriente el medio de regeneración de los filtros 4 y 5, cuando deba efectuarse esa operación; mientras que el número 9 identifica la válvula superior de regeneración de los filtros que, a través de la línea 8, conecta con una planta de azufre (no mostrada).With reference to Figure 2, the number 7 represents the line through which the regeneration means of the filters 4 and 5 are passed countercurrently, when that operation should be performed; while the number 9 identifies the upper filter regeneration valve that, through line 8, connects with a sulfur plant (not shown).
La figura 3 es un diagrama de flujo, mucho más detallado, que ilustra el sistema de regeneración a que se refiere la presente mejora. Se ha identificado con "A" la entrada de vapor caliente seco (sin humedad); con "B", la salida de agua que contiene azufre hacia la planta recuperadora de aguas amargas; y con "C" la entrada de agua desmineralizada virgen.Figure 3 is a flow chart, much more detailed, illustrating the regeneration system referred to in the present improvement. The dry hot steam inlet (without moisture) has been identified with "A"; with "B", the sulfur-containing water outlet to the bitter water recovery plant; and with "C" the entrance of virgin demineralized water.
Como se ha representado claramente en la figura 3, en esta mejora también los filtros 4 y 5 (que corresponden a los filtros de igual numeración ilustrados y reivindicados en la solicitud mexicana mencionada antes) están dispuestos en la misma relación con respecto a las torres 1 , 2 y 3 igualmente definidas en dicha solicitud anterior. Donde reside la mejora de la invención es en la manera de regenerar los filtros 4 y 5. Como se explicó más atrás, uno de los filtros 4, 5 (que puede ser representativo de un tren de filtros) es puesto en operación. A medida que la sílica gel contenida en el filtro va reteniendo el azufre contenido en la corriente de filtración, se va saturando con el resultado de que el contenido de azufre en el producto va incrementándose. En este punto, se saca de línea el filtro, reemplazándolo con el otro (5, 4) (que también puede ser representativo de un tren de filtros). Mientras este otro filtro está en operación, el filtro retirado de línea es sometido a los pasos de regeneración.As clearly shown in Figure 3, in this improvement also filters 4 and 5 (corresponding to the filters of equal number illustrated and claimed in the Mexican application mentioned above) are arranged in the same relation with respect to the towers 1 , 2 and 3 also defined in said previous application. Where the improvement of the invention lies is in the way of regenerating filters 4 and 5. As explained above, one of the filters 4, 5 (which can be representative of a train of filters) is put into operation. As the silica gel contained in the filter retains the sulfur contained in the stream of filtration, is saturated with the result that the sulfur content in the product is increasing. At this point, the filter is removed from the line, replacing it with the other (5, 4) (which can also be representative of a filter train). While this other filter is in operation, the filter removed from the line is subjected to the regeneration steps.
El filtro que va a ser regenerado es sometido primeramente a un paso de lavado, como se muestra con las líneas punteadas, hasta el momento en que el agua de salida esté limpia y clara, sin color amarillo. En ese momento estará libre de azufre. Se efectúa una comprobación de la ausencia de sulfatos visualmente o bien (preferido) mediante una prueba comúnmente utilizada con acetato de cadmio. Si se comprueba que el agua está límpida y clara, se volverá a usar el agua para la regeneración, en ciclo cerrado.The filter to be regenerated is first subjected to a washing step, as shown with the dotted lines, until the moment the outlet water is clean and clear, without yellow color. At that time it will be free of sulfur. The absence of sulfates is checked visually or (preferred) by a test commonly used with cadmium acetate. If it is verified that the water is clear and clear, the water will be used again for regeneration, in a closed cycle.
El agua empleada encontrará a temperatura elevada, de preferencia equivalente a por lo menos el punto de ebullición. Esto producirá, como es normal, vapor de agua húmedo, que podrá ser usado repetidas veces, secándolo. De preferencia, se recalienta el vapor. Una vez lavada la sílica gel con el agua a una temperatura por lo menos equivalente al punto de ebullición, como se dice arriba, se la somete a secado, de preferencia a una temperatura de alrededor deThe water used will be at an elevated temperature, preferably equivalent to at least the boiling point. This will produce, as usual, wet steam, which can be used repeatedly, drying it. Preferably, the steam is reheated. Once the silica gel has been washed with the water at a temperature at least equivalent to the boiling point, as stated above, it is dried, preferably at a temperature of about
115°C. Una vez seca la sílica gel, el filtro está en condiciones de ser utilizado nuevamente en la filtración de la gasolina u otro producto que contenga azufre.115 ° C Once the silica gel dries, the filter is able to be used again in the filtration of gasoline or other sulfur-containing product.
E J E M P L O Una gasolina catalítica, con un contenido inicial de azufre de 0.17% en peso, fue sometida a purificación en un filtro de la invención, a base de un lecho de gel de sílice. Se mantuvo la filtración hasta que la sílica gel arrojó resultados negativos de filtración. En ese punto se lavó la sílica gel a contracorriente con vapor recalentado, hasta que el agua de lavado resultante fue límpida y clara. Se repitió por dos veces este ciclo de operaciones, efectuando una operación de retrolavado y secando la sílica gel después de cada saturación del filtro. Los resultados de las tres operaciones de filtración fueron los siguientes:EXAMPLE A catalytic gasoline, with an initial sulfur content of 0.17% by weight, was subjected to purification on a filter of the invention, based on a bed of silica gel. Filtration was maintained until the silica gel showed negative results. of filtration At that point the silica gel was washed countercurrently with superheated steam, until the resulting wash water was clear and clear. This cycle of operations was repeated twice, performing a backwash operation and drying the silica gel after each saturation of the filter. The results of the three filtration operations were the following:
TABLA I RESULTADOS DE FILTRACIÓNTABLE I FILTRATION RESULTS
Figure imgf000008_0001
Figure imgf000008_0001
Si bien se utilizó únicamente tres veces el filtro en este ejemplo, es de señalar que el paso de regeneración permite la reutilización de la sílica gel prácticamente sin límites; siempre y cuando se observe la práctica de regenerarla cada vez que se sature. Los resultados se mantendrán invariablemente dentro de la escala de reducciones señaladas, siempre inferior al 0.1%.Although only three times the filter was used in this example, it should be noted that the regeneration step allows the silica silica to be reused practically without limits; as long as the practice of regenerating it is observed every time it is saturated. The results will invariably remain within the scale of indicated reductions, always below 0.1%.
De lo anterior se verá que en todos los casos la gasolina filtrada en el filtro regenerado de acuerdo con la presente invención redujo el contenido de azufre en alrededor del 50% respecto al contenido inicial; demostrando de esa manerala efectividad de la operación de regeneración hecha de acuerdo con la presente invención.From the foregoing it will be seen that in all cases the gasoline filtered in the regenerated filter according to the present invention reduced the sulfur content by about 50% with respect to the initial content; thereby demonstrating the effectiveness of the regeneration operation performed in accordance with the present invention.
Aun cuando se ha descrito el concepto inventivo pormenorizadamente en lo que antecede, se entenderá que sólo se ha hecho en beneficio de la claridad, y no como limitación al alcance de la invención. Even when the inventive concept has been described in detail in the foregoing, it will be understood that it has only been done for the benefit of clarity, and not as a limitation on the scope of the invention.

