DE1809874A1 - Device for the dry distillation of bituminous or oily, fine-grained materials for the purpose of obtaining liquid hydrocarbons - Google Patents

Description

METALLGESELLSCHAFT Frankfurt / Main, Nov. 7, 1968

Aktiengesellschaft DrWer / EV Patent - Department 1809874

No. J57O1

Device for dry distillation of bituminous or oil-containing, fine-grained Materials for the extraction of liquid hydrocarbons

Description;

In recent times, efforts to dry-distill bituminous and oil-containing materials at temperatures between 450 and 650 ⁰ C in order to obtain liquid hydrocarbons, in particular oils and gasoline, and to convert them into a normal refinery by means of hydrogenating treatment, have been increasing to convert natural petroleum-like product. Such efforts exist especially in countries that do not have cheap and sufficient supply of petroleum, but have extensive, easily minable deposits of coal, oil shale, oil sands or the like. So that such an "artificial oil" can compete with natural oil, |

the bitumen or oil content in the feed material should be sufficiently high and, if possible, not below 8%, preferably above 10%. That Feedstock is also said to have a modest outlay in terms of investment and operating costs can be processed.

The distillation device to be used for this must therefore be used in large quantities can process in one unit. It should deliver a high yield of oils but little gas and should remove the distillation vapors without admixing combustion gases and without admixing them

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Make larger amounts of recycled distillation gases available for further processing. Heat consumption and power consumption for the distillation should remain low.

Shaft furnaces or retort furnaces are suitable for such a distillation not because the dwell time of the distillate vapors in them is too long and accordingly the formation of gas and residual coke is too great. Shaft furnaces that operate with purge gas heating or internal combustion are also unsuitable because they are a lumpy input material demand, and because in them the resulting distillate vapors through the Purge gas or combustion gas are diluted. Also the known methods for dry distillation of a fine grain feedstock in single or multi-stage fluidized beds cannot be used. Here, too, the distillate vapors are caused by the fluidizing gas diluted. When the fluidized gas is generated by partial combustion of the consumable material or heated by adding hot flue gases then the distillation gas will also contain nitrogen. This results in a considerable increase in the size of the condensation apparatus and an impairment of the distillation gas produced, which is used as long-distance gas, hydrogenation hydrogen or synthesis gas excludes.

It is known the dry distillation of bitumen and oil containing Materials using circulating heated heat transfer media. Heated ceramic balls or steel balls are used as heat transfer media used, the heat of which is specially transferred to the fine-grained material to be distilled in a rotary tube. This way of working is known for a long time, but could not prevail because the heating and the transport of the balls through the rotary tube and the heater is complicated and expensive.

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In contrast, the use of fine-grain heat carriers offers significant advantages when the solid distillation residue of the fine-grain Input material can be used as a heat transfer medium. There are known methods and devices, the fine-grained heat transfer medium to be heated in a pneumatic conveyor line or in a fluidized bed. Furthermore, methods and devices are known, heat carriers and to mix feedstock by simply running them together in a shaft furnace and thereby heat up the feedstock and distill. Support the released vapors and gases the whirling up and mixing of the heat transfer medium with the feedstock in the bed of the shaft furnace. This simple mixing in ^ a shaft furnace is no longer satisfactory with large amounts of charge and heat transfer media and leads to increased formation of coke and gas and thereby causes considerable losses in the yield of recoverable oils. Heating up very large amounts of circulating Fine-grained heat transfer media in a fluidized bed requires a great deal of effort and often causes unsafe operation. the Heating in a pneumatic conveyor line is therefore preferable.

The invention meets the requirements for a high oil yield with little formation of coke and gas, namely a rapid and i

uniform heating of the input material and rapid removal of the diluted de-distillate vapors from the distillation zone are effectively realized.

The invention is directed to an apparatus for dry distillation bituminous or oily materials such as coal, lignite, oil shale, oil sand or the like in a fine-grained state and the extraction of the distillate, the material to be distilled by means of

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circulating fine-grained, hot heat transfer medium that emerges from the residue separated from the distillation, in a pneumatic conveyor line heated and returned to the distillation apparatus, heated will.

The device according to the invention consists of a vertical pneumatic Conveying and heating section, which at the lower end of the gaseous conveying medium axially and from a concentric annular space, fine-grained heat carriers are fed through slots by means of controllable gas flows,

a separator at the upper end of the conveying path, the means of a _v from the ceiling downwards extending wall into a separation space and a secondary space with the conveying gas outlet and a the two common lower collecting chamber is divided, a mixer similar to that at its input side with the heat carrier derivation from Sifter and is connected to the supply of the feedstock to be distilled, and which has a discharge line on the discharge side for the hot mixture of heat transfer media and fresh distillation residue and for the distillation residue, an intermediate bunker, which on the one hand with the mixer and on the other hand with the annulus is connected at the foot of the conveyor line,

a dust separator in which the distillate vapors from the mixer be dedusted,

a cooling system in which the distillate vapors are precipitated by sprinkling with separated and cooled condensate, a dust separator in the conveying gas discharge line from the classifier, a conveying gas cooler with waste heat boiler
and a solids cooler for the discharged excess solids.

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Part of the distillation residue is used as a fine-grained heat transfer medium conveyed in a vertical pneumatic conveying and heating section and heated at the same time, in a separate room from the Combustion gases separated by free fall and ejection and fed to a mechanical mixer. Be in the mixer the heat transfer medium heated to e.g. 700 ° with the fine-grained feedstock to be distilled, e.g. B. coal, oil shale, oil sand or the like., merged and intensively mixed with one another within seconds, with a very rapid heat transfer from the heat carriers takes place on the fine-grained charge. The heat that passes over brings the material to the desired destination without delay. lation temperature, usually between 450 and 650 °, decomposes the bitumen and drives the oils contained or created in the feedstock in vapor form together with the water vapor formed from the moisture and the chemically bound water. The formation of distillation gas is extremely low. The mix of heat transfer media and fresh distillation residue flows out of the mixer in an intermediate bunker for re-distilling the input material and for expelling hydrocarbon vapors from the gap and pore space of the mixed material by blowing steam or recirculated distillation gases into the drainage from the intermediate bunker Mix. This mix is then added to the lower part of the pneumatic I table conveying and heating section, which closes the circuit of the heat transfer medium through heating and distillation will.

Parts of this device are known per se from U.S. Patents 2,788,314, 3,056,248 and 2,983,653. The combination according to the invention enables simple and effective distillation of fine-grained materials, condensation of distillate vapors and good Heat recovery from the exhaust gas of the heat carrier heating. At

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the distillation zone in the mixer is connected to a cooling system multi-stage sprinkling of the distillate vapors through cooled self-condensate, while the cooling of the För ^ ', gases of the heat transfer medium heating takes place in an air cooler and a waste heat boiler. At the Building large units of the device according to the invention, the specific investment costs are low and the heat and power requirements are low low.

The invention will be explained in more detail with reference to the figures. Fig. 1 is the flow diagram of a plant according to the invention. Figs. 2, 3, 4 are useful embodiments of the mixer and the classifier for separating the heated heat transfer medium from the conveying gas. In Fig. 1 are 1 the vertical, pneumatic conveying and heating line, 2 the separator for separating the heat transfer medium from the combustion gases, 3 the mechanical mixer and 4 the intermediate bunker.

The classifier 2 and the mixer 3 are connected to one another through the feed line 5 connected, which has a shut-off and metering slide 17 in the lower part and thus enables a dense, gas-blocking bed in the supply line 5 above the slide. Also are the intermediate bunker 4 and the conveyor line 1 are connected to one another by the feed line 7, which has a shut-off and metering slide in the lower part 25 and thus also has a dense, gas-blocking bed above of the slide 25 causes. This barrier columns in the supply lines 5 and 7 separate the mixer 3 and the intermediate bunker 4, in which the distillate vapors and a calorific value gas flow from the lower part of the conveyor line 1, in which there is air, and from the classifier 2, in which combustion gases flow.

The common conveying and heating section 1 is in the lower part, in which

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the mix runs through slots 9 into the conveyor line 1, drawn in. Appropriately preheated conveying air is introduced from below, flowing upward through the line 10, which tears up the mix flowing in at the slots 9 and burns off the carbon contained in the mix or attached to the mix, thereby heating the mix to the desired temperature of e.g. B. causes 700 °. If the mix does not contain enough carbon to heat the mix sufficiently, additional fuel is introduced into the conveying air through the line 65 with the nozzle 66, for example in the form of gas, waste oil or coal dust in a metered amount. Combustion proceeds very quickly in the presence of a large amount of mixed Λ good. Most of the heat released from combustion is immediately transferred to the mix. Excessive temperatures or large temperature differences between the combustion gases and the mix are reliably avoided. This rapid temperature equalization also makes it possible to preheat the conveying air to a high level so that Averden can work with the smallest excess air. The amount of air and the additional amount of fuel introduced, if necessary, are measured in such a way that the required heating of the material to be mixed in the conveyor line 1 is achieved.

The conveyor line 1 is generally 20 to 40 m long and is λ

expediently expanded continuously or gradually upwards. In the lower part the speed of the air or the combustion gases must be higher, e.g. 30-40 m / s, in order to accelerate the mix; in the top the speed can drop to 15-25 m / s as soon as the mix is accelerated sufficiently.

The mix runs through the slots 9 of the conveyor line 1 out of the annular space 11, which surrounds the conveyor line 1. Each slot receives a controlled feed through the nozzle 53 of seconds.

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där conveying air that pushes in the mix and according to its Quantities also controls the amount of mix that is pushed in. This ensures that the material to be mixed is actually introduced over the entire circumference of the conveying line and the conveying line is evenly loaded, which is particularly important with a large diameter of the conveyor line of e.g. Im or more. By the conveying air volume, which can be individually adjusted at each slot, can be increasingly introduced at individual slots, if necessary.

