CA1153328A - Method for hydrogenating coal - Google Patents
Method for hydrogenating coalInfo
- Publication number
- CA1153328A CA1153328A CA000378850A CA378850A CA1153328A CA 1153328 A CA1153328 A CA 1153328A CA 000378850 A CA000378850 A CA 000378850A CA 378850 A CA378850 A CA 378850A CA 1153328 A CA1153328 A CA 1153328A
- Authority
- CA
- Canada
- Prior art keywords
- separator
- hot
- product
- distillate
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
- C10G1/083—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts in the presence of a solvent
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Abstract of the Disclosure The invention relates to a method for hydrogenating coal whereby finely crushed coal is stirred into a slurry with a pasting oil. The slurry is pressurized and heated in heat-exchange with hydrogenation products from the top of a hot-separator, and then, by the application of external heat, to the hydrogenation scorching temperature. It is then subjected, in the presence of hydrogen, to catalytically-accelerated hydrogenation. Thus, the hydrogenation product is broken down in at least one hot-separator into a top-product in vapour form and a bottom-product containing a heavy, fluid-distillate oil, non-distillable components, and solids. In accordance with the invention, at least some of the distillate-oil, separated from the bottom-product in the hot-separator, is returned to the hot-separator.
Description
~153328 The invention relates to a method for hydrogenating coal, whereby finely crushed coal is stirred into a slurry with a pasting oil, is pressurized, is heated in heat-exchange with hydrogenation products from the top of the hot-separator and then, by the application of external heat, to the hydro-genation scorching temperature, whereupon it is subjected, in the presence of hydrogen, to catalytically-accelerated hydro-genation' and whereby the hydrogenation product is broken down, in at least one hot separator, into a vaporous top-product and a bottom-product containing a heavy, fluid, distillate oil, non-distilIable components, and solids.
In hydrogenating coal by one method of the type men-tioned above, the top-product from the hot-separator, which contains, in addition to hydrocarbon vapours from the coal, as far as the middle-oil range, unconsumed hydrogen and water-vapour, among other things, is first of all cooled, before pro-cessing in several distilling stages, initially in heat-exchange with fresh coal-slurry to be hydrogenated. In this way, a con-siderable amount of the exothermal reaction-heat arising during hydrogenation may be used directly for heating the coal-slurry.
The larger the amount of this heat, the less additional outside heat required, i.e. the more economical the hydrogenating process.
The most economical conditions would be obtained by operating the hot-separator at the temperature of the hydro-genating reactor (about 475C), since in this case the largest amount of top-product, at the highest temperature, would be available for heat-exchange with the fresh coal-slurry.
It has been found, however, at the hydrogenating-reactor temperatures, unwanted carbonization and baking-on -occurs on the inner wall of the hot-separator, especially near the bottom. After a short time, this greatly impairs, or ~1533Z8 altogether prevents, the functioning of the hot-separator.
In order to avoid these problems in the hot-separator, it is known to cool the hydrogenation-products leaving the reactor, before they enter the hot-separator, in an additional heat-exchanger, to a temperature at which carbonization and deposits no longer occur. Cf., in this connection, "~ompendium 76/77, DGMK Reports at the 4th OGEW/DGMK meeting from October 4th to 6th in Salzburg, Industrieverlag von Herrenhausen KG, 1976, pages 273-383.
One`of the disadvantages of this intermediate cooling, however, is that distillate-oils leaving the hydro-genating reactor condense out in the form of vapour and collect in the bottom of the hot-separator, together with higher-boiling-point distillate-oils, the non-distillable hydrogenation-residue, and solids such as unconsumed coil, ash, and catalyst particles. Renewed separation of these heavy distillate-oils from the bottom-product is relatively costly. Furthermore, the amount of hot-separator top-product available for heat-exchange with fresh coal-slurry is de-creased by the amount condensed-out by the cooling. This leaves a smaller amount of top-product, at a lower temperature, available for heat-exchange with the fresh coal-slurry.
