BE506081A - - Google Patents

Description

       

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  -PROCEDE AND APPARATUS'D SHYDRGFORM ATION.



   The present invention relates to the catalytic conversion of hydrocarbon fractions boiling within the boiling limits of low explosive power engine fuels into high octane engine fuels, the invention relates especially to a method and apparatus whereby such a conversion is accomplished by the fluidized solids technique.



   Catalytic cracking of hydrocarbon oils by the fluidized solids technique is a well known and widely practiced process today. In such cracking processes, the conversion as well as the revivification or regeneration of the catalyst is carried out substantially at atmospheric pressure. In addition, the deactivation and regeneration of the cracking catalysts does not produce any significant change in the chemical nature of the components of the catalyst. catalyst.



   It has generally been suggested, in numerous patents specifically relating to catalytic cracking by the fluidified solids technique, that the process developed is applicable to other catalytic conversions comprising the reformation or hydroforming (hydroforming) of the fluid. naphtha or boiling hydrocarbon fractions., in the boiling range of motor fuels. Fluid hydroformation, if properly conducted, would have several fundamental advantages over fixed bed hydroformation of heavy native naphtha for the improvement of octaneo number A partial list of the advantages of operating with solid fluids dified for hydroformation is given below:

   
1 operations are continuous
2 vessels and equipment can be designed for one rather than two functions,
3 the reactor temperature is constant and reproduces the

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 isothermal fixed bed operating conditions
4 Regeneration is easily controlled or regulated.



   When we tried to achieve, using the solids technique
 EMI2.1
 Fluidized, hydroforming of boiling petroleum fractions in the range of motor fuels, many problems peculiar to this process have been found to be raised. First, the hydroforming is carried out at an elevated pressure of about 100 to 500 pounds per square inch rather than atmospheric pressure, which raises several problems.
 EMI2.2
 Second, the regeneration of the catalyst particles deactivated by carbonaceous deposits, through the removal by burning of the latter!} Brings about a change in the chemical nature of the composition of the catalyst.



  In the case of catalysts containing molybdenum oxide, the removal by burning of carbonaceous deposits on the spent catalyst can oxidize the catalytically active form to a relatively inactive form. When such
 EMI2.3
 regenerated catalyst is contacted with a hydrogen-containing gas such as process gas) in a similar gas, the inactive form is covered in an active form by an exothermic reaction which, especially under pressure and at the temperature establishing in the reaction system, is difficult to control or regulate and can lead to permanent deactivation of the catalyst.



   An object of the invention is to provide a method by
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 to which hydrocarbon fractions boiling in the boiling range of engine fuels can be hydroformed using the fluidized solids technique.



   It is also another object of the present invention to provide a reaction apparatus or system in which hydro = fractions.
 EMI2.5
 Carbides boiling within the boiling limits of engine fuels can be hydroformed using the fluidized solids technique.



   These objects of the invention and others will emerge more clearly from the detailed description and from the following claims.



   Figures 1 and 1 show schematically a planned system
 EMI2.6
 for the hydroforming of hyda-ocarb es9 fractions boiling in the bn.l.litin limits of engine fuels ($) using the fluidized solids technique according to the present invention.



  The stirring or filler material ,,, which may be a native naphtha, a fractionated naphtha, a Fischer-Tropsch naphtha or the like, is introduced through a line 11, a pump 12 and a line 13 into.
 EMI2.7
 a 7.1s preheater. (figure la) in which it is subjected to an indirect heat exchange with hot vapors of the reaction product. The preheated feed material is then passed through line 15 to a combination furnace 16 where it is heated to substantially the reaction temperature.

   The preheated charge material is then conducted
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 through a pipe 17 at the base of a large reactor 18, above a grid 18ao. The feed material is preferably admitted through a series of tubes or nozzles, as shown, in the lower part of the flow bed. catalyst 19 which will be described later.
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  The reactor is charged with a mass of the finely divided hydroforming catalyst above the 18ao grid. Suitable catalysts include oxides of Group VI metals, such as oxides of molybdenum, chromium or tungsten. or mixtures thereof, provided on a support such as activated alumina, zinc aluminate spinel or the like. Other catalysts or ingredients can be used. The catalyst particles are, for the most part, of sizes between 200 and 400 meshes or about 0 to 200 microns in diameter with a substantial proportion of between 20 and 80 microns.

   A stream of hot gas containing hydrogen and having the catalyst in suspension is introduced at the base of the reaction.

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   tor below the grid 18a which serves to distribute the catalyst and gas evenly over the entire section of the reactor. By priming
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 the process for the first time the gas containing hydrogen can be supplied from a foreign source. The process, however, normally develops hydrogen which can be recycled to the reactor.

   The naphtha vapors and the hydrogen-containing gas are passed, as a mixture, upwardly through the reaction zone at a superficial velocity.
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 about 0.2 to 0.9 feet per second at reactor conditions depending on the pressure. For example, the speed should be less than 0.6 feet per second in the pressure range of 200 to 250 pounds per square inch.
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  The velocity should be sufficient to maintain a dense, turbulent liquid-like bed of solids and gases at a level with, above, an increase of gases and solids in the dilute phase. The lower linear gas velocities are used at higher pressures to obtain dense fluidized beds.

   If desired, the reactor 18 may be provided with perforated baffles arranged horizontally and spaced vertically, or with baffles arranged vertically and
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 spaced apart, to improve the contact between the hydrocarbon vapors and the catalyst A vertical interior duct 21 is provided in the reactor 18,
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 for catalyst removal, directly from dense bed 190 The upper end of conduit 21 extends above level 20 and has apertures or lumens 21 'at one or more points along its length to allow entry of the conduit. catalyst in line from bed
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 dense As the catalyst and the hydrocarbons are introduced at the lower end of the reactor 18,

   that product vapors are removed at the top and that catalysis is removed near the top of the bed of
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 catalyst 19, there is a general concurrent displacement of d9lyd carbide vapors and catalyst in reactor 180. Lumen 219 may be located in the upper part of bed 19, in order to achieve maximum concurrent displacement of catalyst and vapor. oil up
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 through bed 190 However, light 219 should be sufficiently below level 20 to account for any normal fluctuations in level 20.

   More than one orifice, or lumen, may be provided at different levels in conduit 21, and each lumen may be provided with valves to control the flow of catalyst in conduit 21.



