DE2363064A1 - COAL LIQUID - Google Patents

Description

Coal liquefaction

The present invention relates to coal liquefaction,
in particular, a new and improved process for liquefying coal with easier ash removal.

Coal can be converted into valuable products by
one of the charcoal solvent extraction with or without
Subjecting hydrogen to a mixture of coal extract and undissolved carbon residue including undissolved extractable carbonaceous material, pusain and mineral materials or ash.

The finely divided mineral material or ashes and
non-unsaturated coal must be separated from the coal extract; generally consists of this separation step
the principal disadvantage, which stands in the way of a successful implementation of the coal extraction process. The two

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ORIGINAL INSPECTED

Fine particle sizes occurring in coal solvation processes create numerous difficulties if you follow the usual Attempts to use separation methods such as filtering, centrifuging, or settling.

The present invention provides a new and improved one Process for coal liquefaction, the subsequent Removal of insoluble material is facilitated.

The invention is explained in more detail in the following description and in the accompanying drawings simplified schematic flow diagram of an embodiment of the present invention.

The present invention is generally that one controls the coal liquefaction so that the subsequent Separation of finely divided coal residue is facilitated.

In particular, the liquefaction of coal is controlled so that the coal liquefaction product obtained, which consists of a liquid coal extract of dissolved carbonaceous material in a coal liquefaction solvent and insoluble Material (ash and unreacted coal) ', and a ash removal index (D.I.) as defined below is within a specific area. It was surprising found that by controlling the ash removal index of a coal liquefaction product, the subsequent Separation of the insoluble material can be greatly facilitated while losing the desired carbon products the coal extract becomes minimal.

According to the present invention, coal liquefaction controlled so that a coal liquefaction product is obtained, which from in a coal liquefaction solvent

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dissolved carbonaceous material and in the liquefying solvent dispersed insoluble material and a ash removal index (D.I.) of about Io to has, preferably about 11 to 15, where

DI = lbs, Ashless Benzene-Insoluble / lm product χ loo lbs. Moisture-ase-free (MAF) carbonaceous material derived from the coal, dissolved and dispersed in the coal liquefaction solvent

The benzene insolubility of the carbon product can be determined in a known manner, for example by ASTM test 0367-67. As is well known the determination of the benzene insolubles includes the ash content of the product and accordingly becomes the Determination of the ash removal index used the ash-free benzene-insoluble factor determined by the fact that Amount of ash in the product subtracted from the amount of benzene-insolubles in the product. The denominator of the index is that Amount of moisture-ash-free carbonaceous material, dissolved and dispersed in the liquefaction solvent at the end of the coal liquefaction stage.

The coal liquefaction is carried out by removing the coal in the presence of a coal liquefaction solution after a the numerous known "processes (catalytic or non-catalytic) hydrogenated. The catalytic liquefaction is carried out by one of the numerous known methods, e.g. in a fixed catalyst bed, in the catalytic Fluidized bed or in an expanded or foamed bed.

The coal liquefaction solvent can be selected from a large number selected solvents used for coal liquefaction including the hydrogen donor solution

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medium, non-hydrogen donor solvents and mixtures the same. These solvents are well known to those skilled in the art so that the present invention can be fully understood no detailed explanation is required. A coal liquefaction & fuel, which is preferably used in the context of the present invention is a 315- ^ 82 ° C solvent (the components boil either over the entire area or only part of it), which from the Coal liquefaction product is obtained and not yet the was then subjected to hydrogenation.

The ash removal index of the liquefaction product is checked, by determining the content of benzene-insolubles in the coal liquefaction obtained from hydrogen treatment controlled product (the ash content of the coal is fixed, so that by controlling the total amount of benzene-insolubles increases and / or decreases the Xndex counter, so that the ash removal index also rises or falls). The amount of benzene insolubles in the coal liquefaction product is best controlled by controlling the hydrotreatment flow rate at specific Catalysts, reaction temperatures and hydrogen partial pressures controlled; an increase in the flow rate increases the amount of benzene-insolubles. The selection of special temperatures, flow rates, Catalysts, hydrogen partial pressures, etc. to achieve the amount of benzene-insolubles in the hydrogen treatment— product that delivers the desired ash removal index, should be easily possible for the skilled person ".

