DE1668219A1 - Hydrogenation of fats and oils - Google Patents

Description

Hydration of Petten and Blen ==================================== The invention relates to continuous manufacturing processes for alcohols and glycerine with detergent properties.

It is known that straight-chain aliphatic alcohols are important Have value as wetting agents and detergents. The possibility of using these connections (which are also called fatty alcohols) all household cleaning agents either in Porm don alcohols aelbat or in port of the sulphated alcohol has long been recognized. Detergents, those made from such petroleum alcohols have excellent foaming properties, good detergent properties and yin very mild in terms of their effect on the skin. It is important that this Substances are also biodegradable, so that wastewater disposal difficulties practically avoided as a result of their use o The high cost of fatty alcohols and their sulfated derivatives, however, have hitherto prevented their widespread use. At first glance over @@ chen the high cost of these alcohols as they are made up of different Fats and oils can be produced that are relatively cheap and in sufficient quantities Amounts are available. Considerations of the blxherlgon Verabreammfinahmen for The production of fatty alcohols from fats, however, leaves the reason for their high cost lends become apparent. For example, in one manufacturing process, the fat is hydrolyzed or saponified to a mixture of glycerine and fatty acids. The fatty acids are then separated from the glyserine, esterified, using sodium see below don alcohols reduced and deastered.

In the case of the multi-stage process, almost all operational steps are carried out in batches carried out, which greatly increases the overall process costs. If sodium for the Reduction is used, special construction materials are required always In addition, it is absolutely necessary to avoid any air entry into the system Even if catalysts other than sodium are used for the hydrogenation stage The usual process measures will be carried out, with the ester being donated in batches finely divided catalyst is brought into contact with many difficulties, related to the elimination of the catalyst from the end product, whereby the catalyst is filtered out and then used for further batches must become.

In theory, a typical triglyceride can be converted directly to glycerol and a mixture of fatty alcohols in a single step as follows In the example, the alkyl groups R and r can have different chain lengths depending on the origin of the triglyceride. The alkyl groups can also be unsaturated (r) or saturated (R). As can be seen from the equation above, the main reaction in the conversion is the hydrogenative cleavage of a carbon-oxygen bond. In parallel, unsaturated alkyl groups or saturated alcohols can be hydrogenated. Such a splitting reaction by hydrogenation can produce saturated alcohols having carbon numbers from about 10 to about 20 depending on the origin and composition of the fat or triglycerides used as the feed material. In fact, alcohols having from about 10 to about 114 carbon atoms are more desirable than those having from about 16 to about 20 carbon atoms because they generally have better detergent properties. The more valuable alcohols, however, are generally difficult to obtain using an inexpensive raw material such as tallow, which has such a molecular structure that the simple reaction indicated above produces predominantly longer chain length alcohols.

It was clear9 that considerable efforts had already been made In order to explore the possibilities, fatty alcohols were used in a one-step hycrier process to produce, instead of producing them in the multistage process, since the hydrolysis and reduction of a carboxylic acid or its ester conditional. These efforts that are geared towards a one-step procedure, but apparently have to none Success led. It @st from the reaction shown above that the hydrogenating Cleavage reaction must be carefully controlled in order to get the theoretical product distribution to obtain. Uncontrolled reactions produce propylene glycol, or even propanol Propanol instead of the more valuable glycerine and also lead to a reduction of the total product leads to an excessive consumption of valuable hydrogen, too strong hydrogenation can even reduce the pett alcohols produced to a considerable extent Convert the reduction in product value into the corresponding hydrocarbons.

In addition to the reduced value of the products produced and the excessive consumption of hydrogen increases the uncontrolled hydrogenation, in'item ale many different types of products sur result that has separation difficulties and makes the final recovery of the products much more difficult.

Through these difficulties: the one-step hydrogenation of fats too control, efforts in this direction have to be carried out in batches or semi-batches Proceedings conducted. As is well known, these are carried out ohargemweise Processes were far inferior economically to continuous processes the experiments with the one-step process with high hydrogen pressures (from 100 bia 300 atmospheres) highly active catalysts that are easily poisoned and relatively low temperatures of around 277 ° C (530 ° F) to about 349 ° C (660 ° F) carried out. The high pressures require heavily constructed autoclaves between The individual res @ @ @ @ @ res @ @ @ @ @ @ @ @ the associated difficulties must be tightly closed and opened again. The highly active catalysts that have been used (generally copper chromite or zinc chromite catalysts) are ksatspialig and are poisoned leioht, especially by Schwafele when they are as Slurry to be used together with the reaction mixture, ea is necessary considerable care is taken in their subsequent separation from both the point of view the recovery of catalysts ala also from the point of view of the preservation of an end producta9 that is free of catalyst traces to be used.