In addition to this, since the full amount of the hydrogenation-product flows through the heat-exchanger used for cooling it, this heat-exchanger is very costly and is also subject to carbonization and deposits.
It is therefore the purpose of the invention to develop a method for hydrogenating coai which makes it a simple matter to make available the largest possible amount of the exothermal reaction-heat produced in the hydrogenating - reactor for heating the fresh coal-slurry.
~53328 In the case of a method the type mentioned at the beginning hereof, this purpose is achieved, according to the invention, in that at least a part of the distillate-oils separated from the bottom-product is returned to the hot-separator.
The distillate-oils returned to the hot-separator result in dilution of the hot-separator bottomt so that no carbonization occurs here, even at high temperatures. In this connection, it has been found desirable to return only distillates having boiling points above the bottom-temperature, in order to prevent vapourization of the said distillates and thus renewed concentration of the bottom. According to another characteristic, the invention provides for the dis-tillation of distillate-oils from the bottom-product to be carried out by vacuum distillation, for the vacuum-oil-vapours ~ thus produced to be subjected to fractionated condensation ; in at least two stages, and for at least a part of the heavy distillate-oil fraction to be returned to the hot-separator without further cooling.
It has been found to be particularly advantageous to distribute the returned distillate-oils uniformly over the inner wall of the hot separator. A thin protective and cleaning film occurs on the inner wall of the upper part of the hot-separator, as a result of the distillate-oil running down the wall, whereas a so-called sludge-dilution zone occurs in the wall-area of the sump. Surprisingly enough it has been found that the film and dilution-zone prevent any baking-on or carbonization on the wall itself, even at high temperatures.
The return and distribution of distillate-oils may be effected by providing, in the upper part of the hot-separator, a ring-line comprising equally spaced apertures.
~lS3328 The method according to the invention thus makes it possible to dispense with cooling of the hydrogenation product before it enters the hot-separator, i.e. this can be operated on the steam side at the full temperature of the hydrogenating reactor (about 475~C). As a result of this, a maximal amount of top-product, at the highest possible temperature, is avail-able for heat-exchange between the top-product and the fresh coal-slurry, for heating the said slurry, and the additional outside heat required to heat the slurry is reduced to a minimum. This provides a considerable improvement in heat-balance.
In accordance with a particular embodiment of the invention there is provided a method for hydrogenating coal, whereby finely crushed coal is stirred into a slurry with a pasting oil, is pressurized, is heated in heat-exchange with hydrogenation products from the top of a hot-separator and then, by the application of external heat, to the hydrogen-ation scorching temperature, whereupon it is subjected, in the presence of hydrogen, to catalytically-accelerated hydro-genation, and whereby the hydrogenation product is broken down, : in at least one hot-separator, into a top-product in vapour form and a bottom product containing a heavy, fluid distillate-oil, non-distillable components, and solids, characterized in that at least some of the distillate-oil, separated from - the bottom-product in the hot-separator, is returned to the said hot-separator.
The invention is explained hereinafter in greater detail in conjunction with the example of embodiment illus-trated diagrammatically in the figure attached hereto The said figure illus rates a method for hydro-! genating coal in which finely crushed coal is passed through .
~153328 a line 1, an iron-oxide catalyst is passed through a line 2, and pasting oil is passed through a line 3 to a container 4 where it is thoroughly stirred to form a slurry. ~y means of a pump 6, this slurry is raised to the hydrogenating pressure of about 300 bars. It is initially heated, in a heat-exchanger, with hot hydrogenation product, to a temperature of about 400C
and then, in an externally heated tubular furnace, to the scorching temperature of hydrogenation, namely about 430C.
The necessary hydrogen is passed to the coal-slurry through ; 10 a line 6.