In general, the hydrotreatment is carried out at temperatures carried out from about 371 - ^ 82 C, preferably about

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C; the pressure is around 7 o - 28o atm. The flow rate of the liquid is generally about l, o to _t h o St. ", the hydrogen partial pressure around 56 - (. Absol) 21o At the hydrogen treatment is generally a suitable hydrotreating catalyst in the presence of, for example, cobalt molybdate. Tungsten-nickel sulfide, nickel-molybdate, mixtures thereof, etc. The water treatment is generally carried out in a foamed bed, as described in US Pat. No. 2,987,465 (Johanneson) *

According to the present invention, this control of the sludge index is that obtained from coal liquefaction Product facilitates the separation of the ash without causing excessive loss of the desired carbon products occurs, measured on the ash-free + ** 55 ° C product, which is not isolated from the coal * It was found that a reduction in the ash removal index below a value of Io leads to a reduction in ash removal, while an increase in the ash removal index above 18 does result in acceptable ash removal, but to one Increase in the loss of ash-free carbon + ^ 55 carbon product leads.

The insoluble material is preferably from the coal liquefaction product separated by using a liquid promoter whose aromatic properties are less are than those of the liquefaction solvent, whereby the Separation of the insoluble material is intensified and accelerated and a liquid charcoal extract is obtained which is practically free of insoluble material.

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The liquid used to enhance and accelerate the separation of the insoluble material from the coal liquefaction product is generally a liquid hydrocarbon with a characterization factor (κ) of at least about 9 »751, preferably at least about 11.0, where

K = \ / ^T B

T_ = molar average boiling point of the liquid

^B C.)

G = specific weight of the liquid (15.6 ° C / 15.6 ° C)

The characterization factor is the index of the aromatic / paraffinic properties of hydrocarbons and petroleum fractions, as reported by Watson & Nelson Ind. Eng. Chem. 25 880 (1933); more paraffinic materials have a higher value of the characterization factor (κ). A promoter liquid is used with a characterization factor (κ) over 9 »75» which is also less aromatic than the liquefying solvent, i.e. the characterization factor (κ) of the promoter fluid has a value which is generally at least 0.25 higher as the characterization factor of the liquefaction solvent.

In the following table are some representative characterization factors (κ) compiled for different materials:

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Tabel

Anthracene 8.3

Naphthalene 8.4 22o-26o ° C coal tar distillate 8.8

288-482 ° C "" "9.1

315-482 ° C "η» 9, ο

204-232 ° C "" 9.4

Benzene. 9.8

Tetrahydronaphthalene 9.8

o-xylene lo, 3

Decahydronaphthalene lo, 6

Cyclohexane 11, ο

22o-26o ° C bp kerosene 11.9

n-dodecylbenzene 12, ο Propylene oligomers (pentamer) 12.2

Cetene - 12.8

Trxdecane 12.8

n-hexane 12.9

Hexadecane or cetane 13, ο

The liquid used to enhance and accelerate the separation of the insoluble material is further characterized as having a 5 vol .-% destination temperature of at least about 121 C and a 95 vol .-% distillation temperature of at least about 177 C and not higher than about 400 ° C. The promoter liquid preferably has a 5% by volume distillation temperature of at least about 155 ° C., preferably at least about 2040 ° C. The 95% by volume distillation temperature is preferably no greater than about 315 ° C. The most preferred promoter liquid has one 5 vol. / B — distillation temperature of at least about 22o C and a 95 vol. - ^ - distillation temperature of no more than about 260 C. The promoter liquid can be a hydrocarbon, for example tetrahydronaphthalene; In this case, the 5 vol. ¹ P and 95 vol. 5'o-explosion temperatures are the same, ie the hydrocarbon has a single boiling point. In this case, the boiling point of the hydrocarbon must be at least about 177 ° C. Vol .- ^ - Distillation temperature of at least about 121 ° C and one