If tallow is used as a raw material, it must go to manufacture particular care must be taken to ensure that the sebum contains a minimum amount of sulfur so that a minimum of xatalyaator-poisoning sulfur is present.

As mentioned above, when sebum is used as a raw material9 produces large noses of the less valuable fatty alcohols. For all of these reasons Alkohoep are the durci one-stage hydrogenation from a cheap feedstock, how sebum are produced, for example, are very costly and are therefore not widely used as detergents or surface-active Substances found.

In one method according to the invention, one feed, the triglycerides ton of alcohols with between 16 and 20 carbon atoms in a mixture from fatty alcohols, the little ata fa a 10% concentration of alcohols with between Contains 10 to 14 carbon atoms, converted by catalytic hydrogenation, wherein the feed is melted and the molten feed together with Waeaeratoff in an amount of 2.0 to 4.0 kg of water per 100 kg of charge up through a contact soae that contains a catalyst bed that consists of a sulfur-resistant, catalytically active contact mass exists at one temperature between 316 and 454 ° C (600 and 850 ° F) and a total pressure in the range of ton 35 kg / cm2 (500 psig) to 141 kg / cm2 (2000) psig) is the hydrogen partial pressure maintained within a range of 17.6 kg / cm2 (250 psi) to 127 kg / cm2 (1800 psi), the speed of the gas and the liquid is adjusted so that the catalytic effective filling us little ata 10 fa of its original Volunone and a boundary layer is created and maintained below which the catalyst density greater than 80.6 kg / m3 (5 pounds per cubic foot) and above the catalyst gate density less a18 is 1.6 kg / m3 (0.1 pounds per cubic foot) with no facilities used to loosen up become the particulate contact mass in the catalyst filling in an amount between 0.001 and 1.0 kg of catalyst per 100 kg charge is replaced that the liquid product is above the boundary layer is deducted.

Preferred embodiments according to the invention are based on the figures for example explained.

Figures 1 and 2 such flow diagrams of fat conversion arrangements.

Figure 1 shows the simplest embodiment of an inventive Arrangement of 3Ma of melted fat is stored in a reservoir 10 sucked off with a pampa 12 and puspto Waeaeretoff sue the line 14 Line 16, which is compressed to operating pressure by the Komproe-or 18, is the line 20 is introduced into the line 14. The mixture is made one by one passed through a preheating furnace 22 and a heat exchanger 24 and then in the reactor 26 was introduced.

The reactor 26 is a pressure vessel with a uniform cross section and a grid 28, us distribute the mixture of fat and hydrogen su. This reactor is filled with catalyst in a suitable manner so that the liquid fat and the hydrogen flowing up through the catalyst, the catalyst m @@ se by at least 10% over their Ll. ii E. tSF n. . '. ':. : i'ayT (f r '' R ~., C :,% 3.. "Z. ° movement in the reactor liquid ver @@@ assen. The liquid AucfluS wir6 in the objet part of the reactor separated into a product stream mre a recycle stream. The circle @@ fstrom wr8 aQht gets::; r? ! through the middle of the res @@@ en @@@@@ with @@@@@ Pum @@ 32 is pumped, which the circuit @ tron to a @ @ teli @ under the Grid 28, which reintroduces the K @@@ ly @@ torf @ llung plus @@@@@@ t. The water @@@@ f @@ d flössiges @@ tt entering the reaction zone @ verder by de @ Kreisl @@ f @ tro @ preheated to a temperature practically close to the reaction temperature.

Catalyst can periodically @@@@ dur @@ a K @ catalyst supplement system 34 added and @@ glei @ her We @@@ discharged through ei @ catalyst extraction system 36 will. These Sy @@ ems are only shown schematically.