   Steam or an inert gas, such as nitrogen, flue gas or the like, or mixtures of these gases are sent into the duct 21 through a duct 22 near the base of this duct 21 for expelling or removing. - lift hydrogen, hydrocarbon reactants or reaction products
 EMI3.9
 flowing in the pipe 21 at the same time as the catalyst, the stripping gas or p: # i ± 'i @ ation being led upwards in the pipe 21p against = -current with respect to the catalyst later. The superficial velocity of the stripping gas should be equal to or greater than the superficial velocity of the vapors and gases which flow upward through the reactor 18.



   The stripping or cleaning gas and removed components are discharged at the top of line 21 into dilute phase 20 'and are combined with vapors of the reaction product leaving dense bed 19; the mixture is passed through a or more cyclone separators 21a or
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 Similar for the removal of the entrained catalyst particles and then the mixture is discharged through line 23 to suitable equipment described below for heat and product recovery.
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  Catalyst cleaning decreases the amount of combustible material which must be burnt off during catalyst regeneration as will be discussed later. If desired, the separate outer cleaning vessel can be used for the cleaning or purification phase of the catalyst, the cleaning gas and the removed materials leaving the system.
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 cleaning agent being taken to the outlet 23 of the reactor or being treated separately for the recovery of hydrocarbons.

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   The lower end of the duct 21 is of decreasing diameter as in 23a and forms a vertical pipe 23b having a diameter smaller than that of the duct 21. This pipe serves to develop an additional pressure necessary to overcome the pressure drop at through the regeneration system. The catalyst flowing from the large section 21 into the reduced section 23b will carry a sufficient amount of entrained gas to be maintained in a free flowing fluid state, and this state should be maintained during the passage of the catalyst through. the channel
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 reduced cross-sectional area 23b. If necessary, gas addition can be made at one or more gap points in section 23b.

   However
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 However, as the process is carried out under a high pressure of 100 pounds per square inch or even higher which is much greater than the pressure drop across the regeneration system 1 - the amount of pressure rising through the pipeline is relatively low compared to the process pressure $ therefore there is less compression.
 EMI4.3
 dre of gas entering the top of section 23b as the solids move downward, so that in most cases there is no need to add additional gas aerator in section 23bo. This is particularly correct if in section 23bj) the downward flow rate of the solids in the pipeline is relatively high,

   so as to prevent deaeration of the catalyst. By making the diameter of the line relatively small relative to the cleaning section, the velocity in the section of the line will increase, thereby reducing the tendency for the catalyst to deaerate.



   Line 23b is provided at its lower end with a valve 23c to control the rate of removal of the cleaned catalyst exiting the line.
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  The catalyst, at the base of line 23bd) is discharged into line 24, in which it is carried by a stream of air or other carrier gas supplied by line 25, and is carried to the regenerator. 26 where carbonaceous deposits on the catalyst are burnt off. It has been found that the rate of burning of carbonaceous deposits starting from the catalysts
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 Hdrfoaati sors of the type described is much faster than the rate at which carbonaceous deposits burn off from the conventional cracking catalyst, such as silica-alumina gel. Rapid catalyst burning can cause the catalyst to overheat as it passes through line 24 unless special precautions are taken.

   This can be avoided by introducing some or all of the air for regeneration,
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 separate line to the regenerator, and using only part of the air for regeneration or an inert gas for transporting the catalyst in line 24 to the regenerator. About 15-40% of the total air required for regeneration can be used for trans-
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 carry the cleaned spent catalyst to the regenerator without overheating the catalyst. The remainder of the air, or about 60 to 85% of this air, can be sent directly to the regenerator through line 27.

   Both lines 24 and 27 discharge into regenerator 26 below a grid element 27ao Although line 27 is shown having a single outlet opening in the regenerator, it will be understood that this line can be extended above. of the grid 27a in the regenerator and
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 provided with a series of openings, at vertically spaced points inside the regenerator, to provide temperature uniformity in the mass of catalyst undergoing regeneration.

   
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 The velocity of gas passing from bottom to top through the regenerator is controlled to maintain a dense, highly turbulent lower fluidized bed 27 'and an upper dilute suspension of catalyst and gas, at a level or line of. 27bo separation To achieve this, the superficial velocity of the regeneration gas in the regenerator 26
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 may be on the order of 0.03 to 1.5 feet per second depending on the pressure, eg, less than 1 foot at a regeneration pressure of about 200 to 250 pounds per square inch. The conduit 28 extends through the dense bed 27 'of catalyst and passes through the grid 27a and the base of the regenerator.

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 26.

   The regenerated catalyst is discharged from the regenerator through line 28 having a large amount of cleaning management in the vessel and a reduced compartmentalization section 28b which is constructed and which functions in the same manner as lines 21 and 23b for the removal of waste. Catalyst Outside the Reactor The vertical line 28b is provided at its base with a valve 28a for controlling the rate of catalyst growth. The catalseut, from the base of the pipe 28b, is deeharge in a pipe 30 where it is carried away by hot recycle gas, which will be discussed later, to form a slurry, and @ elle = @! is introduced at the base of the reactor 18 under the grid 18a as previously described.



   When the freshly regenerated catalyst, which is at substantially the temperature and pressure of the regenerator, is contacted in line 30 with hydrogen or with recycle gas containing it.
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 With hydrogen, an exothermic reaction difficult to control resulted and this reaction can deactivate the catalyst unless special precautions are taken. This can be avoided by making the transport line 30 extremely short connecting the line 28b from the regenerator to the regenerator.
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 reactor 28p and maintaining a relatively dilute suspension of the catalyst in the gas within this line.



  By applying to the regenerated catalyst a limited treatment with the hydrogen-containing gas, before contacting with the naphtha vapors, the catalyst can be restored, to the desired valence so that the inactivity and selectivity of the catalyst can be better maintained. naked.



   Various manual or automatic control means can be used to maintain the desired operating conditions.



  One of these control means is shown in the drawing but the invention is not
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 not limited to this means. A level controller 28d is provided for the regenerator 26 to adjust the valve 28a in the line 28b. Temperature sensitive means 24a is placed in transfer line 24 and is connected to valve 23c in line 23b to adjust this pressure.
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 pope 23a.

