DE1284951B - Process for the activation and regeneration of hydrocracking catalysts - Google Patents

Description

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The invention relates to a method for activating conventional regeneration methods with frequent re- and regeneration of a nickel sulfide or nickel recovery in many cases has adverse effects on the sulfide — molybdenum sulfide containing hydrogenation catalyst. There is therefore a clear need catalyst with high metal content, which is more than for a process for reactivating deactivated 10 weight percent sulfur in connection with 5 catalysts containing nickel sulfide. With help Nickel or nickel-molybdenum on a heat-treated the present invention receives the deactivated contains permanent oxide carrier, which thereby ge catalyst even greater effectiveness than a is characterized by the fact that the catalyst is first fresh catalyst.

for the conversion of the nickel and molybdenum components in the process for the hydrogenation conversion

nents in nickel and molybdenum oxide with a gas that maintains the deactivation combustion increases at temperatures of the catalyst usually between 288 and 510 ⁰ C and increased pressure, the severity of the conditions used. The more active the person is after initially converting the nickel oxide into a catalyst, the less sharp nickel can be at elevated temperatures below 538 ° C with the conditions used, and the less rapid the deactivation of a hydrogen-containing, reducing gas below 15, as a result that brings increased pressure into contact, then regeneration or reactivation less frequently renewed with a gas that maintains the combustion, are necessary.

preferably under the conditions of the first oxy- With the method according to the invention it is possible

dation stage treated to nickel in nickel oxide for the life of a catalyst, which converts from nickel sulfide, and then the catalyst is at elevated 20 on a heat-resistant oxide carrier, to temperatures below 455 ⁰ C again sulfided. lengthen, taking turns with the catalyst

The process according to the invention is used in the oxy-hydrogenation-hydrocarbon conversion stage, preferably using a process, and then regenerated until the nitrogen-air mixture is carried out at a pressure above the regeneration of the catalyst its original 14 kg / cm ² , and the sulphidation is 25 lent effectiveness can no longer reproduce, and preferably with a sulfidizing gas, such as H ₂ S, then reactivated the catalyst to at least its mixtures of H ₂ S and hydrogen or mixtures of initial activity.

of hydrogen and organic sulfur compounds- According to the present invention, a catalyst

genes that _{can be reduced to H 2} S, with a catalyst made of nickel sulfide or nickel sulfide-molybdenum, a catalyst temperature below 399 ° C, passed through sulfide on a heat-resistant oxide carrier. activated or regenerated by the metal compounds

Certain catalysts that fertilize nickel sulfide one after the other first in nickel oxide or contain a heat-resistant oxide carrier, molybdenum oxide, then the nickel oxide in nickel, prove to be particularly useful for procedures in which this is done again in nickel oxide and finally the which hydrocarbon oils convert 35 metals into sulphides at elevated temperatures, and pressure with an excess of hydrogen and the catalyst consists of nickel sulfide or

Catalyst at conditions brought into contact with nickel sulfide — molybdenum sulfide on a homogeneous, resulting in a net use of hydrogen refractory oxide carrier. It can e.g. B. a nickel and lead to the conversion of the oil into a more valuable prosulfide-silica-alumina hydrocracking catalyst or duct. The hydrogen can be consumed: 40 be a nickel sulfide-molybdenum sulfide-alumina-hydrogenation- (1) in the conversion of olefins and other catalyst. Further nickel sulfide-containing unsaturated compounds in more saturated compounds. Catalysts for which the present invention bonds; (2) applies to the conversion of impurities, arise for the skilled person by themselves. B. organic nitrogen, oxygen, for example, the combinations of nickel sulfide, sulfur and halogen compounds in easily ent- 45 with one or more other metals of the removable NH ₃ , H ₂ O, H ₂ S and acid halides and in groups VIII, VIb and Ib of the Periodic Table of Hydrogenated Organic Compounds; (3) are mentioned in the cracking and as a heat-resistant oxide carrier hydrogenation or the hydrocracking of compounds alumina, silica, magnesia, in nature predecessors with higher molecular weight in compound earths and clays and mixtures of them, fertilize with lower molecular weight or (4) at 50 In addition, activating, improving a combination of some or all of the above and stabilizing ingredients, such as. B. Halide reactions. The term used here "Um- and metals of groups Ia and II a, present conversion with the help of hydrogen" should be for each of the. The processes for the production of these types of processes apply. Until now, lysers are numerous and well known; they do not need a catalytic process for the conversion of 55 not to be enumerated here. Hydrocarbon oil with the help of hydrogen is a particularly successful application