The effluent leaves the reactor through line 38 and then becomes cooled in the heat exchanger 24, as well as passed through a high pressure separator 40 The Wasaeratoff is discharged head through the line 42, after the passage by the valve 44 relaxed, accustomed in the scrubber 46 and through the line 48 with the aid of the compressor 50 to the ~. r. , rx. . : i. ac = f '=. r,? xwIcr ~ "erN e = u", m.., R. s t'a,,, er '' 'f: $ tll 8ltB I 0lTllQ @@ pa @@@@@ 40 are withdrawn via line 52, @ @@@@@ em @ i @ d @@ V @ ntil 54 will be shaved have, de-energized and headed to ei @@@ Verdam @ f @@ tr @ mmel 56, from which the vaporous @@@ ducts withdrawn via line 58 and the liquid ire @@@ via line 60 will. A raw separation from the unconverted feed is converted into an @ @ raktionierk @ l @@@ e 62, from which the products are removed via line 64 and to further separation "" Io * cleaning devices @@. Not converted @@@ @@ tt and @@ ch @@@ the components are denoted by the words '' = ikr '', 3'E;:, yaa..s dciatsB.i.Mtlf.ty -. <. at least 10% it is necessary to expand the catalyst @ @@ by at least 10% expandi @@ en, @@@ @@@@ Function of the viscosity of the liquid, the thickness of the liquid and the size and density of the catalyst sites in addition to the speed of the liquid @ elb @@. The speed of the gas must be so great, @@@ @@@ die willkär @@ ohe Movement of the catalytic converter parts demands, however, it must be smaller All be the load that is required to cause the catalyst to open the reaction zone demand.

The use of such a system, known as the "billowing" catalyst fill system improves and eliminates most of the procedural shortcomings that the older processes for the production of Pettalcohols adhere to. For example, the Tezpersturelnotstellung in de reactor trots the strong exothermic behavior of the hydrogenation reaction in of the order of 0.56 to 2.78 ° C (1 to 5 ° F) throughout the reaction zone obtain. This is achieved by the random movement of the mixture of catalyst particles, Liquid and Su reached in the catalyst filling, which in the pull through the internal circulation of the liquid from the top of the reactor to the bottom is completed will. This narrow or short term creates the need for an external heat exchange device and, more importantly, it eliminates the risk of overheating in any part of the reaction system. The catalyst can therefore be used at optimal Temperatures can be operated without uncontrolled reactions occurring, the products of low value result in increasing hydrogen consumption and recovery don’t produce a costly and complicated machin.

The Turbulent In do * reactor serves further to the hydrogen without to keep any mechanical machinery dispersed in the reactor. the Turbulent drives through a very effective contacting of the charging liquids with hydrogen, which increases the rate of the desired hydrogenation reactions enlarged and thereby the size of the reactor that is required @@ a certain To process menu of loading, diminished.

The catalyst is kept in the reaction zone and not atit the liquid is hosted. A pilter operation that is usually required around the catalyst from the products su green, in% therefore not ndtl6, t the total expenditure of the system and simplifies the operation.

In addition, aie has a high density of the catalyst in the reaction ton can be 80 to 1130 kg / m2 (5 to 70 pounds per cubic foot), much more Katalyaator available in the reaction zone sur Polge than dai bicher was the case. Since the catalyst concentration is large, it is possible to use less active catalysts to use them as they were previously used and to replace them with substances, dia are more robust and more resistant to sulfur poisoning. It is clear that the high density of catalyst in the reactor is also largely the Reduced response time that is necessary to get the response perform.

Since the catalytic converters are ultimately poisoned or deactivated, aind facilities provided in the illustrated embodiment according to the invention, around the exhausted Katalyaator continuously or semi-continuously su ruts Die lreatsgesohwindigkoit of course varies with the amount of catalyst poisons that included in the charge.

Such a continuous addition to the gate enables a boatimate Unlimited catalyst activity is obtained. Therefore, the product distribution unlimited without fluctuations caused by operation Day and with an exhausted catalyst on another day, be maintained. This continuous supplementation or freshening is therefore an essential factor in making product extraction and cleaning equipment economical To be shaped, to guarantee a constant product quality is important to emphasize that modes of operation with constant catalyst activity and selectivity u @ possible with continuously catalytically active Festhett reaction systems and d are practically impossible with so often loaded reaction systems, where the exhausted catalyst must be reused.

Suitable feeds for the process according to the invention are substances the ale flap and bold are just denoted.

The patte and oils come from plants and animals, in donna they occur in bulk and in an easily available form.