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95 vol .-% distillation temperature of at least about 177 C. to meet. The promoter liquid is preferably a mixture of hydrocarbons, in this case the 5 vol. and 95 vol .- ^ - distillation temperatures not identical *

The 5 vol.-fo and 95 vol .- ^ - distillation temperatures are usually determined in accordance with ASTM No., D 86-67 or No. D II60, the former for liquids with a 95 vol. Fo distillation temperature below 315 C and the the latter is preferred for those above 315 ° C. The methods for determining such temperatures are well known so that it is not necessary to fully understand the present invention further details are required. Of course, the temperatures mentioned are also corrected to atmospheric pressure.

The following are examples of such liquids: kerosene or kerosene fractions from paraffinic or mixed base crude oils; Middle distillates, light gas— oils and gas oil fractions from paraffinic or mixed Base crude oils; Alkylbenzenes having side chains of Io or more carbon atoms; paraffinic hydrocarbons with more than 12 carbon atoms; ¥ ice oil or white oil fractions Crude oil; cC-oiefine with more than 12 carbon atoms; fully hydrogenated Naphthalenes and substituted naphthalenes; Propylene oligomers (pentamer and higher); Tetrahydronaphthalene, heavy naphtha fractions. Most preferred liquids are kerosene fractions, ice oil, fully hydrogenated naphthalenes and substituted naphthalenes and tetrahydronaphthalene.

The amount of material used to enhance and accelerate the separation of insoluble material from the coal liquefaction product Dissolved liquid promoter depends on the specific used liquid, the coal liquefaction agent

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tel, the coal used as the starting material and the manner in which the coal liquefaction is carried out. As will be readily apparent to those skilled in the art, the amount of liquid promoter should be minimal in order to reduce the overall cost of the process. It has been found that using a liquid having controlled aromatic properties in accordance with the present invention, one can accomplish the desired separation of the insoluble material with moderate amounts of the liquid promoter. In general, the weight ratio of liquid promoter / charcoal solution is in the range from about 0.2: 1 to 3%, preferably about 0.3: 1 to 1.5: 1, in particular about 0.3: 1 to 1.5: 1 Using the preferred pro-red liquid, namely a kerosene fraction with 5 VpI .- $ - and 95 vol .- ^ - distillation temperatures of 22o or 26o C, a weight ratio of promoter liquid / coal solution in the order of magnitude of ο.4 · 1 to o, 6: 1 proved particularly successful. Of course, larger amounts of the liquid promoter can also be used, but the use of such larger amounts is uneconomical. In addition, the use of an excess of liquid promoter can lead to the precipitation or separation of a very large amount of the desired carbon products from the coal extract. In particular, as the amount of liquid promoter used increases, a larger amount of ash is separated from the coal solution; At the same time, however, there is also an increased separation of the desired carbon products from the coal solution. When using the liquid promoters described above, not only can moderate amounts of the solvent be used, but the ash can also be effectively separated from the coal solution, ie in amounts of more than $ 99 "without an excessive loss of the desired coal products occurring."