Claims

Reivindicaciones Claims
1.- En un procedimiento para reducir el contenido de azufre en gasolinas catalíticas y en destilados intermedios de crudo, mediante filtración en al menos un filtro empacado con sílica gel, donde la sílica gel del al menos un filtro se somete a un paso de regeneración, la mejora caracterizada porque la regeneración incluye los pasos de: lavar el al menos un filtro con agua a temperatura elevada hasta que el agua de lavado esté sustancialmente libre de derivados de azufre y sea límpida y transparente a la vista; secar el al menos un filtro a temperatura elevada y tratar los fluidos de lavado para recircularlos a una operación de regeneración posterior.1.- In a procedure to reduce the sulfur content in catalytic gasolines and in intermediate distillates of crude, by filtration in at least one filter packed with silica gel, where the silica gel of the at least one filter is subjected to a regeneration step The improvement characterized in that the regeneration includes the steps of: washing the at least one filter with high temperature water until the washing water is substantially free of sulfur derivatives and is clear and transparent to the eye; Dry the at least one filter at elevated temperature and treat the wash fluids to recirculate them to a subsequent regeneration operation.
2.- Mejoras de conformidad con la reivindicación 1 , caracterizadas además porque el agua es introducida al filtro a contracorriente, y se encuentra por lo menos a la temperatura de ebullición.2. Improvements according to claim 1, further characterized in that the water is introduced to the counter current filter, and is at least at the boiling temperature.
3.- Mejoras de conformidad con la reivindicación 1 , caracterizadas además porque el paso de secado se efectúa a alrededor de 115° C.3. Improvements in accordance with claim 1, further characterized in that the drying step is carried out at about 115 ° C.
4.- Mejoras de conformidad con cualquiera de las reivindicaciones precedentes, caracterizadas además porque el agua se encuentra al menos parcialmente en la forma de vapor de agua.4. Improvements in accordance with any of the preceding claims, further characterized in that the water is at least partially in the form of water vapor.
5.- Mejoras de conformidad con cualquiera de las reivindicaciones precedentes, caracterizadas además porque toda la operación de regeneración se efectúa como un ciclo cerrado. 5. Improvements in accordance with any of the preceding claims, further characterized in that the entire regeneration operation is carried out as a closed cycle.
PCT/MX2002/000084 2001-08-24 2002-08-23 Improvements made to the treatment used to reduce sulphur in catalytic gasoline and in intermediate crude distillates by means of silica gel WO2003018717A1 (en)

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MXPA/A/2001/008582 2001-08-24
MXPA01008582 MXPA01008582A (en) 2001-08-24 2001-08-24 Improvements in treatment for the reduction of sulfur in.

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WO2003018717A1 true WO2003018717A1 (en) 2003-03-06

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4405276A1 (en) * 1994-02-19 1995-08-24 Otto Luft Klimatech Gmbh Process for the separation of ethylene oxide from exhaust air or exhaust gas streams
US6111162A (en) * 1996-04-22 2000-08-29 Snamprogetti S.P.A. Process for removing oxygenated contaminants from hydrocarbon streams

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4405276A1 (en) * 1994-02-19 1995-08-24 Otto Luft Klimatech Gmbh Process for the separation of ethylene oxide from exhaust air or exhaust gas streams
US6111162A (en) * 1996-04-22 2000-08-29 Snamprogetti S.P.A. Process for removing oxygenated contaminants from hydrocarbon streams

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