They are mainly a product of agriculture, although they are also in considerable quantities from uncultivated tropical plants and won Marine animals breathe. Such fats and oils are essentially triglycerides or esters of glycerine and both saturated ale as well as unsaturated, long-chain aliphatic compounds Acids. However, it is essential for the value of the measures according to the invention and important that fats and oils, which are obtained from nature, with Fremdatof-Zen may be heavily contaminated, including Schwofel and nitrogen contain which can act as catalyst poisons. I see an advantage of the invention in that Do not carefully consider the frette and yole used as a feed must be pretreated in order to reduce the content of such catalyst poisons, before the feed is fed to the hydrogenation stage.

The invention is indeed au @ any @@ lanzliche or animal do and oils a @ reversible, @@ e however has the greatest Bepouture in the @@@ preparation of Fats and oils that are prod @@ ier @ in large quantities, such as tallow, bacon, coco @@@@ oil, Construction @@@ ll @@@@@ oil, soybean oil and flaxseed oil. the Invention has special importance for the treatment of roue, in digestible sebum and sebum fats, which are available in large quantities sur otchwa and relatively bt Dio obéie Letton in the TriglyMridn, of which the sebum is composed, have predominantly lengths of 16 to 18 carbon atoms. As stated above, according to this invention, g becomes this inedible tallow in more valuable alcohol of higher quality with lower chain lengths than the C16 and C18 alcohols Mgewendelt normally obtained from this batch ers would become.

The respective contact materials that are used according to the invention, increase the speed of the ohenic reactions, the course of which is desired and these can be described as any catalytically active agent. These masses are cheap M, the catalytic effect of poisoning by sulfur is relative remains unaffected. Lots of cheap catalysts designed for petroleum technology can be used for the method according to the invention.

Aluminum oxide, combinations of silicon dioxide and aluminum oxide and refined os and effective catalysts for the process according to the invention. Combinations of sun silicon dioxide and aluminum oxide are more effective, possible sales wagon of an aura function that apparently evolved through such a combination will. The contact means mayen with iron, cobalt, molybdenum, chromium, Wlfram or Nickel YerotErkt. If such promoters for the invention Method used will find a catalytic effect from the sulphur Promoter elements received instead of donated metal alone. Copper and zinc are therefore no precautionary factors, as the sulfides of these elements affect the hydrogenation activity are relatively inactive. The nobler elements of group VIII of the periodic table, e.g.

Platinum, palladium, and rhodium can be used, but they are wagon of their high accounts also did not favor alPM-r engines.

The particle size of the catalyst used depends on the different Factors affecting the liquid velocity in the reactor are bigenaehaften the reactor liquid elbot and affect the density of the catalyst.

In all cases the velocities of the upflow offset Gas and the liquid flowing close up at the particle size used the contact means in random motion in the reactor fluid and expand but laseen the catalyst mass by at least 10% above its near state These speeds do not cause any significant loss of catalyst from the reactor S no subsequent contamination of the product stream with catalyst. It was shown to be pelletized or extruded 8atelysator with part size ton 1.59 mm (1/16 inch) diameter or less for the process of the present invention wirlc is. Unshaped particles with an average particle size in the range from 1.19 to 0.053 mm (16 to 270 mesh) are also effective. Preferably is this range is 0.59 to 0.074 mm (30 to 200 mesh) with a diameter of 5 % of the grazed particles not larger than three times the diameter of the 5% smallest Particle is.

In all cases the dense reactor phase contains at least 80 kg (5th pounds) catalyst per m3 (cubic feet) in the catalyst room, whereas the room lasts less than 1.6 kg (0.1 pound) catalyst per m3 (oubiefum) without that a broadening of the reactor diameter at its upper end (i.e. additionally a so-called "knock out" - or expansion zone) is necessary in order to this pronounced phase separation to bowirkeno The reaction temperatures, which in of the teaching according to the invention are applied, are considerably more than the3 how they were commonly used for the hydrogenation of fats and oils relatively high temperatures are required, and the aliphatic chain lengths of the alcohols produced, which are caused by the hydrogenative splitting of carbon-carbon bonds, as well as by the easier achievable hydrogenative splitting of Carbon Samer dead bonds are obtained. The reaction temperatures are generally above 316 ° C (600 ° F). A preferred range for the reaction temperatures, applied ranges between 371 ° C and 427 ° C (700 ° F and 800 ° F).