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Coal, _{e.g. bituminous coal 9,} may contain 5 to 10% insoluble material (e.g. fusain) on a moisture-ash-free basis (MAF); accordingly, at least about 5 to 10% of the MAP coal is lost in the process. In the recovery of coal products by a Solvatisierungöverfahren is the potential loss of product durefc, the amount of 455 g of product ψ sat _s selected from the coal not recovered it gets there is EiäiaXiob. this is the fraction, including the insoluble carbon bas-rials (e.g. fusain), which - not; from the solid residue of the coal deashing can be recovered, Macli of the present invention (based on a MAF Eohle starting material) the product loss of the ^ 55 C ψ-ΕοέΏροκΘΒύοίπι (on an ash-free basis) on a value of not msfiz · as about Jo Ges ·? «, - ^ held, preferably no more than 25 G-ex-J _o - / £ ° Xeh generally the loss of 455 G - ^ - products (on the basis of a MAF-Kohie) is about Io to 25 G9fJ "-fa ₅ A ^ uerdera the pure coal product (the extracted carbonaceous material excluding the promoter liquid ₈ of Verfliissigungslösungsmittels and gaseous product ©) contains - hereinafter sometimes referred to as" coal product ¹¹ - less than about Q ₂ 5 wt fs insoluble material _a The specific amount of insoluble material that may be present in the carbon product depends on the product standards; the ash removal x "is controlled ₉ so that the required specifications are met" sis of Illinois-type manufacturing eiaes Kohleprodiakts corresponds to sit less than ₅ o o5 G © w .- ^ ar "- soluble material of more than 99% strength ⁿ © Aseheentfernung. as the skilled person readily appreciated _9, the percent ash removal depends to Gexihnung a carbon product with the required minimum. Amount of insoluble material depends on the initial ash content of the coal. According to the present invention, the liquid promoter is added to the carbon solution in such an amount (as described above) that a carbon product is obtained in which the insoluble material is in a

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Amount less than about 0.05 wt .- ^ is present, wherein the loss of 455 ° C + product is about 10 to 3o wt .- ^, preferably about 10 to 25 wt .- ^ (based on a MAF carbon base product); i.e., about 7 to 90 weight percent of the MAF coal feedstock is obtained either as gas or liquid fuel.

The liquid promoter can also be prepared in that a material with a characterization factor below 9 »75 mixed with a material, its characterization factor is above 9 »75 - provided that the mixture has a characterization factor about 9575 and the ones described above Has boiling properties. Using mixed materials is a convenient way of regulating the characterization factor.

As a further alternative, the liquid promoter from the Procedure originate; it is obtained by hydrotreatment a portion of the isolated carbon product as disclosed in the S.N. 3o4 32o of November 7, 1972.

The separation of the insoluble material from the coal extract is generally carried out at a temperature of about 1 ^ 9 to 315 ° C, preferably at about 177 to 26o ° C; the pressure is approximately 0 to 35 atmospheres, preferably approximately 0 to 21 atmospheres. Of course you can use / higher pressures, however, it will be readily apparent to those skilled in the art that lower pressures are preferred. The insoluble material will preferably separated by gravity settling, the charcoal extract practically free of insolubles above and the insoluble material is peeled off at the bottom. With such gravity deposition, the amount should be taken from below Products should be minimal so that the loss of the heavy products below is minimized. The one to achieve the desired Results required withdrawal speed of the

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products taken below should be clear to those skilled in the art. Generally the rate is about 20 to 25 weight percent of the
Total amount ("liquefaction product and promoter liquid). The residence time during settling is generally in the order of magnitude of about 0.5 to 6 hours, preferably about 0.5 to 3 hours.

The invention is also characterized in that the heavier material obtained from the coal extract, ie the + i * 55 ° C or + U82 ° C liquid product, furthermore one
Hydrogen treatment can be subjected to its
To reduce sulfur content. In controlling the first hydrotreatment to achieve the desired deashing index, the hydrotreatment may not be sufficient to achieve the desired reduction in sulfur content; according to the present invention one can
subject the heavier product to a further hydrogen treatment in order to further reduce the sulfur content.

The use of a second hydrotreatment can also be advantageous in those cases where the desired sulfur reduction is not achieved in the first hydrotreatment could be. In these cases, the first hydrogen treatment is controlled so that the liquefaction product has the desired ash removal index without, however, the required reduction in the sulfur content taking place. The latter is then subjected to a second hydrotreatment achieved.

This method offers the advantage that there is no liquefying solvent is required in the second hydrotreatment, thereby reducing the reactor volume and achieved an increase in the flow rate. It also comes with an ashless hydrotreatment

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Starting product carried out, eliminating the use of different Process technologies becomes possible, i.e. a different catalyst and / or a different Procedure, a fixed bed instead of an expanded bed.

The invention will now be described in more detail with reference to the accompanying figure explained. Of course, however, the invention is not restricted to this.