   If for some reason the temperature rises in line 24, temperature sensitive means 24a will operate to open valve 23c, thereby allowing more catalyst to come from line. line 23b to enter line 24, and, as this catalyst from the reactor is cooler than during regeneration, the temperature in line 24 is reduced to the desired value o By introducing more catalyst into line 249 there is has a temporary rise in the level of catalyst in the regenerator,

     and the 28d level controller in action to
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 open the 2S @ s> valve to allow more catalyst removal from the regenerator to maintain the desired level.
The temperature control in the regeneration zone is influenced by cooling coils 31 arranged in the regenerator and in which a cooling medium circulates.



   An advantageous method of controlling bed temperatures in the regenerator is to have 60-75% of the stiffening area very close to the bottom of the lite. This section can be used to remove a fixed amount of heat at all times. . The remainder of the cooling surface is provided with a wider spacing, relative to the bed, at the top of the regenerator. Any desired part of this cooling surface can be submerged in the bed by raising or lowering the level of the dense bed in the regenerator.



  The drawing shows an installation in which the heat released in the
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 regenerator is used to produce steam. All the oerpentines should be tubes h # ides> @ ge # lt = to say that there would be a film of water on the part of the tubes with the temperature control being carried out by varying the amount of surface of the tube. submerged heat exchange

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 in the dense bed. The heat transfer coefficient of the dense bed is considerably higher than that of the dilute suspension above the bed.

   This arrangement is particularly effective in the present process since the regenerator contains a relatively small amount of catalyst compared to the reactors so that changes in level.
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 in the regenerator n% ffbct, not seriously set the level of the dense bed in the reactor. The temperature in the regenerator can be automatically
 EMI6.2
 cally regulated by operation of the valve 28o at the base of the conduit 28 intended to allow the change of the height of the lito
Regeneration gases are removed at the top of the regeneration.
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 21 through one or more oxygen separators 28c which remove entrained catalyst. The gas then passes through a pressure reduction valve 31 'and is sent to the boiler room through 32.

   In order to regulate the amount of catalyst in the system, special precautions are taken.
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 for the introduction and removal of the catalysis =, as noted below.



  Hot catalyst can be carried from the regenerated catalyst line 28b into line 33 with the removed catalyst passing through catalyst cooler 34. The catalyst pressure is then released.
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 in stages by passing it through fixed orifices 35. The decompressed catalyst is then discharged through a line 36 into the catalyst storage hopper 37.



   Fresh catalyst supplied in hopper cars or similar systems is discharged into a deposit pit 38, transferred to a conduit 39 by means of a propeller pump or similar device and taken to
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 The fresh catalyst storage hopper 40 is fed into the catalyst storage hopper 37 by an adequate gas flow. Cyclone separators (not shown) can be used to recover the catalyst from the gases leaving hoppers 37 and 40. This catalyst in the hoppers
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 Hoppers 37 and 40 is placed under adequate pressure to feed it into the system by the introduction of high pressure dry air through lines 41, 42 and 43.

   The catalyst to be added is removed from the hopper 37 or 40 and transported by high pressure air to a mixing tank 44 where. it is mixed with part of the naphtha feed introduced through line 45. The mixture of catalyst and naphtha is pumped by a pump 45 'into the reactor 18 via a control valve.
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 pressure 46 and through line 47. The mixture is preferably conveyed into the reactor above the grid 18a, through one or more
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 Its nozzles are similar to adding fresh feed to the reactor.

   Lines 49 and 50 connect the base of hoppers 40 and 37 to line 51 in which the catalyst for the initiation of the reaction.
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 tor is transported therein by a dry stream of gas (eg air) at high pressure.



   On returning again to reactor 18, the reaction products, as previously noted, are removed at the top of the reactor after passing through one or more cyclone separators which remove most of the entrained catalyst but not all of it.
 EMI6.11
 foîs these products then pass through line 23 to drum 52 (Figure la). Heavy cooling oil which may be formed during the process is introduced into line 23 through line 53.



  The amount of cooling oil introduced into the vapors should be sufficient to cool the vapors below the vaporization temperature of that oil. The resulting mixture comprises small oily droplets of gaseous and vaporous reaction products, together with a quantity of catalyst which is then fed tangentially into drum 52 or liquid droplets and the catalyst particles. are separated from the gases.



   Cooling oil has a higher boiling point than the naphtha feed and consists mainly of constituents
 EMI6.12
 or high boiling polymers formed during the hydrofoilization9 although a foreign oil is used at the start of the operation.

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 EMI7.1
 Oil and analyzer are removed from the base of the taabe'ar by a pump 54.9 A portion of this mixture is sent to a cooler 55 and then 'recycled through line 53 and injected into line 23. freshly.
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  The remaining portion of the mixture stream is removed by a
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 pipe 56p passed through a cooler cavity 57 and then introduced into a filter 58s> for 19 removal, of the catalyst qq part of 19hui =
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 the clarified forming the filtrate is sent through line 59 which joins line 53 to form a mixture with the cooling oil. The
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 filter 58 is periodically washed> in the reverse direction of eireulation, with naphtha d.9alimentati@ns> if it is desired to recover and reuse the catalyst. In this case, the mixture of catalyst and naphtha is sent through line 60 and line 47 into the reactor.

   If the catalyst should
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 to be removed it is washed with water with stirring and removed by
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 from 611. 1.9 clarified oil, in addition can be evacuated from the system by 599, it instead of the drum 52p a bubbling tower can be used for the removal of the entrained catalyst> out of the vaporsq and also for the cooling and there separation of polymer oil with a higher boiling point formed during the process,
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 The stream of gaseous and vaporous reaction products * is
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 removed at the top of the drum 52 by a pipe 62p and a part of this oo-orant can pass through the exchanger 14 for the preheating of the fresh naphtha feed, while another part can be sent to an exchanger. heat 63 for preheating the recy- cling gas containing l.9hyd:

  "genes> which he dealt with later.
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 partially cooled rant of gauze = and vaporous reaction products
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 is then sent through a pipe 65 to a eondeuseur 66 which serves to condense the hydroformate. The products coming from the condenser 66 pass into a receptacle 67 in which the liquid hydroformate separates from the gases -
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 not condensed. The liquid hydroformate is evacuated at the base of the separator 67 and sent through a line 68 to a stabilization or other installation (not shown). Non-sounding gases that contain a high percentage
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 Hydrogen percentages are removed at the top of separator 67 through conduit 69, passed through a separator drum 70 to remove any impeded liquid.

   The gas relatively liberated from liquid is then eompri = me in an a (ciflpresseur 71 and,!) From therep passed through a pipe 72 in the e-
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 heat changer 63 in which it is preheated by heat exchange
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 indirect with hot reaction products passing through line 62 as already discussed.

   The heated gas which is recycled in the process
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 die is then sent through coils 73 into furnace 16 in which the gas is heated sufficiently above reaction temperatures.
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 tion can provide the required heat in addition to and greater than, - it is heated by the regenerated hot and preheated catalyst o L-9 excess treatment gas from line 69 is evacuated by scnduite 69a
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 as tail gas
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 One method of starting and f'iQ) n (ti @ J1ilUlement of the reactor system according to the invention is as follows. Catalyst is transferred from storage hopper 37 or 40 to the reactor and regenerator by use line 51 by means of air current When the reactor and the regenerator are loaded with catalyst,

   Inert gas produced in inert gas generator 741 (Figure 1) is fed into the reactor system to purge it of 19aU-. Inert gas generated in gas generator 749 is compressed to the desired operating condition in a compressor,% sic3 ,,, x 74a and then sent to reactor 18 through line 74.

   At the same time, hot air which can be heated by the coils 73 of the furnace 16 during the start-up operation is sent into the regenerator until the temperature of the latter reaches approximately 800 Fo

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 After the removal of air from the reactor is complete
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 and that the regenerator is at around 800 F,

   the passage of air through furnace 16 is interrupted, oil is then burnt in the regenerator to further heat the catalyst and the catalyst circulation is reduced.
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 mencéeo Refinery fuel gas is sent to recycle gas circuits 73 and 74 to purge recycle heating coil 73 and is then used to transport catalyst from the base of the tank.
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 28b of the regenerator to the reactor 18 via a pipe 30.



  Catalyst circulation is continued until the reactor reaches about 850 Fo. When this is reached, the feed of naphtha begins.



   As soon as sufficient carbon is produced on the catalyser,
 EMI8.4
 which, by burning in the regenerator, is sufficient to maintain the heat balance the oil supply to the regenerator should be turned off; the feed rate of the naphtha is then gradually increased and the plant is brought to operating pressure.



   The naphtha feedstock, preferably a native naphtha, sent to the system has a range of boiling points varying from about
 EMI8.5
 175 to 4500FS! preferably from 200 to 350 F, is preheated by indirect heat exchange with the product vapors in exchanger 14 to about 500 - 600 F, and is then further heated in the combination furnace to.
 EMI8.6
 8000 - 1000OFe preferably about 950 Fo Preheating of the naphtha should be as high as possible, while avoiding thermal degradation of said naphtha, by limiting the residence time in the transfer line 270
Recycle gas, which should contain 50 to 70% by volume, preferably 60%,

   of hydrogen is preheated by indirect value exchange with the product vapors in a heat exchanger 63 to about
 EMI8.7
 600 F, and then further preheated in the combination oven to about 11; 00 - 12000F. preferably at about 11850F. The recycle gas is heated to this temperature to maintain the temperature of the reactor
 EMI8.8
 at about 900 F. Recycle gas should flow through the reactor at a rate of between 1000 and 4000, preferably 3000, cubic feet per barrel of feed.



  The reactor temperature should be between 850 and 25 F9 preferably 900 F $! and reactor pressure between 100 and 500 pounds per square inch., preferably 200 pounds per square inch
 EMI8.9
 Temperatures above 900 F, cause increased carbon formation and lower catalyst selectivity to gasoline fractions, while at temperatures below 900 F, operation is less severe and should therefore require rework. - excessively large reaction vessel Lowering the reactor pressure below 200 psi results in increased carbon formation which becomes excessive below
 EMI8.10
 d-9 'approximately 75 pounds per square inch.

   Above 200 pounds, however, the selectivity of the catalyst to light products (C4) increases rapidly.



   A particularly important factor in carrying out the procedure is the weight ratio of catalyst relative to the oil introduced into the reactor, or the rate of flow of the catalyst between the reactor and the regenerator relative to the reactor. speed
 EMI8.11
 oil supply. It is preferred to operate at a catalyst / oil ratio of 1 since ratios greater than 1 to 1.5 result in excessive carbon formation from the naphtha. Increased catalyst circulation speeds resulting from higher ratios
 EMI8.12
 catalyst / oil tends to entrain more hydrogen into the regenerator unless excessive removal is taken.
 EMI8.13
 executed.

   The hydrogen is so much better retained9 in a tenacious way, by the catalyst that the latter is transferred in large quantity of the

 <Desc / Clms Page number 9>

 
 EMI9.1
 reactor in the regenerator c Higher circulation speeds of the
 EMI9.2
 catalyst, not only increase the amount of naphtha converted to carbon but also considerably increase the cost of regeneration,
 EMI9.3
 increase in the amount of heat exchange surface necessary to remove heat ,, and 19 s.i:

  rë 'which must be compressed,
 EMI9.4
 Catalyst / oil ratios can be as low as -
 EMI9.5
 0.5 o If higher pressures, the catalyst / oil ratio may be increased, a 3/1 ratio suitable for pressure of about 500 pounds per square inch, Space velocity is defined as pounds of feed.
 EMI9.6
 per hour, per pound of catalyst in the reactor, This spa-
 EMI9.7
 in the reactor depends somewhat on the degree of age or activity
 EMI9.8
 tee of the catalyst. A space velocity for a mo- oxide catalyst
 EMI9.9
 lybdenum on an azmin gel can vary, for example, from about 1.5 wt / hour / wt (pound of feed / per pound of catalyst) to about 0> 15 depending on the activity of the catalyst. desired d90tan6 number of the product and the feeding characteristics.

   The temperature in the regenerator should be maintained between about 10500 and 1200oFo The following table summarizes the results obtained during the fone-
 EMI9.10
 operation, under a series of given conditions, according to the present invention Example
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 Feed material 200o = 430oF Heavy native naphtha m Gel type catalyst ss Operating conditions Reactor temperature, OF 900 Pressure at the top of the reactor 9
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<tb> pounds <SEP> per <SEP> inch <SEP> square <SEP> 200
<tb>
 
 EMI9.13
 Ratio @ atalysis / oil9 by weight 1.2 Space velocity9Pa! Ha! In 0927 Carbon on wall oatalysis regenerates-% by weight -of 0p05
 EMI9.14
 
<tb> <SEP> rate of <SEP> gas <SEP> of <SEP> recycling, <SEP> feet
<tb>
 
 EMI9.15
 - standard tubes per barrel of fresh feed 3575% H 2 in recycle gas 63,

  4 Gasoline production -% in 'al' # MS 83ç3 to 4 total -% in volumes' 05 total = '% GD volumes' Dry gas% at paldo 1396 Carbon% by weight 098 Hydrogen blade paddle acorn o /
 EMI9.16
 
<tb> barrel <SEP> feed <SEP> fresh <SEP> 602
<tb>
 
 EMI9.17
 InspectIong of 0, Gazoline ¯¯ IZ4 Reaheroe Octane Rating CFR = 96e5
 EMI9.18
 
<tb> clear
<tb>
 
 EMI9.19
 DPOctan index AoSaToMo = elair 85.4 M. Reid vapor pressure -l.p.poe, 9.3

 <Desc / Clms Page number 10>

 
 EMI10.1
 Severity = OAPI 5g,
 EMI10.2
 
<tb> <SEP> inspections of <SEP> the <SEP> material <SEP> feed
<tb>
 
 EMI10.3
 Severity = 0API 53j13 Octane number
 EMI10.4
 
<tb> Search <SEP> G3R <SEP> - <SEP> clear <SEP> 43
<tb>
 
 EMI10.5
 AoS.T.M.

   clear 38
 EMI10.6
 
<tb> Point <SEP> of aniline, <SEP> F <SEP> 128
<tb>
<tb> Sulfur <SEP> = <SEP>% <SEP> in <SEP> weight <SEP> 0.11
<tb>
 
 EMI10.7
 Aoboin Distillation
 EMI10.8
 
<tb> 10 <SEP>% <SEP> to <SEP> F <SEP> 252
<tb>
<tb> 50 <SEP>% <SEP> 282
<tb>
<tb>
<tb> 90 <SEP>% <SEP> 346
<tb>
<tb>
<tb>
<tb>
<tb> Analysis <SEP> of <SEP> type <SEP> of hydrocarbons <SEP> - <SEP>% <SEP> in <SEP> volume
<tb>
<tb>
<tb> Aromatics <SEP> 8
<tb>
<tb>
<tb> Paraffins <SEP> 48
<tb>
<tb>
<tb>
<tb> Naphthenes <SEP> 40
<tb>
<tb> Olefins <SEP> 0
<tb>
<tb>
<tb> <SEP> repository (not <SEP> analyzed) <SEP> 4
<tb>
 
 EMI10.9
 sag the catalyst containing approximately 8p5% of molybdenum trioxide on an alumine gel prepared by co-precipitating molybdenum oxide and alumina,

   Specifications for a fluid bdrfoation process will now be given for a business unit capable of processing 14,400 barrels of heavy native naphtha per running day. The reactor is a
 EMI10.10
 Cylindrical container, internally insulated, 18 feet in diameter and 85 feet high (right side dimension) The regenerator is a cylindrical container 7e5 feet in diameter and 25 feet (right side dimension) high with a refractory lining. In the regenerator. \! additional saddle heat used to provide warmth to the
 EMI10.11
 reactor is used to produce steam at 200 pounds per square inch.



   The naphtha feed is preheated in heat exchangers
 EMI10.12
 heat to about 575 F and then to about 9500P in the combination furnace The heated feed at a pressure of 100 to 500 pounds per square inch is then sent through line 17 to the base of the catalyst bed
 EMI10.13
 fluidized 19 in reactor 18. At this feed temperature, the flow of airflow through the pipe should be controlled to avoid thermal cracking and degradation. Conduit 17 has an internal diameter of 6 inches.

   The reactor is maintained at a temperature of
 EMI10.14
 About 9000F. The recycle gas is heated to a temperature of about 1185A The amount of recycle gas containing about 70 mol% hydrogen is about 300,000 standard cubic feet per minute. The thus heated recycle gas passing through line 74 is mixed with hot regenerated catalyst which is at a temperature of about 11500F and is discharged from line 28b, to form a dilute slurry which is sent through line 30 to the base of the reactor 18 under the grid 18a.

   The catalyst living time in transfer line 30 should be less.
 EMI10.15
 After 5 seconds, to avoid overheating and degradation of the catalyst before it comes into contact with the naphtha vapors in reactor 18. Line 30 is about 26 inches in diameter.

 <Desc / Clms Page number 11>

 



   The average residence time of the catalyst in the reactor can be on the order of 3 to 4 hours, while the residence time of the catalyst in the regenerator can be 3 to 15 minutes.



   The superficial velocity of the gas-like material moving upward in reactor 18 is about 0.5 feet per second and the
 EMI11.1
 The density of the fluidized bed 19 is about 30 pounds per cubic foot. The density of fluidized bed 27o in regenerator 28 is about 28 pounds per cubic foot. The regenerator is at a pressure of about 205 pounds per square inch and a temperature of about 11500P.



  The product vapors exit the top of the reactor 18 into
 EMI11.2
 a pipe 23 at a temperature of about 900oF are cooled to about 800F by cooling oil introduced at an in-
 EMI11.3
 about 5000P at 54. The product vapors are then cooled to below about 1050F to separate the hydroformat product from the recycle gas. Approximately 130,250 barrels of crude hydrochloride will be produced per normal day.



  The)] 'M: ttOYi, # 21 conduit in reactor 18 has a diameter of about 2 feet and at its base is reduced to a 7 inch tube to form a 23bo duct. of line 23b is about 25 ftso Superheated steam is introduced to the base of cleaning line 21 at the rate of about 2940 pounds per hour.

   Most of this vapor is directed upward through the cleaner
 EMI11.4
 219 counter-current with respect to the descending catalyst but a certain quantity of vapor and gas is carried away in the catalyst which moves in the pipe 23bo
The cleaner duct 28 in the regenerator 26 is about 2 feet in diameter and at its base is reduced to a diameter of about 7 inches.
 EMI11.5
 these to form a pipe 28b. The effective line height of 28b is approximately 50 feet. The amount of inert gas used for cleaning line 28 in the regenerator is 4900 pounds per hour.



   Line 24 leading from line 23b to regenerator 26 is about 8 inches in diameter and line 27 is about 4 inches in diameter.



   For the installation described, about 260 tonnes of catalyst will be needed and about 250 tonnes will be in the reactor., About 9 tonnes will be in the regenerator and the rest will be in the reactor.
 EMI11.6
 in lines leading to and from the reotor and regenerator. The density of the catalyst mixture in lines 23b and 28b is about 44 pounds per cubic foot but can be about 38 to 44 pounds per cubic foot.



    CLAIMS.
 EMI11.7
 



  == d ===================== 1. Processed for converting naphtha into an engine fuel with high anti-knock power by hydroformation comprising the passage of naphtha vapors in combination with hot process gas containing 1-hydrogen through a dense fluidized bed of finely divided hydroforming catalyst in a reaction zone at a temperature of 850 F -
 EMI11.8
 925 F and a pressure of 100-500 pounds per square inch at a ratio of ca- ta1ye'IW / oil by weight ojs to the removal of the stream of reaction products substantially liberated from catalyst at the top of the zone of. reaction 1 (removing a stream of catalysis particles directly from the dense fluidized bed in said reaction zone (Pe))

  The removal of the adsorbed hydrocarbon material from the catalyst stream - the regeneration of the cleaned catalyst particles, by burning the carbonaceous deposits in a dense fluidized bed in a regeneration atom9 the adjustment of the

 <Desc / Clms Page number 12>

 
 EMI12.1
 temperature of the catalyst undergoing regeneration to less than about 1200oF Removal of catalyst particles from the regeneration zone and their
 EMI12.2
 recycling to the reaction zone separating entrained residual catalysis material with the reaction product stream passing through
 EMI12.3
 19 a7.iyaatatia in fresh naphtha in indirect heat exchange compared
 EMI12.4
 with the curant of reaction products to remove a certain quantity of
 EMI12.5
 heat 3 another heating of naphtha naphtha

  preheated to 800oF = 1000oF prior to introducing this feed to the reaction zone = further cooling of the reaction product stream to condense the hydroformate separation of the hydroformate from the reaction products
 EMI12.6
 gaseous or process gas and heating these to
 EMI12.7
 temperatures of 1150 00F and their recycling to the reaction zone.

   
 EMI12.8
 20 Process for converting fractions of naphtha into gasoline
 EMI12.9
 high anti-knock power including the passage of hydrocarbon materials
 EMI12.10
 vaporized in combination with hot process gas containing hy-
 EMI12.11
 drogen, through a dense fluidized bed of lover hydroformation catalyst divided into a reaction zone in the ratio of 1000 to 4000 cubic feet per barrel of naphtha feed at a temperature of 850OF-9250F and a pressure of 100-500 pounds per. square inch at 0.5 to 3 catalyst / oil ratio, and 0915 to 1.5 space velocity (pounds of hydrocarbon feed per hour per pound of catalyst) - 19 removal of fuel.

  9a stream of reaction products substantially liberated from catalyst at the top of said reaction zone the removal of a stream
 EMI12.12
 of catalyst particles directly from the dense fluidized bed in said
 EMI12.13
 reaotîonµ the removal of the adsorbed hydrocarbon material,
 EMI12.14
 catalyst stream the regeneration of the cleaned catalyst particles by burning carbonaceous deposits in a dense fluidized bed in a regeneration zone, the temperature control of the catalyst being subjected to the
 EMI12.15
 regeneration,

   less than about 1200] removing catalyst particles from the regeneration zone and recycling them to the reaction zone separating entrained residual catalysis material from the reaction product stream $ the passage of 19a1iMntation in naphtha
 EMI12.16
 charge in indirect heat exchange to the reaction product stream to remove a certain amount of heat out of said
 EMI12.17
 reaction products further heating of the naphtha feed preheated to 800 = 1000 before it is introduced into the reaction zone
 EMI12.18
 further cooling of the reaction product stream to condense
 EMI12.19
 l9hdraoratq the separation of lnhyd o,

  arat gaseous reaction products or process gas9 heating this gas to a temperature of 1150 = 100 "and recycling it to the reaction zone.



  3. Process for converting fractions of hydrocarbons boiling in the range of combustion of engine fuels> into fuels
 EMI12.20
 engines with high anti-knock power including the passage of vaporized hydro-carbonated materials in combination with hot process gas
 EMI12.21
 containing PbyaF6gene passes through a dense fluidized bed of finely divided hydroformatioD catalyst,

   in a reaction zone at a temperature of 8500 = 9250F and a pressure of 100-500 pounds per square inch a catalyst / oil ratio of 095 to 33 is obtained.
 EMI12.22
 reaction products substantially liberated of catalyst at the top of the zone
 EMI12.23
 Reaotion The removal of a stream of catalyst particles directly from the dense fluidized bed into said reaction zone to release the adsorbed hydrocarbon material.

   of the catalyst stream
 EMI12.24
 transport of the catalyst stream to a regeneration zone with at least
 EMI12.25
 plus about 40% of the total air required for regeneration 1-'addî-
 EMI12.26
 tion of the rest of the regeneration air directly to the regeneration zone.
 EMI12.27
 tiaa9 the temperature control of the catalyst undergoing regeneration less than about 9200oFJ '19 removal of the catalyst parts from the
 EMI12.28
 regeneration zone and their recycling to the reaction zone the separation of the residual catalysis material entrained with the stream of
 EMI12.29
 reaction produced by the passage of the fresh hydrocarbon feed
 EMI12.30
 in indirect heat exchange with respect to the stream of reaction products

 <Desc / Clms Page number 13>

 yours to remove a certain amount

  heat% another blackmail
 EMI13.1
 of the preheated hydro-fuel feed, to 001000 before introducing this feed into the reaction zone, further cooling of the reaction product stream to condense the hydrofoil and the separation of 1 brdfmat from the gaseous reaction products or the reaction gas. treating and heating these to temperatures of 1150-1200 F and recycling them to the reaction zone.

   fla Process for converting hydrocarbon fractions boiling in the starting range of engine combiatibles, into engine fuels with high anti-knock power comprising ,. the passage of hy-
 EMI13.2
 drooarburized vaporized in combination with hot process gas containing hydrogen, through a dense fluidized bed of hydrogen catalyst.
 EMI13.3
 Finely divided formation in a reaction zone in the ratio of 1000 to 4000 cubic feet per barrel of hydrocarbon feed at a temperature of 850 = 925F and at a pressure of 100-500 pounds per square inch at a catalyst / oil ratio from 0.5 to 3 and at a space speed of 0.15
 EMI13.4
 at 1.5 (pounds of hydrocarbon feed per hour per pound of catalyst)

   19 removing a stream of substantially liberated reaction products of catalyst at the top of said reaction zone 9- 19 removing a stream of catalyst particles directly from the dense fluidized bed in said reaction zone # 9 19 removing adsorbed hydrocarbon material from the stream catalyst transporting the catalyst stream to a regeneration zone with at most about 40% of the total air required to
 EMI13.5
 regeneration9 adding the remainder of the regeneration air directly to the regeneration zone adjusting the temperature of the catalyst undergoing regeneration? less than about 1200 F;

  removing the catalyst particles from the regeneration zone and recycling them to the reaction zone; the separation of the residual catalysis material into
 EMI13.6
 dragging with the reaction product stream the passage of fresh hydrocarbon feed in indirect heat exchange to the reaction product stream to remove heat therefrom;

   another heating of the preheated hydrocarbon feed,
 EMI13.7
 at 8000 = 10000F before 19 iat d.tia of this feed in the reaction zone further cooling of the reaction product stream to condense 19hydroformatp the separation of 1Phydroformat from the gaseous reaction products or the process gas and heating of the latter at
 EMI13.8
 temperatures of l150 -1200 P and their recycling to the reaction zone.



   5.Process for converting hydro-fuel fractions boiling in the boiling range of engine fuels, into engine fuels with high anti-knock power, comprising:
 EMI13.9
 vaporized hydrocarbon materials in combination with hot process gas containing hydrogen,

   through a dense fluidized bed of finely divided hydroformation catalyst in a reaction zone at a temperature of 850 '= 925 ° F' and at a pressure of 100 = 500 pounds per square inch at a catalyst / oil ratio of 095 to 3 removal d-a stream of reaction products substantially liberated of catalyst at the top of said reaction zone 1 raising a stream of catalyst particles directly from the dense fluidized bed in said stripping zone removing the adsorbed hydraarburized material from the stream catalyst regeneration of cleaned catalyst particles by burning
 EMI13.10
 carbonaceous deposits in a dense fl-aidified bed in a regeneration zone setting the temperature of the atala 'a.biaat the regeneration to less than about X200 Fj 19

  catalyst of the regeneration zone and their recycling to the reaction zone; separating the entrained residual catalysis material from the stream of reaction products and higher boiling closed materials in the process by introducing a relatively high boiling point hydrocarbon oil into said cutting edge to effect the separation of liquid oil and catalyst particles 9 ', the passage of
 EMI13.11
 The fresh hydro-fuel feed in exchange of indirect heat by rap =

 <Desc / Clms Page number 14>

 flow of reaction products to remove some heat from them further heating of the feed

    preheated hydrocarbon
 EMI14.1
 fairy> to 800 = 1000 F before 19 introduction of this feed into the reaction zone, 9 further cooling of the reaction product stream to condense the hydroformate the separation of the hydromat from the gaseous reaction products or the process gas and heating them to
 EMI14.2
 temperatures of 1150 -1200 Q and their recycling to the reaction zone.



  60 Process for converting boiling hydrocarbon fractions
 EMI14.3
 within the boiling limits of engine fuels, in engine fuels with high antiknock properties including the passage of hydrocarbon materials, vaporized in combination with hot process gas containing hydrogen)

   through a dense fluidized bed of finely divided hydroformatio catalyst in a reaction zone at a temperature of 50 FS F and a pressure of 100-500 pounds per square inch at a catalyst / oil ratio of 0.5. removal of a substantially liberated stream of reaction products of catalyst at the top of said reaction zone; removal of a stream of di- catalyst particles
 EMI14.4
 straightening the dense fluidized bed into said reaction zone - removing adsorbed hydrocarbon material from the catalyst stream * conveying the catalyst stream to a regeneration zone with at most about one third of the air required for regeneration, - adding the remainder of regeneration air directly to the regeneration zone,

   adjusting the temperature of the catalyst undergoing regeneration, unless
 EMI14.5
 d9envirox 1200OFo 1 - removal of the catalyst particles from the regeneration zone and their recycling to the reaction zone. 9 separation of residual catalysis material entrained with the stream of reaction products and higher boiling material trained during
 EMI14.6
 process by introducing a relatively high boiling point hydro-fuel oil into said stream to effect the separation of oil and catalyst particles passing the fresh hydrocarbon feed in indirect heat exchange to the gas stream. reaction products to remove a certain amount of heat therefrom further heating
 EMI14.7
 age of matter

  hydrocarbon preheated to 800-1000 F before the introduction of this feed into the reaction zone; further cooling of the reaction product stream to condense the hydroformate separation of the hydroformate from the gaseous reaction products or gas.
 EMI14.8
 processing, and heating them to temperatures of 11500-12000P and recycling them to the reaction zone.



   7 Process for converting hydrocarbon fractions boiling within the boiling limits of motor fuels into fuels of
 EMI14.9
 A high-knockout engine comprising passing the vaporized hydrocarbon material in combination with hot hydrogen-containing process gas through a dense fluidized bed of finely divided hydroformatiox catalyst in a reaction zone at a temperature of 850 - 925 F and at a pressure of 100-500 pounds per square inch at a catalyst / oil ratio of 0.5 to 3;

   removing a substantially liberated stream of reaction products of catalyst at the top of said reaction zone, removing a stream of catalyst particles directly from the dense fluidized bed in said reaction zone; the removal of
 EMI14.10
 the adsorbed hydrocarbon material of the catalyst stream regenerates the cleaned catalyst particles by burning off the carbonaceous deposits
 EMI14.11
 in a dense fluidized bed in a regeneration zone, setting the temperature of the catalyst undergoing regeneration to less than about 1200 F; Removing the catalyst particles from the regeneration zone and recycling them to the reaction zone;

   separating entrained residual catalysis material from the reaction product stream by introducing a foreign oil into said stream and subjecting the stream to centrifugal forces sufficient to effect the separation
 EMI14.12
 removal of oil droplets and catalyst particles; removal of a mixture of catalyst particles in oil;

   separating the catalyst particles from the oil and recycling the oil

 <Desc / Clms Page number 15>

 
 EMI15.1
 slarified to said oil introduction phase the passage of the fresh hydrogen fuel feed in exchange for heat and with respect to the reaction product stream to remove a certain amount of heat therefrom further heating of the hydrocarbon feed preheated to 8000-1000F prior to the introduction of this feed into the reaction zone further cooling of the reaction product stream to condense the hydrorormate the separation of the hydrofilm from the gaseous reaction products or the gas treatment9 and heating the latter to temperatures of 11500-12000F and recycling them to the reactivation zone.



  8. Preceded by the conversion of hydrocarbon fractions boiling within the boiling limits of engine fuels, into engine fuels with high anti-knock power, comprising the passage of vaporized hydro-carburized material in combination with hot process gas containing hydregeme. , through a dense fluidized bed of the finely divided hydrochloride catalyst 1)) in a reaction zone at a temperature of 85 0 = 925 OF e at a pressure of 100 = 500 pounds per square inch at a catalyst / oil ratio of 095 to 3rd 19 removing a substantially liberated reaction product stream of catalyst at the top of said reaction zone; removing a stream of catalyst particles directly from the dense fluidized bed in said reaction zone ;

     take it off
 EMI15.2
 of the adsorbed hydrocarbon material, from the catalyst stream transport the transport of the catalyst stream to a regeneration zone with at most about 40% of the total air required for the regeneration the addition of the rest of the air from regeneration directly at the regeneration zone the temperature control of the catalyst undergo regenerations to less than about 1200 F;

     removal of catalyst particles,
 EMI15.3
 regeneration zone and their recycling towards the reaction zone the separation of the residual catalysis material entrained with the stream of
 EMI15.4
 reaction products and higher boiling point material formed during the process by introducing a higher boiling point hydrocarbon oil than naphtha into said stream to effect separation of the oil and catalyst particles by removing a mixture of catalyst particles in oil;

   separating the catalyst particles from the oil and recycling the clarified oil
 EMI15.5
 to said oil introduction phase the passage of the fresh hydro-fuel feed in indirect heat exchange with respect to the stream of reaction products poixo removing a certain amount of heat another heating of the preheated hydro-fuel feed, to 8000-10000F before 19 Introduction of this feed, into the reaction zone a further cooling of the reaction product stream to condense the hydroferm, the separation of the hydroferm from the gaseous reaction products or the process gas and the heating of the gas. these last temperatures
 EMI15.6
 deletions of llso -l2oo F and their recycling to the reaction zone 9.

   A process of hydroforming hydrocarbon fractions to produce high octane engine fuels comprising passing hot gas containing hydrogen, hydroearburized vapors and finely divided hydroformation catalyst through a reaction zone under conditions such as a dense fluidized bed of catalyst is formed with a higher dilute phase and so that a general concurrent displacement of vapor gauze and catalyst is obtained in said reaction zone; Removing reaction products substantially liberated to catalyze at the top of said reaction zone;

     removing catalyst particles from the upper part of said dense catalyst bed of the reaction zone but below its upper level, by
 EMI15.7
 a vertical duct, the top end of which opens into the dilute phase of said reaction zone and which extends downwardly through the dense bed.
 EMI15.8
 from this reaction zone 19 introduction of cleaning gas to the lower part of said conduit and 19 removal of cleaning gas and material removed by cleaning from the top of said conduit into said dilute gas;

     removing the cleaned catalyst from this line and regenerating it and returning it to the reaction zone.

 <Desc / Clms Page number 16>

 



  10. Process for converting naphtha to motor fuel
 EMI16.1
 with high antiknock power by hydroformatio119 comprising passing naphtha vapors in combination with hot hydrogen-containing process gas through a dense fluidized bed of finely divided hydroforming catalyst in a reaction zone at a temperature of 850 - 925F and at a pressure of 100-500 pounds per square inch at a catalyst to oil ratio by weight of 0.5 to 3; removing a stream of products from
 EMI16.2
 reaction at the top of the reaction zone Removing a core of catalyst particles directly from the top of the dense fluidized bed in said reaction zone;

   the separation of the adsorbed hydrocarbon material,) from the removed catalyst the regeneration of the cleaned catalyst particles by burning the carbonaceous deposits in a dense fluidized bed in a regeneration zone% the regulation of the catalyst temperature
 EMI16.3
 undergoing regeneration at less than about 1200, OFo the removal of catalyst particles from said regeneration zone the suspension of the removed catalyst at substantially a regeneration temperature in a gas con
 EMI16.4
 holding hydrogen> in the form of a dilute suspension,

   the gas being heated to a temperature higher than that of the regenerated catalyst and the passage of the dilute suspension of regenerated catalyst and gas containing
 EMI16.5
 flow of hydrogen through a short conduit into said reaction zone 11. A process for the hydoomation of naphtha comprising passing vapors of naphtha and gas containing hydrogen through a dense bed of hydroformation catalyst in a reaction zone under xaroomat3o conditions such that the temperature of the reaction zone is about 900 F and the pressure about 200 pounds per square inch and at a catalyst / oil ratio of about 1;

     removal of reaction products from said reaction zone removal of catalyst from said dense bed of catalyst and its cleaning regeneration of cleaned catalyst in a regeneration zone in which the temperature is maintained below about 1200 F; removing the regenerated catalyst from the regeneration zone and returning it to said reaction zone, the residence time of the catalyst in this reaction zone being at least 25 times the residence time in the regeneration zone.
 EMI16.6
 



  12o Fluid formatting process, in which a large reactor and a small regenerator containing a dense fluidized bed of finely divided catalyst is used, the naphtha feed being heated to a temperature higher than that of the reactor only shortly before
 EMI16.7
 its contact with the catalyst> the regenerated catalyst which is substantially at the regeneration temperature? being suspended after gel cleaning, in hydrogen containing gas heated to a temperature above that of the hot regenerated catalyst, the slurry being rapidly sent to the reactor so that heat is supplied thereto by the reactor. hot regenerated catalyst, the gas containing hydrogen and the naphtha feed