Ee a lot important, don hydrogen partial pressure in don reaction eyes, especially when the catalyst is active, to limit the hydrogenation of the alcohol groups of primary fatty alcohol and glycerin products. The control of the Hydrogen partial pressure can be adjusted by controlling the total pressure or the concentration de Waaseratoffa in the reaction zone. Diane's concentration left her generally in the order of 50 to 90% and at total pressures of 35 kg / cm2 (500 * to 140 kg / cm2 (2000 psig) hydrogen partial pressures are in the range from 7.5kg / cm (250pai) to 27kg / CB? (1800pai) .The choice of the optimal Waaaeratoff partial pressure The range depends on the feed, the catalysts, the temperature and the degree of hydrogenation breakdown, along with various other factors significant are o The amount of hydrogen added to the reaction zone can of course be considerably larger than the net hydrogen -Feed by recycling the hydrogen according to FIG. The net waaaeratoffbeaohiokung, which corresponds to the previous requirements of the hydrogenation splitting reactions, fat generally greater than 1 kg waeaeratoff per 100 kg fat or oil charge and is normally in the range from 2 to 10 kg of water content for 100 kg of charge.

The reactor 26 can be used without an internal control unit or IPIUS unit, As used in Figure 1, it is constructed with the control of the reactor temperatures practically duroh the turbulent the. Feetatoffe, liquids and gases in the reactor is effected. Without the internal liquid backflow in the reactor 26, the Liquid velocities in the reactor are significantly below those in the corresponding reactor of Figure 1 are.

Be t therefore possible to use a catalyst with a much smaller average Particle size to use.

In Figure 2 is a flow diagram of a multi-stage arrangement in this Invention shown. The systems for loading waaaeretoff and fats that erate stage of the reactor system and the entapreohenden main separation stages similar to that shown in FIG. The fractionation column 62-. Lot one, however multi-bottom distillation device, from of light gases that Containing hydrocarbons from methane to done, in dom overhead vapor through the Line 64 can be discharged. Flueaige products, which are described below $ So the middle of the column is discharged through line 88 (from this line From there they are finally directed to the usual cleaning and separation devices). The sump is withdrawn as a liquid through line 66.

The temperatures in the fractionation column are controlled so that the products that are withdrawn via line 88 are glycerine and the valuable ones Contain C10, C12 and C14 fatty alcohols. The higher boiling C16, C18 and CQ alcohols tsrdea outside the column together with a small amount of unconverted glycerides withdrawn through line 16 and using a Pompe 90 on don Druok pumped to the second reactor stage, moored with hydrogen from line 92, in the device 94 again and nooh welter heated in the heat exchanger 96 and @ initiated in the reactor 98 of the second stage.

The reactor of the world stage is essentially the same as the reactor of the The first level is similar and has the same design features. He has one Manifold 100, an external reflux line 102, an internal pump 104 and catalyst feed - and discharge systems 106 and 108 respectively. The catalyst in the reactor of the second stage is aioh similar to that in the first stage reactor in a state more arbitrary Movement and is expanded so that it is at least 10 * larger in volume ale in dos detached or resting state of the crowd. In the reactor wlrd maintain a boundary layer under which the Featatoffxaaae in a concentration griser than 80 kg / m3 (5 found per cubic foot) and above which the Peatatoffe in opiner Consentration should be less than 1.6 kg / m3 (0.1 pounds per cubic foot) without that a settling zone or other separation device is used. The products are taken from the reactor 98 through line 110 and through the Waraetauacher 96 where all parts would be found, AU direz heat exchangers are all over the line 112 su don entry of the primary recovery arrangement, which is directed from don containers 40, 56 and 62 as described above.

In the multi-level device according to Pigur 2, the fat becomes practical VellatRndig converted to glycerine and higher alcohols in the eraten stage. That Glycerine is removed via line 88 and the higher alcohols become dmrmwf to the more valuable lower alcohols in the reactor 98 of the second pipe Split hydrogenation. This arrangement enables dater Use of various catalysts in reactors 26 and 98 and / or other catalysts Operating conditions in the two reactors, such as the catalyst and operating conditions in the first stage mainly to break the carbon-oxygen bond dienong whereas the catalyst and the operating conditions in the reactor second stage are chosen so that a maximum selectivity in the cleavage the carbon-carbon bond that is required to produce the is obtained to produce more valuable pettalcohols.

Dan special separation system (generally in the fractionation column 62 embodied) allows indiaaemtallaine complete suppression of the less valuable higher alcohols. However, other variations of these embodiments can be made sain, from which these less valuable alcohols are removed only to the extent that as far as there is in the market for them. In the same way, other systems can carry out sur Equivalent separations be provided, whereby ta of the fractionation column 62 a Vacuum distillation takes place. With other variations, glycerin can be obtained from the raw product using water washers to wash out the alcohol can be separated by conventional distillation processes. It is the specialist clear that many other systems for separation, recovery and purification the Products according to this invention can be used and that the invention measures are not limited to the separation, extraction and purification described are.

Example 1 The aa example relates to the use of the in Figure 1 described device, In the inedible beef tallow su fatty alcohols with relatively high detergent properties and relatively high value together with glycerine should be implemented. The catalyst is extruded and has a diameter 0.7938 mm (1/32 inch) and a surface area of 8430 cm2 (310 square inches) per The analysis of the fresh catalyst shows 84% alumina, 3.5% CoO and 12.5% McO3. The sebum load has an iodine number of 44 and an amount of freezing of 195. The analysis of the long-chain aliphatic groups in sebum shows about 25% saturated C16 groups, 25% saturated C18 groups, 40% unsaturated C18 groups, the remainder being made up of other acid groups (and impurities).

Hydrogen is being accelerated in the reactor system at a net rate corresponding to 2.5 kg per 100 kg charge. There are velocities in the reactor maintained9 and a state of voluntary movement su erseugen inde the. Catalyst is expanding, un about 30 1 of his withdrawal or To take rest volume. The K-: @lysator density in the reactor is 450 kg / m3 (28 pounds per CubiofuB) e The reactor has srrar no separation, the catalyst density however, less than 0.8 kg / m2 (0.08 kg / m2) 005 pounds per cubio foot). The reactor is operated at a temperature of 399 ° C (750 ° F) and a total pressure of 140 kg / on? (2000pagehalten, which is a hydrogen partial pressure of 112 kg / cm2 (1600 psi) enteprioht. The Katalyeator is continuously se des Reactor directed and at a rate of 0.10 kg per 100 kg of feed deducted. The space velocity of the feed is chosen to be practical the entire triglyceride charge is converted.

@ The first column of Table I contains the yields for this Case. The glycerine yield is substantial, at least about 80 op ders theoretical. ut the invention, however, was mainly due to the relatively large amount seen on lower alcohols (33.6%) produced, although as above Mentioned the composition of the concentration of tallow a the yield of definitely less than 10% of such lower alcohols would entepreohon and probably a yield Ton only 5% @ giant £ * Doron alcohols. Another Boweis, a sizeable one Splitting by hydrogenation of the higher alcohols was achieved, is sue don large amounts of hydrocarbons, which are absorbed as products, and aue der Tateache su saohnon that these hydrocarbons have chains that are derived from 1 (methane) to 6 (hexane) vary. The unspecified material is likely to be breathed from unconverted triglycerides, impurities, glycols and lower alcohols. The Geaaatauabeate exceeds 100%, since about 2% Wäaeerateff with the loading is consumed.

A catalyst that sur use without internal noisy in reactor 26 suitable is bauxite, which was previously used to decolorize a certain petroleum product was used and which has an average particle size of 0.074 m (200 mesh) is milled before use. The Aaalyae diesels rial gives 92 s Al2O3, 4% Fe2O3 and about 2% non-volatile organic material (probably coke).

Saah don grinding, the contact mass is sifted, leaving 5% a sieve Pass with a clear width of 0.053 mm (270 mesh). The contact means has a surface of 55 m2 per gram.

Example 2 The example explains the use of the two-stage AuafChrungaform according to the invention. A scheme is shown in FIG.

In this example the reactor 26 (the reactor of the first stage) covered with a Kraok catalyst, which essentially consists of 99% S102 and A1203 exists. This contact medium has a surface area of over 425 m2 per g and The Porz from Perlent has the seed through a sieve of a clear mesh size Ton 0,42 mm (40 mesh) fall through, but from a sieve with a clear mesh size be retained by 0.25 m (60 m). The sitar stage reactor wlrd with a 0.79 inch (1/32 inch) catalyst extrudate containing 56% silica, Contains 19% aluminum oxide, 6% nickel sulphide and 19% tungsten sulphide. Dionor catalyst has an initial surface area of 275 a / g. An internal reflux is used in both reactors provided to jean katalyeator in inez state of voluntary movement and, in this Case, to a volume of over 35% don the corresponding Abeetzvoluaena or resting volume e su hold. The sebum charge is identical to that used in Example 1 above. The net hydrogen charge corresponds to 3.5 kg per kg of charge tallow. Of the The pressure in the reactor 26 is 126 kg / m2 (1800 psig), whereas the pressure in the Reactor 98 increases somewhat. The reactor 26 is on a The temperature is maintained at 399 ° C (705 ° F) while the reactor 98 is at a temperature at 421 ° C (790 ° P).