According to the figure, ground or pulverized coal, generally bituminous, sub-bituminous or lignite, preferably bituminous coal introduced through line Io into a coal solvation and pulping zone 11, along with a coal liquefaction solvent in line 12. The coal liquefaction solvent can be obtained from the a large number of solvents known for this purpose can be selected, including the hydrogen donor solvents, Non-hydrogen donor solvents and mixtures thereof. These solvents are known so that no detailed description appears necessary in order to fully understand the present invention. How special is the coal liquefaction solvent a 315 to ^ 82 ° C solvent, which is obtained from the coal liquefaction product wins and which was not subjected to the subsequent hydrogenation. The solvent will be the Coal added in an amount sufficient to effect the desired liquefaction; in general it is Amount such that the solvent / charcoal weight ratio is about 1: 1 to 2o: 1, preferably about 1.5: 1 to 5: 1.

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A coal paste is drawn off from zone 11 through line 13 and introduced into a coal liquefaction zone Ik , where the coal is converted into liquid products in a known manner. The liquefaction zone Ik is operated in a known manner; it can be catalytic or non-catalytic and can be carried out in the presence or absence of hydrogen. The hydrogenation can be carried out in a fixed catalyst bed, in a catalytic fluidized bed, or in an expanded or foamed bed, preferably an expanded bed as described in US Pat. No. 2,987,465 (Johanson). As already stated, the hydrogen treatment is controlled so that a coal liquefaction product with an ash removal index of about 10 to 18 is obtained. The hydrogen treatment is known to reduce the sulfur and nitrogen content of the liquid coal product obtained.

A coal liquefaction product, consisting of a liquid coal extract of dissolved carbonaceous materials in the coal liquefaction solvent and ? ^ Insoluble material (ash and undissolved coal) is withdrawn from the liquefaction zone lh through line 15, and introduced into a separation zone 16, where from the coal liquefaction product at least the Materials are separated which-up to the 95 VolL - ^ - distillation temperature of the liquid 7, which was used to accelerate and intensify the separation of insoluble material. The deposition zone 16 may contain an atmospheric or vacuum evaporation chamber or tower; As specifically described, the deposition zone 16 is operated to separate the components which boil up to about 288 ° C.

A Kohleverflüssigungsprodokty which is free of the components up to about 288 C boiling _r is -and withdrawn from the separation zone through line Io 17th in line 21

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with a promoter fluid of controlled aromaticity mixed; i.e. the characterization factor of the promoter liquid has a value which is generally at least 0.25 Units greater than the characterization factor of the coal liquefaction solvent is. As specifically described, the promoter liquid is a fraction of kerosene which 5 vol. # And 95 vol. $ Distillation temperatures in the range from about 22o to 26o C and comes from a phenolic or paraffinic crude oil.

The combined stream of coal liquefaction product and the promoter liquid in line 22 goes to the gravity separation zone 23 introduced, which consists of a gravity separator of the type known in the literature, where an upper stream practically free of solids is separated from a lower stream containing the solids will. In principle, any known gravity separator can be used, but preferably a special one Type as it was developed for the present invention (see application S.N. 3o4 319 of November 7, 1972).

The upper stream practically free of insoluble material is withdrawn from the separation zone 23 through line Zh and introduced into a recovery zone 25 where the promoter liquid and various fractions of the coal extract are recovered. The recovery zone 25 can consist of one or more fractionators through which various fractions are distilled off from the product. As specifically described, the recovery zone is operated so that the following fractions are isolated: 1. A fraction with a 5 volume and 95 volume distillation temperature of 42o to k60 ° C, which is used as a promoter liquid for amplification and Accelerating the separation of solids from the coal liquefaction product is used; 2. A fraction (k6o to 315 ° C) which

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used as a distillate-fuel mixture; 3 · A fraction (315 to 482 ° C), part of which can be used as coal liquefaction solvent in line 12 and another part can be recovered as product; H. A residue (+ 482 c) with low ash and reduced sulfur content. The promoter liquid obtained in the recovery zone is mixed with the liquefaction product in line 17, and replenishment can be added through the line.

The stream withdrawn from separation zone 23 through line 3I below, which contains dispersed insoluble material, is introduced into an evaporation zone 3 ² where material boiling below 482 ° C. is evaporated and by conduit

33 is introduced into the recovery zone 25. The ashy one Evaporation residue in line 3 ^ can then be used for calcination or subject to coking. You can also use part of the evaporation residue as a starting material for a use partial oxidation process to produce hydrogen. Another alternative is that one can use part of the evaporation residue as operating fuel. These uses and others are for those skilled in the art are readily apparent on the basis of the invention described in the present application. According to the present Invention contains the evaporation residue in line

34 about 10 to 30 weight percent of the MAF coal. Also contains the carbon product (the product obtained from zones 16 and 25, excluding the liquefying solvent and the promoter liquid) less than 0.05 wt% insoluble material.

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The low ash, reduced sulfur residue (+ 482 ° C) withdrawn from recovery zone 25 through line 2k can be introduced into a hydrotreating zone kl to further reduce its sulfur content. The hydrogen treatment is carried out in the absence of a pasting or liquefying solvent in a known manner with hydrogen gas which is introduced through the line k2 . The hydrogen treatment is generally effected in the presence of a suitable hydrodesulfurization catalyst, for example at a temperature of about 315 to 55 ° C. and a pressure of about 70 to 210 atmospheres. The hydrotreated product with a further reduced sulfur content is withdrawn from the zone kl through the line kj and used as a fuel with a low sulfur content or in a mixture with such fuels.

The present invention is illustrated in the following examples explained in more detail, without this being restricted to this. Unless otherwise stated, all parts refer to and percentages on weight.

For example

ko wt .-% bituminous coal and 60 wt. 56 of a 315 to 482 C-coal tar distillate are entered together with hydrogen from above into a catalytic reactor with an expanded bed, which is a mixture of cobalt and nickel Mo lybdate contains in sulfide form as a catalyst. The temperature is 42o to 455 ° C, the pressure 98 atm, the flow rate 2.3 hours; the hydrogen feed 23 SCF / Ib. Money. The coal product has a ash removal index of 12.8.

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The coal liquefaction product is freed from ashes;, by you put it in a 150 ml Ktrast stoff flask using a kerosene boiling in the range of 22o - 26o ° C (K »11.9) at a promoter liquid / carbon solution weight ratio of o.75 can be deposed. Sas settling is at a temperature of 177 ° C and a pressure of 0 atu »where the settling time is 3 * 8 hours and a current is drawn from above which is about $ 75 of the starting material.

The ash removal (based on the current withdrawn above) is greater than> 99.7 $ «nd the loss of + 455 ° C MAF carbon less than - <C27 $ (based on MAF carbon feedstock).

example

ko wt .- ^ bituminous coal and 6o wt .- # of a 315 to 48 * ° C coal-tar distillate are placed together with ¥ hydrogen from above into a catalytic reactor with an expanded bed, the cobalt molybdate in sulfide form contains as a catalyst. The temperature is 415 ° -35 ° C., the pressure 98 atmospheres, the flow rate 0.98 hours, the hydrogen supply 25 SCF / lb. coal. The coal product has a degas index of 3.22.

The coal liquefaction product is freed from ashes by allowing it to settle in a 1500 ml plastic flask using a kerosene boiling in the range of 22o - 260 C (Κ = 11 »9) at a weight ratio of promoter liquid / coal solution of 0.75. The deposition is carried out atm at a temperature of I77 ⁰ C and a pressure of 0, where the settling time is 3.8 hours and above, a current is removed, which makes up about 75 $ of the starting material.

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The ais removal (based on the current withdrawn above) is greater than> 96.5 # and the loss of + * »55 ° C-MAF ~ coal
less than <$ 18 (based on MAF carbon feedstock).

This example shows that the distance of the sight is not optimal is when the ash removal index is below the inventive Range.