found, in which the catalyst is not de-active at the end of the process present in the reactivation of devolatized which is usually the result of the gradually activated nickel sulfide-molybdenum sulfide-alumina-Ka- (or rapid) deposition of carbonaceous catalysts with high metal content and nickel sulfide material is commonly referred to as "coke." 60 silica-alumina catalysts that are beneficial at Once the catalyst is deactivated, it must be used in a two-step process Neither be replaced, nor its activity must be replaced by a hydrocarbon oil that is nitrogen Treatment to be restored. Contains impurities, in a first stage under spoiling The regeneration is done by burning the first-mentioned catalyst with water Coke applied. Often, however, the 65 fabric treated and then the purified oil in is sufficient mere removal of coke is not enough, as others ent- a second stage using the second activating Effects with regard to the catalytic converter - called catalytic converter hydrocracked. When the carbon structure can occur themselves. In addition, the hydrogen oil feed has a high boiling point,

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like ζ. A heavy gas oil, and / or a high one. B. a shale oil distillate, catalyst by contact with a steam are relatively strict conditions with a mixture of air and a between about 455 and about higher temperature and pressure required around the 621 ⁰ C maintained catalyst temperature. Nitrogen Compounds and Other Impurities 5 In the present process, the best can be hydrogenated in the first stage. Achieving results on the catalyst if you use the catalyst, carbon-containing deposits form, which cause an ever increasing loss of activity through contact with a nitrogen-air mixture. a catalyst temperature kept below 510 ^° C. So far, the process had to be terminated and the oxidized. In particular, if nickel sulfide-molybdenum catalysts are replaced, if they are not replaced by verio sulfide-alumina catalysts with a high metal content, the carbon-containing deposits of the 4 to 10% nickel and 15.5 to 30% molybdenum decatalysts burn and renewed sulfidation is regenerated became. It has been found that the regeneration of the temperature during the oxidation is useful, nickel sulfide-molybdenum sulfide-alumina catalyst to avoid damage to the catalyst, by conventional methods no more than two or 15 preferably allows the oxidations to be carried out successfully three times in the case of catalysis. door temperatures carried out at least during

With the help of the present invention, the activity of the freshly produced 399 ° C is maintained again between about 288 and about catalyst during the first combustion, with nitrogen in the case of a catalyst. As the increased pressure of over 14 kg / cm ² , described below, is circulated, the effectiveness of a strongly de-active one can be seen. Air is added, so that a fourth catalyst is preferably used, in which the conventional gas contains 0.1 to 4 mol percent oxygen. Very regeneration methods only about 50% of the activity is advantageous to use the same pressure to restore in the fresh state, by which the present invention is normally used in hydrocarbon treatment, and to bring between 14 and speed than in the fresh state. As a result, it can be 25 700 kg / cm ^2. Combustion products, the starting catalyst charge can be very much like e.g. B. CO ₂ , SO ₂ and H ₂ O, will use the cycle for a long time. running gas removed. The above conditions are for

On the other hand, the gradual deactivation takes place - the use of nickel-molybdenum-alumina cata-

tion of nickel sulfide - silica - alumina - hydrolyzers with a high metal content preferred, the more

cracking catalyst by poisoning by the not 30 than 10 ° / (, in connection with the nickel and sulfur