It is very important to separate the conveyed and heated heat carriers again from the conveying gas in such a way that there is no harmful wear of the apparatus walls and a considerable formation of fine abrasion. Meets this requirement the device 2 placed on the conveyor line 1 for separation and viewing the heated, pneumatically conveyed heat transfer media. The vertical conveying path ends in a greatly enlarged separation space 13, which is 5 to 20 times, preferably 7 to 12 times, the cross section the conveyor line owns. The speed of the conveying gases falls in this room strongly. By means of a downwardly extending partition wall 12 which extends downward from the ceiling and is open at the bottom, the conveying gas is flowed to deflected downwards, the solids being thrown out, and the separated conveying gas through the adjoining space 14 upwards to the outlet flows.

The sifter 2 is in its lower part at the same time as a collecting bunker 15 for the heat transfer medium is formed, which is connected to both the large separation space 13 and the smaller adjoining space 14. Depending on the position of the partition wall 12, the adjoining space 14, in which the hot combustion gases flow upwards again, and finally be discharged through the line 60, larger or smaller

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μ y—

be chosen. This is important because the upward speed the hot combustion gases in the space 14 is determined by the cross section of this space. The upward speed is in turn decisive for the amount of heat transfer medium separated.

According to the invention, the distance between the ceiling of the separation space 13 and the upper edge of the vertical conveyor line 1 is 3 - 10 m, preferably 5 - 7 m. At this distance there is practically no wear the ceiling of the separation room, which is provided with an abrasion-resistant, ceramic lining, is observed more closely. ™

Instead of the sifter 2 with the vertical conveyor line opening into it 1 a cyclone separator can be used, which is connected to a collecting bunker at the bottom. In this case, the upper end of the conveyor line will be deflected by 90 ° to the horizontal and connected to the cyclone separator.

From the lower part of the classifier 2, which is designed as a collecting bunker 15 A narrow feed line 5 leads to the inlet of the mechanical mixer 3 in order to separate the heated heat transfer medium Part of this line 5 is a slide 17 with which the men f

ge the heated heat transfer medium is controlled, the continuously the Mixer flows in. This slide 17 ensures the formation of a closed bed of the heat transfer medium above the slide. Around To absorb the thermal expansions, the ceramic-lined supply line expediently receives an expansion joint above the slide 17 16, which can also be provided with a supply line 18 for an auxiliary gas, e.g. water vapor. Through this auxiliary gas will be the gaps in the bed of the downward flowing heat transfer medium are filled in order to avoid that combustion gases from the classifier

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be carried in the mixer 3.

The fine-grained feedstock to be distilled is introduced from the bunker through the line 20 into the mechanical mixer 3. In this core material and hot heat transfer medium from line 5 are quickly and intensively mixed with one another. The fine-grained feedstock is heated to a specified temperature between 450 and 650 ° within a few seconds by rapid heat transfer, so that the bitumen is broken down by dry distillation and the oils are released in vapor form. At the same time, the moisture and the chemically bound water of the input material are released in vapor form. In addition, there is also a small amount of distillation gas, about 5 to 100 Nm, mostly 10-40 Nm ³ per ton of charge.

The mixer 3 is shown in its longitudinal section in Fig. 2, and in its cross section in Fig. 3. It has two shafts 21 rotating in the same direction, each of which has two diametrically opposed blades 22. The wings of both shafts interlock and guide the material to be mixed around the two shafts. This bypass is created by the fact that a wing of one mixing shaft wipes off the material to be mixed from the other mixing shaft, guides it around the mixing shaft in its own space of movement and transfers it back to the other mixing shaft. During the stripping process, the space filled by the material to be mixed constantly changes its shape, with the material of the edge parts being pushed towards the inside and that of the inner parts towards the edge. The blades are preferably placed helically on the shafts and also convey the mix forward axially to the shafts. The helical course of the blades also favors a more even load on the mixing shafts and the upstream gear. By inclining the mixing shafts downwards by 5-45 °, preferably 20-30 °, the forward conveyance of the material to be mixed can be supported. The intertwining

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The grip of the wings of both shafts causes mutual cleaning both !!! swell around the both wings of each mixed sill. If any deposits in this lens cross-section interfere, the wings themselves can be kept in lens shape. The blades of both shafts also clean the mixer housing in their movement space.

The blades 22 are expediently smoldered directly onto the mixing shafts 21. It is advantageous «not to keep them on continuously in order to avoid dangerous thermal stresses. The blades are therefore at a distance of 100 - 500 mm, preferably 150 - 300mm, etc. through a gap of 1-10 mm, preferably 2-5 mm of interrupted. Continuous wings can also be interrupted by notches right up to the weld seam and made more elastic. The blades and mixing shafts are only exposed to little wear and tear and can be made from normal steel or from a material with little increased wear resistance. It is important to equip the wing edges with a highly wear-resistant armored weld using suitable electrode material or to make them replaceable from high-carbon steel by screwing, clamping or welding.

