EP0949966A1 - Method for treating a catalyst having an active sulphurous phase and contaminated by a mercury compound - Google Patents

Method for treating a catalyst having an active sulphurous phase and contaminated by a mercury compound

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Publication number
EP0949966A1
EP0949966A1 EP97936747A EP97936747A EP0949966A1 EP 0949966 A1 EP0949966 A1 EP 0949966A1 EP 97936747 A EP97936747 A EP 97936747A EP 97936747 A EP97936747 A EP 97936747A EP 0949966 A1 EP0949966 A1 EP 0949966A1
Authority
EP
European Patent Office
Prior art keywords
catalyst
mercury
contaminated
treating
compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
EP97936747A
Other languages
German (de)
French (fr)
Inventor
Paul Berthier
Jean-Paul Bournonville
Christian Ladirat
Bernard Nocher
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pro Catalyse SA
Original Assignee
Pro Catalyse SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pro Catalyse SA filed Critical Pro Catalyse SA
Publication of EP0949966A1 publication Critical patent/EP0949966A1/en
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/28—Regeneration or reactivation
    • B01J27/30—Regeneration or reactivation of catalysts comprising compounds of sulfur, selenium or tellurium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/64—Heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/96—Regeneration, reactivation or recycling of reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/02—Heat treatment

Definitions

  • the present invention relates to a process for treating used catalysts contaminated with mercury in order to regenerate and reuse them.
  • One way of removing mercury from these gases is to bring them into contact with a catalyst based on a sulfur compound, for example a supported catalyst having an active phase based on a sulfur compound, for example copper.
  • the mercury present in the gases reacts on contact with these catalysts to form a mercury compound, in particular mercury sulfide, which remains ad / absorbed on the catalyst.
  • An object of the present invention is to provide a process for the treatment of used catalysts of this type making it possible not only to remove the mercury therefrom but also to regenerate the initial active phase of said catalyst, so as to be able to use it again in the same application without having to re-deposit an active phase.
  • the invention relates to a process for treating a supported catalyst having an active phase based on a sulfur compound and contaminated with a mercury compound, which consists in heating said catalyst to a temperature between 300 and 1000 ° C under an inert atmosphere.
  • the invention therefore relates to a process for the treatment of a supported catalyst having an active phase based on a sulfur compound and contaminated with a mercury compound, which consists in heating said catalyst to a temperature between 300 and 1000 ° C. under an inert atmosphere.
  • the temperature can be between 400 and 600 ° C.
  • the inert atmosphere can be composed of at least one of the following gases: Ar, He,
  • M is preferably argon.
  • the residence time can be variable. Preferably, it is between 1 and 15 hours
  • the sweep rate of the gas mixture can vary and is preferably between 0.1 and 10 liters of gas per hour and per gram of catalyst.
  • the catalyst can be heated in any type of oven, but preferably a tubular oven is used.
  • Mercury is generally removed in gaseous form during processing and is recovered by condensation. Mercury is recovered in the form of mercuric sulfide or metallic mercury.
  • the process according to the invention is particularly useful for treating a supported catalyst having an active phase based on copper sulfide.
  • the amount of this compound in the catalyst to be treated can be variable. This type of catalyst captures mercury in the form of mercuric sulfide.
  • the supported catalyst can have an inorganic support based on alumina, silica, silica-alumina or carbon.
  • the elimination of mercury is followed by analysis by means of the various known analytical techniques for the determination of mercury, in particular by plasma emission spectrometry (SEP).
  • SEP plasma emission spectrometry
  • This catalyst is used in a unit to remove mercury from a natural gas. At the end of the gas treatment, the catalyst comprises 5.2% by weight of mercuric sulphide relative to the weight of the catalyst.
  • the catalyst is emptied from the unit to be treated according to the method of the invention.
  • Procedure 100 g of used catalyst are introduced into a tube furnace.
  • the Argon flow rate is 300 liters / hour.
  • the heating is started at a temperature rise rate of 5 ° C / minute until a temperature of 410 ° C is obtained.
  • the catalyst is kept at this temperature for one hour.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Catalysts (AREA)

Abstract

The invention concerns a method for treating a supported catalyst having a sulphurous compound active base and contaminated by a mercury compound. This method consists in heating the contaminated catalyst at a temperature between 300 and 1000 °C in an inert atmosphere. As a result of this treatment, the catalyst has the same characteristics as it had before being contaminated by mercury.

Description

PROCEDE DE TRAITEMENT D'UN CATALYSEUR PRESENTANT UNE PHASE ACTIVE SOUFREE ET CONTAMINE PAR UN COMPOSE DU MERCURE PROCESS FOR TREATING A CATALYST HAVING AN ACTIVE SULFUR PHASE CONTAMINATED BY A MERCURY COMPOUND
La présente invention concerne un procédé de traitement de catalyseurs usagés contaminés par du mercure afin de les régénérer et les réutiliser.The present invention relates to a process for treating used catalysts contaminated with mercury in order to regenerate and reuse them.
De nos jours, le traitement des produits usés, contaminés, est une activité prenant de plus en plus d'importance. Les contraintes en matière d'environnement conduisent à épurer tous types de liquides, solide ou gaz visant à abaisser leur taux de matières polluantes et éviter le rejet de ces dernières dans l'environnement.Nowadays, the treatment of used, contaminated products, is an activity taking more and more importance. Environmental constraints lead to the purification of all types of liquids, solid or gas aimed at lowering their rate of pollutants and avoiding their rejection into the environment.
De nombreux catalyseurs ont été développés dans le but d'éliminer ces impuretés par absorption, adsorption ou réactions chimiques. Cependant, une fois que les produits contaminés ont été épurés, les impuretés se retrouvent à fortes concentrations dans ces catalyseurs que l'on doit stocker ou détruire.Many catalysts have been developed with the aim of eliminating these impurities by absorption, adsorption or chemical reactions. However, once the contaminated products have been purified, the impurities are found in high concentrations in these catalysts which must be stored or destroyed.
Actuellement, on tend à essayer de traiter ces catalyseurs usagés de manière à en éliminer les impuretés. Ce traitement vise, d'une part, à récupérer des impuretés pour les valoriser ou les transformer sous une forme facilement stockable, et d'autre part, à régénérer les catalyseurs usagés afin de pouvoir les réutiliser. Ce deuxième aspect permet en outre de réaliser des économies puisqu'il n'est pas nécessaire de racheter un nouvelle charge de catalyseur neuf.Currently, there is a tendency to try to treat these used catalysts so as to remove the impurities. This treatment aims, on the one hand, to recover impurities to enhance them or transform them into an easily storable form, and on the other hand, to regenerate the used catalysts in order to be able to reuse them. This second aspect also allows savings to be made since it is not necessary to buy a new charge of new catalyst.
Parmi les impuretés particulièrement néfastes pour l'environnement, le mercure tient une place importante. Il est notamment présent dans le gaz naturel ou les coupes pétrolières. Un moyen d'éliminer le mercure de ces gaz est de les mettre en contact avec un catalyseur à base d'un composé du soufre par exemple un catalyseur supporté présentant une phase active à base d'un composé du soufre, par exemple du sulfure de cuivre.Among the impurities particularly harmful to the environment, mercury occupies an important place. It is especially present in natural gas or petroleum cuts. One way of removing mercury from these gases is to bring them into contact with a catalyst based on a sulfur compound, for example a supported catalyst having an active phase based on a sulfur compound, for example copper.
Le mercure présent dans les gaz réagit au contact de ces catalyseurs pour former un composé du mercure notamment du sulfure de mercure qui reste ad/absorbé sur le catalyseur.The mercury present in the gases reacts on contact with these catalysts to form a mercury compound, in particular mercury sulfide, which remains ad / absorbed on the catalyst.
Actuellement, les catalyseurs usagés comprenant ces composés du mercure sont détruits ou stockés. Et une nouvelle charge de catalyseur neuf doit être utilisée pour continuer de traiter les gaz.Currently, used catalysts comprising these mercury compounds are destroyed or stored. And a new charge of fresh catalyst must be used to continue treating the gases.
Un but de la présente invention est de proposer un procédé de traitement des catalyseurs usagés de ce type permettant non seulement d'en éliminer le mercure mais de plus de régénérer la phase active initiale dudit catalyseur, de manière à pouvoir l'utiliser de nouveau dans la môme application sans avoir à redéposer une phase active. Dans ce but, l'invention concerne un procédé de traitement d'un catalyseur supporté présentant un phase active à base d'un composé du soufre et contaminé par un composé du mercure, qui consiste à chauffer ledit catalyseur à une température comprise entre 300 et 1000 °C sous une atmosphère inerte.An object of the present invention is to provide a process for the treatment of used catalysts of this type making it possible not only to remove the mercury therefrom but also to regenerate the initial active phase of said catalyst, so as to be able to use it again in the same application without having to re-deposit an active phase. For this purpose, the invention relates to a process for treating a supported catalyst having an active phase based on a sulfur compound and contaminated with a mercury compound, which consists in heating said catalyst to a temperature between 300 and 1000 ° C under an inert atmosphere.
D'autres avantages de l'invention apparaîtront plus clairement à la lecture de la description et des exemples.Other advantages of the invention will appear more clearly on reading the description and the examples.
L'invention concerne donc un procédé de traitement d'un catalyseur supporté présentant un phase active à base d'un composé du soufre et contaminé par un composé du mercure, qui consiste à chauffer ledit catalyseur à une température comprise entre 300 et 1000 °C sous une atmosphère inerte.The invention therefore relates to a process for the treatment of a supported catalyst having an active phase based on a sulfur compound and contaminated with a mercury compound, which consists in heating said catalyst to a temperature between 300 and 1000 ° C. under an inert atmosphere.
De préférence, la température peut être comprise entre 400 et 600 °C. L'atmosphère inerte peut être composée d'au moins un des gaz suivants : Ar, He,Preferably, the temperature can be between 400 and 600 ° C. The inert atmosphere can be composed of at least one of the following gases: Ar, He,
N2. M s'agit de préférence de l'argon.N 2 . M is preferably argon.
Le temps de séjour peut être variable. De préférence, il est compris entre 1 et 15 heuresThe residence time can be variable. Preferably, it is between 1 and 15 hours
De même, le débit de balayage du mélange gazeux peut varier et est, de préférence, compris entre 0,1 et 10 litres de gaz par heure et par gramme de catalyseur. Le catalyseur peut être chauffé dans tout type de four, mais de préférence, on utilise un four tubulaire.Likewise, the sweep rate of the gas mixture can vary and is preferably between 0.1 and 10 liters of gas per hour and per gram of catalyst. The catalyst can be heated in any type of oven, but preferably a tubular oven is used.
Le mercure est en général éliminé sous forme gazeuse au cours du traitement et est récupéré par condensation. Le mercure est récupéré sous forme de sulfure mercurique ou de mercure métallique.Mercury is generally removed in gaseous form during processing and is recovered by condensation. Mercury is recovered in the form of mercuric sulfide or metallic mercury.
Le procédé selon l'invention est particulièrement utile pour traiter un catalyseur supporté présentant une phase active à base de sulfure de cuivre. La quantité de ce composé dans le catalyseur à traiter peut être variable. Ce type de catalyseur capte le mercure sous forme de sulfure mercurique. Le catalyseur supporté peut présenter un support minéral à base d'alumine, de silice, de silice-alumine ou de charbon.The process according to the invention is particularly useful for treating a supported catalyst having an active phase based on copper sulfide. The amount of this compound in the catalyst to be treated can be variable. This type of catalyst captures mercury in the form of mercuric sulfide. The supported catalyst can have an inorganic support based on alumina, silica, silica-alumina or carbon.
L'élimination du mercure est suivie par analyse au moyen des différentes techniques analytiques connues pour le dosage du mercure, notamment par spectrométrie d'émission à plasma (SEP). L'avantage du procédé selon l'invention est que non seulement le mercure est éliminé du catalyseur mais, de plus, que la phase active du catalyseur est régénérée et que le support présente les mêmes caractéristiques que lors de sa première utilisation.The elimination of mercury is followed by analysis by means of the various known analytical techniques for the determination of mercury, in particular by plasma emission spectrometry (SEP). The advantage of the process according to the invention is that not only is the mercury removed from the catalyst but, moreover, that the active phase of the catalyst is regenerated and that the support has the same characteristics as when it was first used.
Les exemples suivants illustrent l'invention sans toutefois en limiter la portée.The following examples illustrate the invention without, however, limiting its scope.
EXEMPLESEXAMPLES
Exemple 1 selon l'inventionExample 1 according to the invention
On part d'un catalyseur présentant les caractéristiques suivantes :We start with a catalyst having the following characteristics:
- Support : . alumine- Support:. alumina
. surface spécifique = 125 m2/g . volume poreux total = 0,75 cm3/g - Phase active . CuS. specific surface = 125 m 2 / g. total pore volume = 0.75 cm 3 / g - Active phase. CuS
. taux : 15,3 % en poids par rapport au catalyseur (soit 10,2 % en poids de cuivre). rate: 15.3% by weight relative to the catalyst (i.e. 10.2% by weight of copper)
Ce catalyseur est utilisé dans une unité pour éliminer du mercure d'un gaz naturel. A la fin du traitement du gaz, le catalyseur comprend 5,2 % en poids de sulfure mercurique par rapport au poids du catalyseur.This catalyst is used in a unit to remove mercury from a natural gas. At the end of the gas treatment, the catalyst comprises 5.2% by weight of mercuric sulphide relative to the weight of the catalyst.
Le catalyseur est vidé de l'unité pour être traité selon le procédé de l'invention.The catalyst is emptied from the unit to be treated according to the method of the invention.
Mode opératoire On introduit 100 g de catalyseur usagé dans un four tubulaire.Procedure 100 g of used catalyst are introduced into a tube furnace.
Puis, on met en oeuvre un balayage sous courant d'Argon du four dans lequel le catalyseur a été introduit. Le débit d'Argon est de 300 litre/heure.Then, an argon current sweep of the furnace into which the catalyst was introduced is carried out. The Argon flow rate is 300 liters / hour.
Le chauffage est mis en route à une vitesse de montée en température de 5 °C/minute jusqu'à l'obtention d'une température de 410 °C. Le catalyseur est maintenu à cette température pendant une heure.The heating is started at a temperature rise rate of 5 ° C / minute until a temperature of 410 ° C is obtained. The catalyst is kept at this temperature for one hour.
Résultats :Results:
- taux en Hg : inférieur à 0,2 % en poids par rapport au catalyseur- Hg content: less than 0.2% by weight relative to the catalyst
- taux de Cu : 10,2 % en poids par rapport au catalyseur, soit 15,3 % en poids de CuS- Cu rate: 10.2% by weight relative to the catalyst, i.e. 15.3% by weight of CuS
- surface spécifique : 130 m /g- specific surface: 130 m / g
- volume poreux total : 0,7 cm3/g - total pore volume: 0.7 cm 3 / g

Claims

REVENDICATIONS
1. Procédé de traitement d'un catalyseur supporté présentant un phase active à base d'un composé du soufre et contaminé par un composé du mercure, caractérisé en ce qu'on chauffe ledit catalyseur à une température comprise entre 300 et 1000 °C en présence d'au moins un gaz inerte.1. A method of treating a supported catalyst having an active phase based on a sulfur compound and contaminated with a mercury compound, characterized in that said catalyst is heated to a temperature between 300 and 1000 ° C. presence of at least one inert gas.
2. Procédé selon la revendication 1 , caractérisé en ce que le gaz inerte ets choisi parmi l'argon, l'hélium ou l'azote.2. Method according to claim 1, characterized in that the inert gas is chosen from argon, helium or nitrogen.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que la température est comprise entre 400 et 600 °C.3. Method according to claim 1 or 2, characterized in that the temperature is between 400 and 600 ° C.
4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que le temps de séjour est compris entre 1 et 15 heures.4. Method according to any one of claims 1 to 3, characterized in that the residence time is between 1 and 15 hours.
5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que le catalyseur est balayé par le gaz inerte à un débit compris entre 0,1 et 10 litres/heure/gramme de catalyseur.5. Method according to any one of claims 1 to 4, characterized in that the catalyst is swept by the inert gas at a flow rate between 0.1 and 10 liters / hour / gram of catalyst.
6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'on chauffe le catalyseur dans un four tubulaire.6. Method according to any one of the preceding claims, characterized in that the catalyst is heated in a tubular oven.
7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le mercure éliminé sous forme gazeuse au cours du traitement est récupéré par condensation.7. Method according to any one of the preceding claims, characterized in that the mercury removed in gaseous form during the treatment is recovered by condensation.
8. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le catalyseur supporté présente un support minéral à base d'alumine, de silice, de silice-alumine ou de charbon.8. Method according to any one of the preceding claims, characterized in that the supported catalyst has an inorganic support based on alumina, silica, silica-alumina or carbon.
9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le catalyseur supporté présente une phase active à base de sulfure de cuivre.9. Method according to any one of the preceding claims, characterized in that the supported catalyst has an active phase based on copper sulfide.
10. Procédé selon la revendication 9, caractérisé en ce que le catalyseur est contaminé par le sulfure de mercure. 10. The method of claim 9, characterized in that the catalyst is contaminated with mercury sulfide.
EP97936747A 1996-08-12 1997-08-06 Method for treating a catalyst having an active sulphurous phase and contaminated by a mercury compound Ceased EP0949966A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9610107A FR2752174B1 (en) 1996-08-12 1996-08-12 PROCESS FOR TREATING A CATALYST HAVING AN ACTIVE SULFUR PHASE CONTAMINATED BY A MERCURY COMPOUND
FR9610107 1996-08-12
PCT/FR1997/001460 WO1998006494A1 (en) 1996-08-12 1997-08-06 Method for treating a catalyst having an active sulphurous phase and contaminated by a mercury compound

Publications (1)

Publication Number Publication Date
EP0949966A1 true EP0949966A1 (en) 1999-10-20

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Application Number Title Priority Date Filing Date
EP97936747A Ceased EP0949966A1 (en) 1996-08-12 1997-08-06 Method for treating a catalyst having an active sulphurous phase and contaminated by a mercury compound

Country Status (6)

Country Link
EP (1) EP0949966A1 (en)
JP (1) JP2000502610A (en)
KR (1) KR20000029943A (en)
CA (1) CA2262489A1 (en)
FR (1) FR2752174B1 (en)
WO (1) WO1998006494A1 (en)

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0562509B1 (en) * 1992-03-26 1996-08-21 Hoechst Aktiengesellschaft Reactivation of an activated carbon catalyst used for preparing 1,1,1,2,3,3,3-heptafluoropropane
US5362694A (en) * 1993-03-30 1994-11-08 Sun Company, Inc. (R&M) Sulfur dioxide regeneration of superacid catalyst

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9806494A1 *

Also Published As

Publication number Publication date
CA2262489A1 (en) 1998-02-19
KR20000029943A (en) 2000-05-25
JP2000502610A (en) 2000-03-07
FR2752174A1 (en) 1998-02-13
WO1998006494A1 (en) 1998-02-19
FR2752174B1 (en) 1998-09-11

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