Example 3

^ o% by weight of bituminous coal and 60% by weight of a 315 - ^ 82 ° C coal-tar distillate are passed from above, together with hydrogen, into a catalytic reactor with an expanded bed, which contains cobalt molybdate in sulphide form contains as a catalyst, the temperature is * H5 to ^ 35 ° C, the pressure 8k atü, the flow rate 1.32 hours ~, the hydrogen supply
25 SCP / Lb. Money. The KoEil product has a ash removal index of 7

The charcoal liquefaction product is ashed by placing it in a 150 ml plastic flask
a kerosene boiling in the range of 22o - 26o ° G (K = II.9) at a weight ratio of promoter liquid / carbon solution of 0.75. Settling is carried out at a temperature of 177 ° C. and a pressure of 0 atmospheres, the settling time being 3 »8 hours, and a stream being drawn off at the top which amounts to about 8 k <^> of the starting material.

The ash removal (based on the current withdrawn above) is $ 97.75.

This example shows that ash removal is not optimal is when the ash removal index is below the inventive. Range.

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Be ispiel k

* 10% by weight of bituminous coal and 60% by weight of a 315 - 482 ° C coal-tar distillate are passed from above into a catalytic reactor with an expanded bed, together with hydrogen. * The cobalt-molybdate in sulphide form contains as catalyst "the temperature is 4Io -. hjo C ₉ of the printing Sk ATII, di © Durchflußgeschwindlgkeit 3 _S 96 Std" ₉ the hydrogen supply 25 SCP / lb, coal «. The eofel product features an entase huags index of 28.

The coal liquefaction product is freed Ύ & η grayling by allowing it to settle in a 1500 ml plastic flask using kerosene boiling in the range of 22o - 26o G (K = Il.9) at a weight ratio of promoter liquid / coal solution of 0.75. Settling is carried out at a temperature of 177 C and a pressure of 0 atu, the settling time being 388 hours and a current is drawn which makes up about 2% of the starting material.

The ash removal (based on the stream withdrawn above) is greater than> 99 $ o and the loss of hh 455 ° C MAF coal is less than £ 33 »^ $ (based on MAP coke starting material).

This example shows that the loss of + ^ 55 ° C product is not optimal if the ash removal index is above the range according to the invention.

The present invention is particularly advantageous because the coal liquefaction is carried out in a manner which making the subsequent removal of insoluble material optimal by maximizing the removal of ash and loss of potentially valuable coal products becomes minimal.

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Numerous modifications are in keeping with the above and variations of the present invention are possible, so that within the scope of the claims the invention is also different can be performed as specifically described.

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Claims (7)

Claims 1. A method for liquefying coal, characterized in that cabbage © hydrogenated in Gegenwai-ΐ a coal liquefaction solvent, so that. to be liquefied, wherein the hydrogenation is so controlled as to obtain a coal liquefaction product _S which is released from the carbonaceous material in the coal liquefaction solvent and insoluble material dispersed in the liquefying agent and having a Entaschungsindex of about Io to 18, wherein Ash removal index s Ια © χ parts by weight of ash-free benzene-insolubles in the product Geitfichtieile moisture-ash-free carbonaceous material dissolved and dispersed in the charcoal liquid solvent, 2. The method according to claim 1, characterized in that on the hydrogenation is carried out at a temperature of about 371 to 482 ° C " 3. Process according to Claim 2, characterized in that the hydrogenation is carried out at a flow rate of about 1.o to J *, o St. " ¹ . k. Process according to Claim 3s> characterized in that the hydrogenation is carried out in the presence of a catalyst. 5. Process according to claim h, characterized in that the hydrogenation is carried out in a foamed bed of this catalyst operated from above. - 23 - 409828/1096 2383064 6. The method according to claim 5 ₁ characterized gekennsgichust- that the pasting solvent in the range of about 315 to 482 - C boils. 7. Method according to Aaspriach 6 ₅ dadareb, geis © Eaas © iciiii®'fe _s that the ash removal index is about Ii to 15 « 409828/1096 Blank page