The mixer 3 has good with an average temperature of 450 - Ä

650 ° to process and in exceptional cases alone with heated Heat carriers acted upon at a temperature of up to 750 °. In order to be able to cool the mixing shafts 21, hollow shafts are expediently used, to which the coolant is fed through a tube in the bore of the hollow shaft to the end, so that it is in the bore around the Feed pipe runs back around again. Cooling water is normally used as the coolant. Should the heat loss through cooling the mixing shafts are kept as low as possible, so circulating oil of a temperature range around 200 ° or another for higher

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Temperatures suitable coolants are used «The other parts of the mixer are expediently not cooled.

The mixing shafts 21 equipped with the helically arranged blades 22 are advantageously located on the inlet side of the mixer 3 short spiral screws 54 upstream, the heat transfer medium and Inevitably advance the load. The spiral worms 54 and the blades 22 of the mixing shafts 21 are formed by appropriately shaped transition pieces connected with each other. The good to be distilled can can also be blown in with recycled decomposition gases. These gases can also be used to remove the gases formed in the mixer Dissipate vapors and gases faster.

The housing 55 of the mixer 3 is in the lower part and in the side parts suitably lined and insulated on the inside and given a gas-tight welded, outer sheet metal jacket. In the top it can be in be carried out in the same way. The cover plate can also be used without Internal insulation welded on or at least partially screwed on so that it can be lifted off easily and the inside of the mixer can be checked. In this case, the cover plate is insulated from the outside.

Between the range of motion of the mixing shafts 21 and the cover plate a free gas collection space 56 is left in order to enable the vapors and gases formed in the mixer to flow off more easily. This free space 56 is closed at the discharge end of the mixer to draw off the vapors and gases to the condensation apparatus a cathedral 50 enlarged. This prevents dust from being carried away the condensation apparatus is suppressed. The free space is advantageously designed so that the speed of the vapors and gases if possible 10 m / sec. does not exceed, while it is in the discharge line

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device 51 to the condensation apparatus to 20 m / sec. and increase more can. The speed in the free gas space should also not be too low, since the vapors remain in the free space for a longer period of time Gas space 56 secondary reactions, especially of the high-boiling hydrocarbons be favored. Distillation gas returned to the mixer 3 supports the rapid removal of the vapors and gases and prevents secondary reactions. For some input materials, simpler mixing mechanisms with vertical mixing shafts can also be used will.

The mechanical mixer 3 with the two rotating in the same direction "

Mixing shafts 21 enables rapid and intensive mixing of large ones Flow rates in a short time and when distilling large amounts of fine-grained material to be distilled by means of large amounts fine-grained heat carriers distillation within a few seconds. The extensive decomposition is only achieved by the sudden heating of the oil vapors avoided and a maximum yield of liquid hydrocarbons from the feed to be distilled possible. Pneumatic mixing of large volume flows has not proven successful, since larger amounts of Steam or recycled distillation gases are required, which unnecessarily burden the condensation apparatus. Mechanical mixer I

Do not mix or grind quickly or intensely enough of any other kind the mix is too strong and not self-cleaning. However, the present invention is not necessarily limited to the use of a mixer instructed with 2 mixing shafts rotating in the same direction. So even in special cases simpler mixers with vertical Mixing shafts are used.

The feedstock is already largely distilled off in the mixer 3 and flows in a mixture with the heat transfer medium at the end of the mixer 3

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through the line 23 down into the intermediate bunker 4, in which the mixture is stored, the heat transfer from the heat carriers to the The feed is completed and the distillation of the feed is ended.

The mix is continuously withdrawn through the line 7 to the annular space of the conveyor line 1. In the lower part of the line 7 is a Slider 25 is provided with which the amount of the mixed material flowing into the annular space 11 is controlled. This slide 25 causes the formation of a closed bed of the heat transfer medium above the slide up to the intermediate bunker 4. The intermediate bunker receives a conical inlet to the line 7, a distribution device 26, z. B. in shape of a pipe ring with outflow openings, installed in order to supply water vapor or recycled distillation gas through line 27 and to distribute it over the bulk of the mixed material by means of the distribution device 26. The introduced water vapor or the gas cause a Driving out hydrocarbon vapors from the gaps in the bed and the pores of the mixed material. According to the invention, the residence time of the mixed material in the intermediate bunker for subsequent distillation, expulsion of hydrocarbon vapors and to compensate for certain irregularities in the circulation of the heat transfer medium 0, 5 - 5 min., preferably 1-2 minutes. Furthermore, the size of the free gas space in the intermediate bunker 4 is a possible residence time of the Mixing goods equal to 1-2 minutes. The intermediate bunker must then be dimensioned. The free gas space of the intermediate bunker The hydrocarbon vapors therefore only flow through slowly and can decompose as a result of secondary reactions. Appropriate Therefore, steam or distillation gas is introduced in such an amount that the residence time of the released hydrocarbon vapors does not exceed 1-2 seconds in the free gas space of the intermediate bunker.

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The feed material is expediently distilled with a grain size of less than 6 mm, preferably less than 4 mm. Breaks the grain during heat treatment the distillation slightly apart, a grain size of up to 12 mm can also be used. The maximum grain size will be determined by the requirement to carry out the distillation process during the short dwell time in mixer 3 as far as possible to the middle of the grain, so as not to impair the yield of oils.

The heat transfer medium used is preferably that during the distillation of the feedstock remaining solid residue is used. The grain size of this residue remains roughly the same as the grain ^, depending on the material used of the input material, also shrinks or drives something or can sometimes have a tendency to disintegrate.

The residue serving as a heat transfer medium should preferably have a grain size have above 0.2 mm, so that the separation in the classifier 2 is largely made possible with simple means and only small amounts fine dust from the vapors and gases formed during the distillation are carried into the condensation apparatus. At the The circulation of the heat transfer medium continuously creates abrasion, which escapes from the circulation system as flue dust with the combustion gases. Further a larger amount of more or less granular residue is continuously formed by distilling the input material, which is made up of the circulation is to be repelled. This can be done through the line 61 at the intermediate bunker 4. At this point, however, a part is fresh distilled residue which has not yet passed the conveying and heating section 1 and which contains carbon. To clear the residue Being able to release carbon into the open air becomes excess residue discharged through the line 28 from the collecting bunker 15 of the classifier and fed through a cooler 43 of the heap.

The vapors and gases released during the distillation are released on

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Discharge of the mixer in the extended gas dome 50th above of the mixing shafts 21 collected, to which also still the in the intermediate bunker 4 formed vapors and gases are passed, and through the line 51 of a dry dust separator 29, preferably in In the form of one or more cyclones connected in parallel or one behind the other, fed in and largely freed from the dust that is entrained. The separated dust is introduced through the line 30 into the lower part of the intermediate bunker 4 or into the line 7.

From the dust separator 29, the vapors and gases flow through the line 68 into a cooling system 69, in which the vapors and gases are intensively washed and cooled by means of cooled self-condensate. This treatment is expediently carried out in several, for example three, stages. In the first stage 30, the heavy oil condensing in this stage is used to cool the vapors and gases, which during washing practically completely absorbs the dust not captured by the dry dust separator 29 from the vapors and gases. The cooling of the circulating oil can take place in a heat exchanger 31 against cooling water, air or the like, or it can also be effected by generating low-pressure steam. A simple solution, provided that no value is placed on the utilization of the waste heat, is to inject water into the washing cooler 30 and evaporate it. The amount of water is then dosed and the temperature of the vapors and gases adjusted so that as much heavy oil condenses in the wash cooler as is necessary to keep the heavy oil with its dust content satisfactorily liquid and pumpable. The vapors and gases are cooled to a temperature between 200 and 300 ⁰ C here. However, the temperature can be lowered even further to allow more oil to condense and to obtain a more dilute heavy oil.

According to the invention, a dust-rich portion of the heavy oil is through

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the feed line 32 is returned to the mechanical mixer 3 and distilled again. It was found that the one in the oil Fine dust agglomerates into larger grains that can be easily separated out. The recycled oil is made through the distillation slightly cracked. Depending on the nature of the heavy oil, its output is 70 - 90% of the recycled heavy oil, while the rest converts to carbon and gases. The 70 - 90% extracted are naturally of a better character than the recycled heavy oil self.

In the second stage of the cooling system in the washing cooler 33, the Ga- ^

se and vapors are cooled by circulating medium oil to such an extent that the oil vapors largely condense, but still no water vapor precipitates. This is at the temperature of the vapors and gases at the exit of the washing cooler 33 of a little over 100 ° C. is the case. The circulating medium oil is for this purpose in a heat exchanger 34 by cooling water, Air or the like re-cooled. Injection and evaporation of water is not applicable in the washer cooler 33 because it is difficult to to evaporate the injection water properly at the low temperatures and thus to keep the circulating oil free of water. That from the Excess medium oil withdrawn from circulation is practically free of dust and water and can be sent directly to further processing or to the tank ger be fed.

In a further stage of the cooling system 69, the washing cooler 35, the remaining mixture of gases and vapors by sprinkling self condensate and water is cooled to about 30 ⁰ C. The circulating water is expediently cooled by air in a first cooler 59 and indirectly in a second cooler 62. The condensed light oils and the gasoline are separated from the process water in a separating container 36. In this cooling stage, the light oils, gasoline and condense

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Steam. An indirect cooler with cooling surfaces can also be used at this point. That remains at the cooling temperature Destination gas saturated with water vapor and gasoline vapors. The gasoline vapors still contained in it can be removed by washing can be obtained with light oil, by compressing the gases with subsequent cooling or by deep-freezing. Part of the distillation gas is returned as flushing gas to the mechanical mixer 3 and intermediate bunker 4.

The distillation gases have a high content of C ₁ - to C 3 hydrocarbons and also containing hydrogen, carbon monoxide and often also carbon dioxide. They have a high calorific value and are practically nitrogen-free. They can be delivered as long-distance gas or processed into synthesis gas or hydrogen.

The combustion gases that have heated the circulating heat carriers in the conveyor line 1 and conveyed them up, and from these in the sifter 2 have been separated, pull from the side room 14 through the line 60 in the cyclone 37, in which the entrained dust is largely out the gases is deposited. This dust can through the line 38 back into the supply line 5 or directly to the mechanical Mixer 3 are fed. Preferably this dust is repelled from the process, e.g. B. through line 39 to the portion to keep dust in the heat transfer medium to a minimum.

An air preheater 40 and expediently close to the cyclone 37 a waste heat boiler 41 with steam collector 64 for generating water vapor in order to utilize the waste heat of the exhaust gases. It's the It is left to the design to determine whether it is not also more useful in individual cases to first use the waste heat boiler 41 and then the air preheater 40

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to be switched on in the exhaust gas path. In the air preheater 40 is for the Conveyor line 1 required and preheated air compressed in the fan 63. Air preheater 40 and waste heat boiler 41 are advantageously so designed so that the waste heat of the exhaust gases is probably largely used, but the dew point of the sulfur dioxide-containing gases with certainty is not fallen below.

After the waste heat has been used, the exhaust gases have to be finely dedusted before they can be discharged into the open through a chimney. Mechanical or electrical fine dust extractors 42 or a combination of both are used for this purpose. In individual cases, this can also be done with your own

be connected to wet laundry. Since the device according to the invention is used in large units of high power and thus very large amounts of exhaust gases are to be released into the open, their content must are also very low on fine dust. This can often only be achieved with electrical fine cleaning in the final stage. A wet wash comes into consideration when the exhaust gases are rich in SO2 and this is to be won. When using electrical fine cleaning it is often necessary to increase the temperature of the exhaust gases before entering the electrostatic precipitator by injecting and evaporating them Lowering water to close to the dew point of the exhaust gases and making the exhaust gases more conductive with a higher proportion of water vapor. For this The supply line 57 is used for the injection water and the nozzles 58 are used for atomizing the water upstream of the fine dust extractor 42 Electrostatic precipitator,

The dust arising from the cyclone 37 is about 700 ^° C. and needs a considerable amount of water to cool down before it can be conveyed to the dump. When it cools down, a larger amount of water vapor is produced, which can only be released into the open after dust has been removed. It is therefore advisable to use the whole of

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the exhaust gases from the classifier 2 entrained dust by the air preheater 40 and the waste heat boiler 41 and thus to install the cyclone 27 only after these two heat exchangers. This The cyclone is then advantageously designed as a multi-clone. Then the heat contained in the entire dust in the air preheater 40 and waste heat boiler 41 are used and the dust is cooled to close to the dew point of the exhaust gases.

The other cyclone 37 through the line 39 and from the fine dust rn 42 through the line 67 extracted dust is to be cooled and moistened before transport and dumping on the heap in order to avoid it Being able to load, transport and tip nuisance caused by large clouds of dust. This cooling and moistening of the repelled Dust in the cooler 43 can be fed all residues that are to be brought to the dump. Cooling and humidifying the hot Residues are preferably carried out in a mixer 43 which, like the mixer 3, has two co-rotating and helical Includes mixing shafts equipped with curved blades. At the point of application for the dust, a supply 44 of water is expedient of condensate occurring in the process, arranged. By injecting and evaporating the water, the dust is raised to a temperature cooled below 100 ° and can optionally be brought to a water content of e.g. 2 - 4% or 10 - 20%.

If the device according to the invention for the distillation of coals is used, in addition to the tar to be extracted, large amounts of coke are also produced. This coke is used as a circulating heat carrier and consumed in a small amount to cover the fuel requirement in the conveyor and heating track 1. The great bulk of the The coke expelled from the circulation is expediently burned in a composite power station or, as far as possible and useful, as sinter-burning.

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material, used as a lean agent in coking plants, as a tar-free, dust-like reduction fuel. This residual coke can also be converted into shaped coke for domestic combustion purposes or into blast furnace coke by briquetting and post-treatment of the briquettes. During the distillation of coal, experience has shown that a temperature at the outlet of the mixer 3 and in the intermediate bunker 4 between 550 and 650 ^° C. is maintained in order to obtain a maximum yield of tar. Experience has shown that, depending on the type of coal, this yield is 100-170% of the tar content of the feed coal that can be detected in the smoldering analysis according to Fischer and Schrader. The device is suitable for the use of both baking and non-baking coal.

Oil shale has an oil content of 2 to over 30% by weight, depending on its origin. All oil shale of various types and origins can be processed in the device according to the invention. Experience has shown that however, the oil content should not be less than 8%, expediently not less than 10%, in order to make processing sufficiently economical. In detail The profitability depends on the cost of the oil shale and the area in which the oil shale can be mined is and how high the price of the natural oil at the recovery point of shale oil is. It is of particular economic advantage if the oil shale residue is partially or entirely for special Purposes can be used and is not simply worthless to dump on the dump. Depending on the composition of the residue it can be used as a hydraulic binder, from raw material for cement production, used for the production of building blocks, for the extraction of aluminum oxide or uranium oxide or the like will.

Oil shale with an oil content of over 20% are often naturally occurring

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plastic or become so when passing through a certain temperature range. The device according to the invention can through the use of fine-grain heat carriers and the distillation in the mechanical mixer 3 also in the cold or hot Condition plastically behaving oil shale operated trouble-free will. The oil yield of oil shale depends on its character different. Compared to what can be achieved in the Fischer analysis Oil application, are in the device according to the invention Yields between 95 and 110 wt.% Achieved.

Oil sands are often difficult to process because they can be plastically even at temperatures around 20 ⁰ C and tend to stick together. By using suitable mechanical shredders, in particular spiked rolling mills, shredding to less than 10 mm can be achieved. If the broken material tends to stick together before it is introduced into the mechanical mixer 3, it is advantageous to add fine-grain residue from the distillation of the oil sands to the broken material immediately after it has been crushed and thereby prevent them from sticking together. Often the oil sand tends to stick to the walls of the shredder and the means of transport. This sticking can be completely prevented if the walls are heated by low-pressure steam or the like.

The oil is present as such in the oil sands. The same goes for oil pastels. It an oil yield of around 95% of the oil content that can be determined by extraction is achieved during the distillation in the device according to the invention Achieve if a favorable distillation temperature and a short dwell time of the oil vapors in the hot part of the device is observed will. By setting a slightly higher distillation temperature, the character of the overall oil obtained can be reduced with a lower

009823/1581 _ ₂₃ _

velvet yields can be improved.

The device according to the invention can be implemented in large, high-performance units that allow 200-4001 of coal, oil shale, oil sands or the like to be distilled per hour. If a total oil output of 10% by weight is assumed, 20-40 t of oil per hour, corresponding to 160,000 - 320,000 t of oil per year, can be obtained in one unit. Based on experience gained, the clear diameter of the conveying and heating section 1 should not significantly exceed 1500 mm. For high throughputs, 2-4 conveyor lines are therefore switched in parallel to one separator 2. As can be seen from Fig. 4 ^ j, the separation space 13 of the separator 2 is divided by transverse walls in a device with several parallel conveyor lines to prevent a full running of a conveyor line if it fails by the other conveyor lines in operation. The mechanical mixer 3 is also limited in its unit output. With a temperature difference of 100-150 ° C between the heated heat transfer medium flowing into the mixer and the heat transfer medium exiting from the intermediate bunker 4, the need for circulating heat transfer medium is normally 4-8 times the weight of the input material to be distilled. Thus, the distillation required 200-400 t feedstock hourly 800-3200 t hourly umlauts Λ Fende heat carrier, The mixing of these large volumes together is advantageously divided in several, expediently two to four mixers, below the common separator 2 arranged in parallel and operated will. It is to be decided in each individual case whether a separate intermediate bunker 4 is to be assigned to each mixer 3. Fig. 4 shows a plan view of a cross section through the device 2 with the mouths of three parallel conveyor and heating sections 1 in the separation space 13 with the partition 12 and the two transverse walls 44. Below the device 2 are two mixers 3 and an intermediate bunker 4 indicated in broken lines.

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The distillation apparatus according to the invention represents a new combination of novel and known devices with special ones
fluidic characteristics and has proven its industrial success. It enables the production of liquid hydrocarbons in high yield from fine-grained, bituminous and oil-containing materials of various origins. It is extremely reliable, can be built in large units with a very high output and, compared to known distillation devices, is good adaptability and economic efficiency.

009823/1581

Claims (1)

Contact 1 Device for the dry distillation of bituminous or oily Materials such as coal, lignite, oil shale, oil sand or the like in a fine-grained state by heating them using circulating, fine-grained, hot heat transfer medium, separated from the residue of the distillation, heated in a pneumatic conveyor line, returned to the distillation apparatus and mixed there with further quantities of the material to be distilled, and for recovery of the distillate, characterized by a) a vertical, pneumatic conveying and heating section 1, the gaseous conveying means at the lower end through the axial feed and from the concentric annular space 11 through slots 9 by means of controllable gas flows from the slots associated with the slots Nozzles 53 fine-grained heat transfer medium are fed, b) the classifier 2, into which the conveyor line 1 opens, and the means a wall 12 extending downwards from the ceiling into a separation space 13, an adjoining space 14 with the conveying gas discharge line 60 and one of these two common lower collecting space 15 is divided with the heat carrier drainage 5, c) the mixer 3, which is connected to the heat transfer medium on its input side 5 of the classifier 2 and connected to the feed 20 for the feedstock to be distilled and on the discharge side with the derivation 23 for the hot mixture of heat carriers and fresh distillation residue and with the derivation 51 for the Is provided with distillate vapors, d) the intermediate bunker 4, which through the discharge line 23 with the mixer 3 and through the line 7 to the annular space 11 at the foot of the 009823/1581 Conveyor line 1 is connected, e) the dust separator 29, which the distillate vapors from the line 51 are supplied, and from which the dusty distillate vapors reach the cooling system 69 via the line 68, while separated dust via the line 30 to the intermediate bunker 4 or can be delivered to line 7, f) the cooling system 68, in which the distillate vapors with separated and cooled condensate are sprinkled, g)> the one connected to the conveying gas discharge line 60 of the classifier 2 Dust separator 37, h) the conveying gas cooler with the air preheater 40 and the waste heat boiler 41 and the fine dust extractor 42 as well as i) the cooler 43, which is in the classifier 2 and / or the intermediate bunker 4 accumulating excess solids and the one in the dust collector 37 precipitated dust is fed through lines 28, 61 and 39 and discharged from this. Claim 2 Device according to claim 1, characterized in that the vertical Conveyor path 1 widens steadily or intermittently upwards and preferably has a mean diameter between 0.5 and 2.0 m from 1.2 to 1.6 m. Claim 3 Device according to claim 1 and 2, characterized in that the Cross-section of the separation space 13 5 to 20 times, preferably BATH ORIGINAL 009823/1581 - " ³ ~ se is 7 to 12 times the cross section of the conveyor line 1 and that the distance from the ceiling above the separation space 13 of the sifter from the upper mouth of the conveyor line 3 to 10 m, is preferably 5 to 7 m. Claim 4 Device according to claims 1 to 3 _# characterized in that that the upper part of the classifier 2 is designed as a cyclone separator is in which the horizontally diverted conveyor line 1 opens laterally. A. Claim 5 Device according to claims 1 to 3 _# characterized in that the subdivided in the separation chamber 13 by partition walls 44 faces 2, two or more parallel-operated heating and conveying sections are assigned. Claim 6 Device according to Claims 1 to 5, characterized in that that the collecting bunker 15 in the classifier 2 two or more parallel i operated mixer 3 are assigned. Claim 7 Device according to Claim 1, characterized by a mixer 3 with two co-rotating screw shafts 21, each carrying two diametrically opposed mixing blades 22 arranged helically around the shaft 21, the mixing blades 22 of both mixing shafts intermeshing. 009823/1581 - ⁴ - An sp rue h. 8th Device according to claims 1 and 7, characterized in that the mixing blades 22 on the shafts 21 as pieces from 100 to 500 mm, preferably 150 to 300 mm in length with gaps of 1 to 10 mm, preferably 2 to 5 mm in width are hardened on the outer edges by armor welding or by screwed or welded hard steel plates are. Claim 9 Device according to Claims 7 and 8, characterized in that that the mixing shafts 21 on the inlet side of the mixer 3, preferably below the solids feed lines 5 and 16, as spiral screws 54 are formed. Claim IQ Device according to Claims 7 to 9, characterized in that the mixing shafts 21 of the mixing mechanism 3 are preferably rotated by 5 to 45 ° are inclined downwards conveying by 20 to 30 ° to the horizontal. Contact 1 1 Device according to claims 7 to 10, characterized in that the housing 55 of the mixing mechanism 3 above the mixing shafts 21 Contains gas collecting space with a dome which is greatly expanded on the discharge side, in which the discharge 51 of the distillate vapors begins. -5-009823 / 1581 Claim 1 2 ·! ■ # . "Device according to claim 1, characterized by a mixer with one or more vertical mixing shafts. Claim 1 3 Device according to claims 1 to 12, characterized by the Distributor 26 with the supply line 27 in the lower part of the intermediate bunker 4 for flushing gas or flushing steam for expelling distillate vapors from the mix. _Λ Claim 14 Device according to Claims 1 to 13, characterized by Slide 17, 25 in the discharge lines 5 from the classifier 2 and 7 from the intermediate bunker 4, respectively. Claim 1 5 Device according to claims 1 to 14, characterized by the Feed 18 for a gaseous or vaporous winding medium into the heat transfer discharge line 5 on the classifier 2. " Claim 1 6 Device according to claim 1, characterized in that the cooling system 69 consists of washing coolers 30, 33, 35 connected in series, in which the distillate vapors are gradually sprinkled be cooled and condensed with chilled condensate accumulating in each cooler. 009823/1581 Claim 1 7 Device according to claim 1, characterized in that the fine dust removal 42 contains an electrostatic dust collector. Claim 1 8 Device according to claim 1, characterized in that the cooler 43 is a twin screw mixer with co-rotating shafts, on each of which two diametrically opposed, helical mixing blades are attached. 0 0 9 8 2 3/1581