The coal is hydrogenated in reaction-chamber 8 at an average temperature of about 475C. The hydrogenation product obtained passes to a hot-separator 9 from the top of which steam is removed at a temperature of about 475C and is passed through a line 10 to heat-exchanger 18. The sludge arising in the bottom of hot-separator 9, consisting of heavy distillate-oils, non-distillable fluid components, and solids, is passed, through a pressure-relieving valve 11, to a vacuum-distillation stage 12. The vacuum-residue and distillates are removed from the distilling unit through lines 13, 14 for further use.
According to the invention, the pressure of some of the heavy distillate-oil is raised, without further cooling, to that of hot-separator 9, to which it is returned through a line 16 and a ring-line 17 in the upper part of the said hot-separator. The feed.is such that the oil runs down the inner wall of the separator, thus producing a thin protective film on the wall in the upper part of the separator and a sludge-dilution zone in the sump-area, which prevents carbonization and baking-on the inner wall. Thus, on the steam side, hot-~53328 separator 9 can be operated at thq same temperature asreactor 8, i.e. at about 475C.
A maximal amount of top-product, at the highest temperature in the process, thus flows through line 10 to heat-exchanger 18.
,,~
In hydrogenating coal by one method of the type men-tioned above, the top-product from the hot-separator, which contains, in addition to hydrocarbon vapours from the coal, as far as the middle-oil range, unconsumed hydrogen and water-vapour, among other things, is first of all cooled, before pro-cessing in several distilling stages, initially in heat-exchange with fresh coal-slurry to be hydrogenated. In this way, a con-siderable amount of the exothermal reaction-heat arising during hydrogenation may be used directly for heating the coal-slurry.
The larger the amount of this heat, the less additional outside heat required, i.e. the more economical the hydrogenating process.
The most economical conditions would be obtained by operating the hot-separator at the temperature of the hydro-genating reactor (about 475C), since in this case the largest amount of top-product, at the highest temperature, would be available for heat-exchange with the fresh coal-slurry.
It has been found, however, at the hydrogenating-reactor temperatures, unwanted carbonization and baking-on -occurs on the inner wall of the hot-separator, especially near the bottom. After a short time, this greatly impairs, or ~1533Z8 altogether prevents, the functioning of the hot-separator.
In order to avoid these problems in the hot-separator, it is known to cool the hydrogenation-products leaving the reactor, before they enter the hot-separator, in an additional heat-exchanger, to a temperature at which carbonization and deposits no longer occur. Cf., in this connection, "~ompendium 76/77, DGMK Reports at the 4th OGEW/DGMK meeting from October 4th to 6th in Salzburg, Industrieverlag von Herrenhausen KG, 1976, pages 273-383.
One`of the disadvantages of this intermediate cooling, however, is that distillate-oils leaving the hydro-genating reactor condense out in the form of vapour and collect in the bottom of the hot-separator, together with higher-boiling-point distillate-oils, the non-distillable hydrogenation-residue, and solids such as unconsumed coil, ash, and catalyst particles. Renewed separation of these heavy distillate-oils from the bottom-product is relatively costly. Furthermore, the amount of hot-separator top-product available for heat-exchange with fresh coal-slurry is de-creased by the amount condensed-out by the cooling. This leaves a smaller amount of top-product, at a lower temperature, available for heat-exchange with the fresh coal-slurry.
In addition to this, since the full amount of the hydrogenation-product flows through the heat-exchanger used for cooling it, this heat-exchanger is very costly and is also subject to carbonization and deposits.
It is therefore the purpose of the invention to develop a method for hydrogenating coai which makes it a simple matter to make available the largest possible amount of the exothermal reaction-heat produced in the hydrogenating - reactor for heating the fresh coal-slurry.
~53328 In the case of a method the type mentioned at the beginning hereof, this purpose is achieved, according to the invention, in that at least a part of the distillate-oils separated from the bottom-product is returned to the hot-separator.