Nitrogen compounds removed from the feed contain molybdenum when the catalyst is in the

gene, carbonaceous deposits and sulphide state. The high metal content seems

Changes in the nickel catalyst itself. Previously, the sintering of the catalyst had to be accelerated, if

the usual regenerations of the nickel sulfide silica the temperatures are not carefully regulated.

earth-alumina catalyst only partially successful 35 Good results can also be achieved if

and could not be used more than once. nickel sulfide catalysts with a lower metal

As a result, the present invention is useful when oxidized in the above-mentioned manner. Catalysis

However, as a method of restoring the agents with a lower metal content,

eligibility of these catalysts. homely less sensitive to increased

The present invention is different from 40 temperature.

Following the usual regeneration procedures. The reduction of the catalyst is particularly one

Details: critical stage in the activation process of the present

The usual regeneration process consists of the invention. This is surprising since the catalytic

two stages, with (1) the catalyst in the course of the catalysts are not active in the reduced state. Much-

Burning of coke deposits oxidizes and 45 more the catalysts have to be sulfided in order

(2) is sulfided again. The invention, however, a high effectiveness for the hydrogenation conversion

includes four stages in the following order: treatment method in which they are used

(1) Oxidation of the catalyst to produce be. The reduction stage is therefore an unexpected one

Nickel oxide, (2) reduction of the catalyst is an essential part of the present invention.

Manufacture of nickel metal, (3) oxidation of the cata- 5 ° With the above-mentioned nickel sulfide-molybdenum sulfide

lysators with the production of nickel oxide and (4) sulfide-alumina catalysts with a high metal content

fidating the catalyst to produce nickel - the nickel can be used according to the present invention

sulfide. In one respect, the invention is therefore a preferably by contacting the oxidized catalyst

Improvement of the process for the regeneration of sators with hydrogen at increased pressure over 14 kg /

Reduce nickel sulfide catalysts on supports by oxy- 55 cm ^a . The pressure is preferably at or

dation and renewed sulphidation, using the catalytic converter close to the pressure

lysator is reduced after the aforementioned oxidation and fabric treatment process is used. The tem-

then the catalyst before the renewed sulfi- perature of the hydrogen is regulated so that the

dieren oxidized again. Catalyst temperature initially preferably between

In the usual regeneration process, the 60 204 and 399 ^° C. and the catalyst is kept ^{below 538 °} C. at all times during the reduction by contact with a steam. The treatment is oxidized by the air / air mixture. With sufficient time in practice to ensure an almost complete implementation of the present process, the reduction of the nickel oxide to the metal can be achieved; best results are achieved if the oxide is usually used for 24 hours or more. If a dilute ion is used using a relatively dry reducing gas, such as e.g. B. a water, the combustion supporting gas such. B. substance-nitrogen mixture, then compared to an exhaust gas or a nitrogen-air mixture, reduction with pure H ₂ carried out longer treatment times. or higher pressures are required.

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It has already been suggested earlier that the nickel break-up should be carried out because it can use emergency catalysts reduce before sulphiding. In being manoeuvrable to the reaction vessel for examination In such cases, bring the catalyst, the nickel open, or the reaction vessel during maintenance contains reduced metal state, in contact with cutting work on other parts of the plant sulphiding medium in order to reduce the nickel 5 ren. Interruptions of the procedure should only then convert directly into nickel sulfide. The benefits of being made when the catalyst is in Oxide Invention cannot be found through such a pre-condition, because many are nickel catalysts because it has been found that the nickel in the reduced or sulphided state is pyrophoric, must be oxidized before sulfiding. According to the following examples illustrate the process at

Reduction of the nickel in the manner described above. When used to reactivate a sulfur-active one, the nickel is therefore preferably re-dated in the same way as sulphided nickel-molybdenum-alumina hydrogenation for the first oxidation with a high metal content. Of course, the catalyst contains very little coal or coke, the first example concerns the hearth known per se at this point in time, and the position and use of such a catalyst is consequently the heat released by the combustion during the sulphided state for the hydrode of the second oxidation a lot of low nitration of contaminated hydrocarbon oils ger. Nevertheless, heat is suitable in oxidizing the nickel, but in either oxidized or non-reducing form. In the case of nickel-molybdenum-alumina catalysts with tem condition relatively inactive for this reaction with a high metal content, the catalyst temperature should be.
therefore initially below 510 ⁰ C and preferably at 288 20.

up to 399 ° C. B e 1 s ρ 1 e 1 1

In the final stage of the invention, the catalyst is impregnated by preformed 0.317 cm

sulfided. This can be achieved in a number of ways. B. H ₂ S, mixtures of water molybdate, calcining, renewed impregnation with Amstoff and H ₂ S and mixtures of hydrogen and monium molybdate and calcining, a catalytic organic sulfur compounds, brought into contact, sator produced. An oxide catalyst was produced which, under the conditions used, can be reduced to H ₂ S - 20.5% molybdenum (expressed as metal) and 6.4%. The catalyst temperature is currency nickel (expressed as metal) being contained on a trend in the Sulfidierens below 455 ⁰ C and preferably 30 borrowed from existing alumina carrier. The kept below 399 ⁰ C. During the sulphidation, the catalyst was not desired in the form of three dormant reductions to the metal. The best beds are introduced into the reaction vessel, and results can then be achieved if the liquid distributor tray catalyst with a mixture of hydrogen and oil was located between the layers. Thereafter, the catalyst was sulfided, a vaporizing organic sulfur compound 35 where one mehdung hydrogen with 1% dimethyl disulfide, such as. B. dimethyl sulfide, isopropyl mercaptan, rere hours at about 232 ° C through the reaction carbon disulfide, etc., at 232 to 343 ° C in contact vessel in the circuit and more than that to Umbringt. The sulfur compound is preferably dissolved in the conversion of all nickel and molybdenum oxides in a light paraffinic solvent, the metal sulfides required theoretical amount of di- and introduced into the circulating hydrogen. Methyl disulfide was added. The effectiveness of the freshly used an excess of the sulphidating agent in order to provide the catalyst was determined by ensuring that an essentially complete conversion of a light cycle oil with a boiling range of nickel oxide to nickel sulphide was achieved. between 204 and 315 ° C and a nitrogen content

All four stages of the invention are preferred from 775 T. p. M. at a temperature of 34O ⁰ C, as carried out when the catalyst is within 45 to a pressure of 56 kg / cm ² and a Raumgeschwinder reaction chamber is in which he normally speed of 1 volume of oil per volume of catalyst for the treatment of hydrocarbon oils is used per hour with the catalyst and with circulating. The nickel sulfide-molybdenum sulfide clays and hydrogen in an amount of 0.094 m ³ in burial catalysts are therefore usually brought into shape. After washing with water and one or more dormant catalyst cleanups, the contact oil contained 0.7 parts p. The ability to use nitrogen in the experimental conditions through which the hydrogen and that to be treated to remove to this extent were referred to as delnding oil to be passed. The hydrogen cycle 100% effectiveness. The above-mentioned catalyst is separated from the outflowing material in a high pressure separator for the hydrotreatment of various carbon pressure separators and returned to the reaction vessel through a gas cycle hydrogen oil between light naphthas and carbon dioxide system. After ren gas oils used, the 200 to 4000 ppm stickder the termination of the flow of hydrogen and oil substance contained, with various conditions from after the deactivation of the catalyst one can the 315 to 427 ° C, 56 to 77 kg / cm ² and 0.3 until 7 through-oxidation, reduction, oxidation and sulphidation rate per hour were used, carry out the stages of the present invention removed so that it finds, using a large part of the devices at operating conditions of 371 ⁰ C, 56 kg / cm ² pressure for handling the cycle gas (since and a space velocity of 1 volume per volume per preferably increased pressure in all stages Hour the nitrogen content of the light) as well as the high pressure separator for washing 65 cycle oil only down to 12 ppm nitrogen with water or lye during the oxidation stages. As a result, had the effectiveness (especially for removing SO ₂ ). The four steps to about 30% of its effectiveness in the fresh state do not necessarily have to be consecutive without undone.

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Attempts to sample the deactivated catalyst equaled or slightly better than the fresh catalyst

from Example 1 by conventional procedures with water.

steam — to regenerate air at temperatures above 455 ° C. The following example illustrates the invention in the

were unsuccessful. Activation of the regenerated catalyst from the

The following example describes a modified 5 game 3.

Water vapor air regeneration that is proportionate. · \ Λ

showed better results. example

Some of the oxidized in Example 3, however, not

Example 2 re-sulfided catalyst was thereby continued

ίο oxidizes that it is treated with a nitrogen-air device

A larger part of the coked catalyst from the mix at 42 kg / cm ² using essentially Example 1 was regenerated on the spot using the same temperatures and procedures as in the Beiman a water vapor-air mixture containing l% acid game 3 brought in contact. Thereafter, the oxidized substance was contained, at 0.14 to 0.35 kg / cm ^a and with a catalytic converter through contact with hydrogen, namely catalyst temperature between 288 and 371 ° C for the 15 2 hours at 42 kg / cm ² , 204 ° C, 16 hours at 232 ° C passed catalyst beds until the combustion and 8 hours gradual increase from 232 to voltage wave or the temperature rise ^{reduced the reaction 483 D} C, until it was certain that the nickel oxide had completely run through in the vessel. Thereafter, the essential to nickel metal (and molybdenum oxide to steam-air inlet temperature was increased by which Ka-molybdenum) was reduced. Thereafter, the catalytic converter temperature was maintained between 371 and 427 ° C using the method described in Example 3 while a second combustion wave was re-oxidized by the process and then moved like a reaction vessel. The temperature in Example 3 was then sulfided again. The effectiveness of the door increased to 483 ⁰ C, and the oxygen content of the catalyst was examined, and it was found that it was increased to 5%, but no further comparison was 120% compared to the fresh catalyst was, incineration instead, indicating that the catalyst was completely regenerated. Thereafter, the catalyst was not only regenerated but even tor cooled and activated using a mixture.

of isopropyl mercaptan in hydrogen in the case of a Ka- As mentioned above, the renewed oxy-

catalyst temperature between 204 and 343 ⁰ C again dation before sulfiding, after oxidation and

sulfided. Subsequently, the effectiveness of the 30 reduction became an essential stage. This is in the

The catalyst was examined and found only about 90% of the following example shown.

Effectiveness of a catalyst when fresh. . .

The e 1 s ρ 1 e ι regenerated according to the description in Example 2

Catalyst was again used for the treatment of In a parallel operation for example 4

Hydrocarbon oils as used in Example 1, 35 a portion of the regenerated unsulfided catalyst

until its effectiveness again to about 30 ⁰ / o of the active from Example 3 at the temperature conditions from

the efficiency of the fresh catalyst had decreased. Since Example 3 is oxidized, then using

after the catalyst was heated by a process of gradually increasing hydrogen from 204 to 483 ° C.

which reduces the better results than the method of low temperatures and then diverges

Example 2 shows and is described in the following example directly with dimethyl disulfide in hydrogen at 232 bis

will practice. 343 ° C sulfided. It was found that the catalyst

Example 3 ^{sator only} ^ ⁵ ° ^ ° ^{so a} ' ^ct ' ^vw * ^e ^ ^he ^ " ^{scne was} catalyst.

The omission of the new oxidation stage resulted

So nitrogen gave poor results at a pressure of 42 kg / cm ^2.

passed through the reaction vessel in which the coked 45 was contained in a sulfur-active nickel sulfide-molybdenum catalyst. Air was added so the high-median sulfide-alumina hydrogenation catalyst had 1% O2 ^{at the} inlet of the reaction vessel, aimed only once or twice for hydrogenation, where the nitrogen-air mixture had a temperature in hydrocarbon oils contained nitrogen content of about 315 ° C, the maximum catalyzer impurities were used, caused a satortemperature to regulate between 315 and 385 ° C, 50 mere regeneration by the process from the moment the first combustion wave through the game 3 itself an activation especially when the action vessel is moving. Thereafter, the nitrogen was increased, the maximum temperature during the oxidation in air-inlet temperature is limited to the catalyst under 455 ⁰ C,
keep temperature between 371 and 427 ° C as soon as. · \ E.
the second wave of combustion through the reaction 55 e 1 s ρ 1 e
vessel ran. When the temperature was increased to 483 ° C. Some of the coked prepared according to Example 1 and the oxygen content increased to 5%, no catalyst was found using the further combustion. During the entire process described in re-game 3, the cycle nitrogen was regenerated and sulphurized with a and then alternately first brought into contact with the caustic solution at around 65 ° C in order to use SO ₂ 60 for the hydrogen treatment of coal and CO ₂ To remove gas before it is returned to the reaction vessel in the case of accelerated coking conditions in the circulating hydrogen oils. At temperatures of 410 ° C. and 56 kg / cm ² during a period following the continuous addition of air to the system, which was closed for about 50 hours or until the system was effectively closed, the pressure rose to about 20% of the activity of the system during the retreat fresh Kageneration gradually to 63 kg / cm ² . Thereafter, the catalyst and then the regeneration and the catalyst were cooled and ^{renewed sulfidation at 42 kg / cm 2} under the conditions of the bisulfidation. When examining the effectiveness of the game 3 exposed, again for hydrogen treatment regenerated catalyst, it was found that they used that, regenerated and sulfided again. While

809 647/1951

Claims (3)

9 10 During the regeneration, a single flow of sulphidation was carried out, the catalyst can be reduced, nitrogen-air was used, these operations finally re-oxidizing and then sulphiding according to the invention carried out in a laboratory test facility. It was found that the regeneration of the Katawar As the following example shows, the process talysators can increasingly less effective 5 also for the activation of a fresh sulfided Katawar. While the catalyst used after the first catalyst was generated around 15% more active than the fresh catalyst, after the fifth regeneration in Example 9 it had only 53% of the activity of the fresh catalyst. A freshly calcined catalyst containing about 6% Ni. To ensure that all coke deposits _{contained 10% and} about 20% Mo on alumina, sulphate was removed, the catalyst, regenerated five times, was cata- fidated and then for 5 hours at 42 kg / cm ² with a analyzer again and again oxidized sulfided as oxidized in a mixture of dry nitrogen and air, the example 3. the activity was contained only up to about 70% 0.5% O _2, at 315 ⁰ C. The Katalysader the fresh catalyst activity improved torhöchsttemperatur was short time 382 ° C. The following example shows the 15 oxidation according to the invention was completed with the deactivated a 1% O ₂ in nitrogen at 483 ⁰ C for the reactivation operation. Thereafter the catalyst was at 42 kg / catalyst. cm ² with hydrogen at 232 ^° C. for 9 hours and in example 7 483 ^° C. for 7 hours. Then the Catalyst at 42 kg / cm ² with 0.5% O ₂ in nitrogen The deactivated sulfided catalyst from 20 483 ⁰ C and finally with 4% O ₂ at 483 ° C again oxyspiel 6, which dated only 70% of the activity in the fresh state. Lastly, the catalyst that had been used was sulphided at 42 kg / cm ² in the case of the corresponding steps im of dimethyl disulphide in H _2. Example 4 described temperature conditions oxy- Thereafter, the catalyst was converted to hydrogen, reduced, re-oxidized and sulfided. Thereafter, conversion of a heavy gas oil tested the activity of the catalyst with a loading Siedebewurde and 25 used ranging from 294 to 516 ⁰ C, the p T. 510. M. carried 105% of the fresh catalyst. Contained nitrogen. With treatment conditions of instead of regeneration, the reactivation 365 ⁰ C, an H ₂ partial pressure of 94.5 kg / cm ² , an approximation method of the present invention can be used repeatedly liquid hourly space velocity per hour of 0.5 and with better results, such as from the example below and a hydrogen cycle of 0.094 cbm / hl of oil. 30 the product oil contained 0.3 ppm nitrogen. Another portion of the fresh calcined catalyst was merely sulfided (by the preferred method) Coking conditions were used, 35 of 0.5, 0.094 cbm H ₂ / hl and 94.5 kg / cm ² H _{2 used} until its activity was reduced to about 20% of the activity in fri-det. A temperature of 377 ° C was required to produce Thereafter, the product nitrogen content was lowered to 0.3 ppm, the catalyst according to the present invention as in and a larger part of the oil was hydrocracked to light products by oxidizing, reducing, oxidizing It has been found that the catalyst deactivates by coke formation much more quickly than the activity of catalyst 11 5% of the activity of the at 365 ° C. The procedure can be carried out according to fresh catalyst. therefore greatly improve when the catalyst activated according to the pre-The reactivated catalyst of Examples was used in the present invention, every relation as good as or better than the fresh one in terms of the effect of the pressure during the prepared catalyst, and it kept the higher Ak - 45 different stages of the process have been experimentally active during a long period of use for the water at normal pressure, 42 kg / cm ² and 84 kg / cm ² carbonization of hydrocarbon oils. That led. It turns out that increased pressure during the reactivation process can therefore repeatedly reduce step is important in order to use the greatest possible, in order to achieve the lifetime of a catalyst improvement activity. If used, the sending should be extended for a very long time. 50 of a circulated nitrogen-air mixture. The present invention can also be used to acti- is increased pressure during the oxidation, especially for the activation of a fresh catalyst, in order to accelerate the oxidation and reduce the temperature. This is particularly advantageous in the case of facilitating the _{removal of SO 2} and H _{2 O from nickel.} Molybdenum-alumina catalysts, since the rate of deactivation by coking is 55 Application of the catalysts for hydrodenitriding claims: mainly depends on the temperature at the beginning of the operation, which is required to activate the embroidery 1. Procedure for activation and regeneration to reduce the substance content to the desired value. There- one of nickel sulfide or nickel sulfide-molybdenum-sulphide, that this starting temperature by also 60 fid-containing hydrogenation catalyst with honur A few degrees Celsius can lower the hem metal content, which is more than 10 percent by weight Extend the duration of the operation just as much as sulfur in combination with nickel or nickel. if you had the operation with a 15 to 20% molybdenum on a heat-resistant oxide carrier more active catalyst started. contains, characterized in that In the activation process, the last CaI can be used to convert the catalyst Finishing stage in the catalyst manufacturing process of the nickel and molybdenum components in nickel die first oxidation stage of the present invention and molybdenum oxide with a combustion be. Instead of this oxidized catalyst directly to be maintained gas at temperatures between Treated 288 and 510 ° C and increased pressure, then to convert the nickel oxide into nickel at elevated temperatures below 538 ° C with a hydrogen-containing, reducing gas under increased pressure, then again with a combustion-maintaining gas, preferably under the conditions the first stage of oxidation treated nickel in nickel oxide to convert, and it sulphided catalyst at elevated temperatures below 455 ⁰ C again. 2. The method according to claim 1, characterized in that a nitrogen-air mixture at a pressure above 14 kg / cm ^{2 is} used for the oxidation. 3. The method according to claim 1, characterized in that the sulfidation with a sulfidizing gas, such as H ₂ S, mixtures of H ₂ S and hydrogen or mixtures of hydrogen and organic sulfur compounds which can be _{reduced to H 2} S, at a Catalyst temperature below 399 ⁰ C performs.