The catalyst is continuously replaced in both reactors. the Exchange rate in reactor 26 is 0.04 kg / 100 kg feed, whereas in reactor 98 it is very low and about 0.005 kg / 100 kg of feed fat is equivalent to. The bottoms from fractionation column 62 passing through line 66 is fed into the reactor 98 of the wide 8 tutu, corresponds to about kg / 100 kg of tallow, which is introduced into the reactor 26.

Table I shows the results of Example 2 * In In this case the yields of glycerine exceed 95% of those theoretically can be obtained in accordance with the sebum analysis. The eye-catching one However, the result obtained in this example is the yield of 64 fa alcohols that boil in the C10 to C14 range and from doyen to more than 10% by weight Is lauryl alcohol. By more careful adjustment of the operation of the fraction column 62 the yields of higher alcohols are of course zero. In az example how shown, there is a small amount of these alcohols in the product fraction.

The higher yields of lower alcohols are in turn by the proportional yields of light hydrocarbons that are produced will.

Table I Yields in Examples 1 and 2 Example 1 2 Arrangement 1 2 Yields in% by weight of glycerine 8.4 10. 5 Alcohols (C10-C14) 33.6 64.0 Alcohols (C16 + 43.0 1.3 Hydrogen-12.4 24.0 Substances Undefined Be-4.6 3.0 Ingredients In don given examples, an inedible tallow of a single origin was used as the feed used to show the various differences in yields and the grade flexibility of product distribution to represent that in the various hn embodiments according to the invention can be obtained. In fact, however may be another example of various differently fats or oils that are next to the Invention can be processed, given. It is emphasized again that the invention is not affected by impurities present in these feed materials are present, is impaired, and that advantageously Besohickungeaaterialien Low quality banks are used

Claims (6)

Patent claim 1. Method for converting a charge that Triglyserides of alcohols containing between 16 and 20 carbon atoms in a mixture of fatty alcohols at least in a 10% concentration Contains alcohols with between 10 and 14 carbon atoms, by catalytic hydrogenation, dadurah indicated that the charge was melted and the charge was melted together with hydrogen in an amount of 2.0 to 4.0 kg of hydrogen per 100 kg Upward loading through a contact zone that contains the analyzer bed There is now a sulfur-resistant, catalytically active contact mass, in the case of a Temperature between 316 and 454 ° C (600 and 850 ° F) and a total pressure in the range from 35 to s 140 kg / cm2 (500 to 2000 paig) is passed that the hydrogen partial pressure The speed is maintained in a range ton 17.6 kg / cm2 (250 psi to 1800 psi) des des and the liquid cement is adjusted so that the catalytically active FUlluw At least 10 g of the original tolumono expanded and a boundary layer generated and risen, under which the Katalyaatcrdiehte gober ale 80, 6 kg / m3 (5 pounds per cubic foot) and the catalyst density is less than 1.6 kg / m3 (0.1 pounds per Cubietuss) amounts without any facilities be used for loosening that the particulate contact mass in the catalyst filling replaced in an amount between 0.001 and 1.0 kg of catalyst per 100 kg of feed and that the liquid product is withdrawn above the limit MMcht. 2. The method according to claim 1, characterized in that the charge contains inedible sebum. 3. The method according to claim 1 or 2, characterized in that the catalytically active contact material aluminum oxide or aluminum oxide and silicon dioxide and, if desired, contains a promoter. 4. The method according to claim 3, characterized in that an iron, Cobalt, molybdenum, chromium, tungsten or nickel fromotor is used. 5. The method according to any one of the preceding claims, characterized as durci, that the catalytically active mass falls within a * part size range of 16 to 270 mesh is applied o 6. The method according to any one of the preceding Aneprttehe, thereby marked, da8 two contact zones are used and d86 glycerine and alcohols in between 10 and 14 carbon atoms are removed from the effluent of the erate contact zone before the discharge is directed into the wide contact zone o