The distillate-oils returned to the hot-separator result in dilution of the hot-separator bottomt so that no carbonization occurs here, even at high temperatures. In this connection, it has been found desirable to return only distillates having boiling points above the bottom-temperature, in order to prevent vapourization of the said distillates and thus renewed concentration of the bottom. According to another characteristic, the invention provides for the dis-tillation of distillate-oils from the bottom-product to be carried out by vacuum distillation, for the vacuum-oil-vapours ~ thus produced to be subjected to fractionated condensation ; in at least two stages, and for at least a part of the heavy distillate-oil fraction to be returned to the hot-separator without further cooling.
It has been found to be particularly advantageous to distribute the returned distillate-oils uniformly over the inner wall of the hot separator. A thin protective and cleaning film occurs on the inner wall of the upper part of the hot-separator, as a result of the distillate-oil running down the wall, whereas a so-called sludge-dilution zone occurs in the wall-area of the sump. Surprisingly enough it has been found that the film and dilution-zone prevent any baking-on or carbonization on the wall itself, even at high temperatures.
The return and distribution of distillate-oils may be effected by providing, in the upper part of the hot-separator, a ring-line comprising equally spaced apertures.
~lS3328 The method according to the invention thus makes it possible to dispense with cooling of the hydrogenation product before it enters the hot-separator, i.e. this can be operated on the steam side at the full temperature of the hydrogenating reactor (about 475~C). As a result of this, a maximal amount of top-product, at the highest possible temperature, is avail-able for heat-exchange between the top-product and the fresh coal-slurry, for heating the said slurry, and the additional outside heat required to heat the slurry is reduced to a minimum. This provides a considerable improvement in heat-balance.
In accordance with a particular embodiment of the invention there is provided a method for hydrogenating coal, whereby finely crushed coal is stirred into a slurry with a pasting oil, is pressurized, is heated in heat-exchange with hydrogenation products from the top of a hot-separator and then, by the application of external heat, to the hydrogen-ation scorching temperature, whereupon it is subjected, in the presence of hydrogen, to catalytically-accelerated hydro-genation, and whereby the hydrogenation product is broken down, : in at least one hot-separator, into a top-product in vapour form and a bottom product containing a heavy, fluid distillate-oil, non-distillable components, and solids, characterized in that at least some of the distillate-oil, separated from - the bottom-product in the hot-separator, is returned to the said hot-separator.
The invention is explained hereinafter in greater detail in conjunction with the example of embodiment illus-trated diagrammatically in the figure attached hereto The said figure illus rates a method for hydro-! genating coal in which finely crushed coal is passed through .
~153328 a line 1, an iron-oxide catalyst is passed through a line 2, and pasting oil is passed through a line 3 to a container 4 where it is thoroughly stirred to form a slurry. ~y means of a pump 6, this slurry is raised to the hydrogenating pressure of about 300 bars. It is initially heated, in a heat-exchanger, with hot hydrogenation product, to a temperature of about 400C
and then, in an externally heated tubular furnace, to the scorching temperature of hydrogenation, namely about 430C.
The necessary hydrogen is passed to the coal-slurry through ; 10 a line 6.
The coal is hydrogenated in reaction-chamber 8 at an average temperature of about 475C. The hydrogenation product obtained passes to a hot-separator 9 from the top of which steam is removed at a temperature of about 475C and is passed through a line 10 to heat-exchanger 18. The sludge arising in the bottom of hot-separator 9, consisting of heavy distillate-oils, non-distillable fluid components, and solids, is passed, through a pressure-relieving valve 11, to a vacuum-distillation stage 12. The vacuum-residue and distillates are removed from the distilling unit through lines 13, 14 for further use.
According to the invention, the pressure of some of the heavy distillate-oil is raised, without further cooling, to that of hot-separator 9, to which it is returned through a line 16 and a ring-line 17 in the upper part of the said hot-separator. The feed.is such that the oil runs down the inner wall of the separator, thus producing a thin protective film on the wall in the upper part of the separator and a sludge-dilution zone in the sump-area, which prevents carbonization and baking-on the inner wall. Thus, on the steam side, hot-~53328 separator 9 can be operated at thq same temperature asreactor 8, i.e. at about 475C.
A maximal amount of top-product, at the highest temperature in the process, thus flows through line 10 to heat-exchanger 18.
,,~
Claims (4)
1. A method for hydrogenating coal, whereby finely crushed coal is stirred into a slurry with a pasting oil, is pressurized, is heated in heat-exchange with hydrogenation products from the top of a hot-separator and then, by the application of external heat, to the hydrogenation scorching temperature, whereupon it is subjected, in the presence of hydrogen, to catalytically-accelerated hydrogenation, and whereby the hydrogenation product is broken down, in at least one hot-separator, into a top-product in vapour form and a bottom product containing a heavy, fluid distillate-oil, non-distillable components, and solids, characterized in that at least some of the distillate-oil, separated from the bottom-product in the hot-separator, is returned to the said hot-separator.
2. A method according to claim 1, characterized in that the distillate-oils are separated from the bottom-product by vacuum-distillation, in that the resulting vacuum-oil-vapours are subjected to fractionated condensation in at least two stages, and in that at least a part of the heavy distillate-oil fraction is returned, without further cooling, to the hot-separator.
3. A method according to claim 2, characterized in that the distillate oils returned are distributed uniformly over the inner wall of the hot-separator.
4. A method according to claim 3, characterized in that distribution of the distillate-oils is effected by means of a ring-line provided with apertures and arranged in the upper part of the hot-separator.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP3021859.8-44 | 1980-06-11 | ||
| DE3021859A DE3021859C2 (en) | 1980-06-11 | 1980-06-11 | Process for hydrogenating coal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1153328A true CA1153328A (en) | 1983-09-06 |
Family
ID=6104339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000378850A Expired CA1153328A (en) | 1980-06-11 | 1981-06-02 | Method for hydrogenating coal |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JPS57500786A (en) |
| AU (1) | AU546261B2 (en) |
| CA (1) | CA1153328A (en) |
| DE (1) | DE3021859C2 (en) |
| GB (1) | GB2090283B (en) |
| WO (1) | WO1981003661A1 (en) |
| ZA (1) | ZA813800B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU576488B2 (en) * | 1983-03-07 | 1988-09-01 | Hri Inc. | Coal hydrogenation and liquefaction thereof |
| US5603760A (en) * | 1995-09-18 | 1997-02-18 | W. R. Grace & Co.-Conn. | Cement admixture capable of inhibiting drying shrinkage and method of using same |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE874439C (en) * | 1944-01-04 | 1953-04-23 | Basf Ag | Process for the pressure hydrogenation of carbons, tars and mineral oils using several heat exchangers connected in series |
| US3841981A (en) * | 1972-12-29 | 1974-10-15 | Hydrocarbon Research Inc | Hydrogenation of tar sand bitumen |
| DE2803916C2 (en) * | 1978-01-30 | 1983-11-17 | Saarbergwerke AG, 6600 Saarbrücken | Process for liquefying coal |
-
1980
- 1980-06-11 DE DE3021859A patent/DE3021859C2/en not_active Expired
-
1981
- 1981-06-02 CA CA000378850A patent/CA1153328A/en not_active Expired
- 1981-06-08 ZA ZA00813800A patent/ZA813800B/en unknown
- 1981-06-11 WO PCT/DE1981/000087 patent/WO1981003661A1/en unknown
- 1981-06-11 GB GB8201490A patent/GB2090283B/en not_active Expired
- 1981-06-11 JP JP56502077A patent/JPS57500786A/ja active Pending
- 1981-06-11 AU AU73222/81A patent/AU546261B2/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| GB2090283A (en) | 1982-07-07 |
| ZA813800B (en) | 1982-06-30 |
| JPS57500786A (en) | 1982-05-06 |
| AU7322281A (en) | 1982-01-07 |
| WO1981003661A1 (en) | 1981-12-24 |
| DE3021859C2 (en) | 1982-05-19 |
| DE3021859A1 (en) | 1981-12-17 |
| AU546261B2 (en) | 1985-08-22 |
| GB2090283B (en) | 1983-06-22 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |