CA1074082A - Process for the agglomeration of fines, in particular coal fines - Google Patents
Process for the agglomeration of fines, in particular coal finesInfo
- Publication number
- CA1074082A CA1074082A CA240,491A CA240491A CA1074082A CA 1074082 A CA1074082 A CA 1074082A CA 240491 A CA240491 A CA 240491A CA 1074082 A CA1074082 A CA 1074082A
- Authority
- CA
- Canada
- Prior art keywords
- fines
- bitumen
- coal
- weight
- agglomeration
- 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
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L5/00—Solid fuels
- C10L5/02—Solid fuels such as briquettes consisting mainly of carbonaceous materials of mineral or non-mineral origin
- C10L5/06—Methods of shaping, e.g. pelletizing or briquetting
- C10L5/10—Methods of shaping, e.g. pelletizing or briquetting with the aid of binders, e.g. pretreated binders
- C10L5/14—Methods of shaping, e.g. pelletizing or briquetting with the aid of binders, e.g. pretreated binders with organic binders
- C10L5/16—Methods of shaping, e.g. pelletizing or briquetting with the aid of binders, e.g. pretreated binders with organic binders with bituminous binders, e.g. tar, pitch
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Working-Up Tar And Pitch (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Coke Industry (AREA)
Abstract
A B S T R A C T
A process for the agglomeration of fines in slurry or powder form by means of a mineral oil product dispersed in water, characterized in that from 5-15% by weight, based on anhydrous fines, of a bitumen emulsion is added to the fines, the bitumen having a penetration at 25°C below 5 and a Conradson value over 35. The resulting granulated product has a excellent non-dusty properties.
A process for the agglomeration of fines in slurry or powder form by means of a mineral oil product dispersed in water, characterized in that from 5-15% by weight, based on anhydrous fines, of a bitumen emulsion is added to the fines, the bitumen having a penetration at 25°C below 5 and a Conradson value over 35. The resulting granulated product has a excellent non-dusty properties.
Description
~07408~
The present invention relates to a process for the agglomeration of fines, in particular coal fines, in slurry or powder form by means of a mineral oil product dispersed in water.
The process can, e.g., be applied to aqueous coal slurries or coal fines containing waste water from the washing treatment and in that case facilitates the sub-sequent separation of the water in a known manner, for example by centrifugation; it can likewise be applied to concentrated slurries or dry dust. In each case the process yields an excellent granular, non-dusty product.
The invention therefore relates to a process for the agglomeration of fines in slurry or powder form by means of a mineral oil product dispersed in water, characterized in that from 5-15% by weight, based on anhydrous fines, of a bitumen emulsion is added to the fines, the bitumen having a penetration at 25C below 5 and a Conradson value over 35. In the preferred em-bodiment ~ the process a bitumen emulsion is utilized which contains as emulsifier a minor proportion, prefer-ably 1-10% by weight based on the proportion of bitumen, of alkaline metal naphthenate.
Preferred fines are coal fines, although this process can also be used for the agglomeration of other fines, such as coke fines, iron fines, sponge iron fines from steel works, ores, such as iron ores. If desirable the ~o7~0~2 granules can be briquetted. Heat treatments can be applied as well. In general 3 mineral fines are preferred.
The recovery and utilization of the portion of fines, in particular those obtained during the production and preparation of coal has always been a problem for the mining industry. With the increasing mechanization in the fields of working and transport the output of fines is growing, as a result of which this problem is being aggravated. The effluents from the washing treatment entrain a lot of coal dust and have to be purified in settling basins and/or centrifuges. The resultant slurries are partly worked up further, at any rate dewatered by means of centrifuges or vacuum filters and nevertheless only yield a dusty, low-grade coal with limited applications.
The same applies to the more or less dry coal dust which is additionally obtained in major quantities.
Several processes are known which facilitate the separation of water from the coal slurries. For example, in the Convertol process and in the newer Olifloc process, mineral oil fractions, namely light or heavy fuel oil, are admixed to the slurries. They act simultaneously as flotation agents for the working-up treatment and as flocculation agents for dewatering the slurries. However, the incorporation of the mineral oil requires special equipment, and the addition of mineral oil has no detect-able effect on the consistency o' the resultant coal fines.
~' .
~ : ' ~7408Z
This also applies to the Esso Research Engineering Company's process (U.K. patent specifications 1,041,547 and 1,123,597), in which relatively low-boiling hydro-carbons are used as pure flotation agents. In this process the addition of liquid surfactants, such as long-chain alcohols, is also suggested. It is then obvious to employ the mineral oil fraction in dispersed form from the beginning, as is in fact known from the process according to U.K. patent specification 1,351,986. This process, however, is not intended for coal fines but for the sludges obtained during bi~ogical sewage purification.
Whereas these known processes are based on liquids which are not water-miscible and which selectively wet coal particles, it has now been found that the corre-sponding flocculation effect can also be achieved with solid bitumen. An admixture of approximately 5-15% by weight, based on anhydrous fines, of bitumen emulsion to the coal fines-containing waste waters or slurries produces a satisfactory flocculation, as a result of which the subsequent removal of water, for example by means of screen-type centrifuges, can be appreciably facilitated.
Suitable bitumens have a Ring and Ball softening point of at least 100C. Although straight-run bitumen can be used, the residue from a thermal cracking treat-1(~74~8Z
ment, brought to the stated specification by high-vacuum distillation, is preferred.
The advantage of the process according to the invention resides in that the dewatered fines, in particular coal fines, agglomerate or granulate durably and are thereby more versatile and more readily applic-able than the coal dust obtained in the customary manner.
For example, the flotation concentrate from a hard-coal washing treatment was, on the one hand, dewatered in the conventional manner over vacuum filters (A), and, on the other hand, prior to dewatering was agglomerated by the addition of 15% by weight, based on anhydrous coal, of a special bitumen emulsion (B). The emulsiom contained approximately 50% by weight of a bitumen having a PEN/25 of 1-2 and a Conradson value of 40. The screen analysis produced the following results:
A B
below 0.2 mm 69% 5%
0.2-0.6 mm 24~ 19%
0.6-2.0 mm 4% 18%
over 2.0 mm 3% 58%
It was further found that the chemical nature of the emulsifier contained in the bitumen emulsion plays a role in the process. Especially the agglomerate formed in aqueous slurries can vary in its microscopic structure from spongy to coarse- grained. This process is affected 1~74~1BZ
very considerably by the emulsifier. A granulated micro-structure means better settling of the agglomerated slurry, more rapid and more complete dewatering in the centrifuge and, in particular, a considerable increase in the filtering rate, in the event of the slurry being dewatered over vacuum filters.
Most emulsifiers generally used for bitumen emulsions, which emulsifiers essentially comprise alkaline soaps of higher fatty acids, are only moderately suitable in this respect. On the other hand, very good results were ob-tained with a special emulsion which had been prepared with, e.g., 3% by weight, based on the proportion of bitumen, of alkaline metal naphthenate. The naphthenates in question are the salts of the higher molecular naph-thenic acids, which preferably have approximately thesame boiling range as the lubricating oil fractions.
Generally, in the vacuum distillation of naphthenic mineral oil these acids are neutralized in the column using caustic soda or caustic potash solution and with-drawn as a side-fraction. The raw product contains, for example, approximately 50% of unsaponifiable material, 25%
of alkaline naphthenate and 25% of water and excess alkali.
The naphthenate is suitably employed in the raw state, being dispersed with the calculated amount of water and the calculated amount of bitumen without further additives being incorporated in this dispersion in a known manner.
1~740~Z
By way of example, filtration tests were carried out with a coal slurry containlng 20% by weight of dry matter having a grain composition as indicated above (A). This was compared with the same slurry, agglomer-ated with 15~ by weight, based on dry matter, of a specialbitumen emulsion as described above (B); this emulsion contained a commercial-grade emulsifier consisting essentially of alkaline soaps of higher fatty acids.
In the further comparison a corresponding emulsion was used which had been prepared with approximately 3% by weight of alkaline naphthenate in the described manner (C). The following table shows the times in seconds in which under identical conditions identical amounts of filtrate had passed.
A B C
20 ml of filtrate 34 117 11 sec.
40 ml of filtrate 56 226 20 sec.
60 ml of filtrate 86 _ 33 sec.
The present process may be applied to more or less aqueous coal slurries. In each case it is sufficient to add the requisite amount of bitumen emulsion at room temperature to the slurry and mix intensively for a brief period, suitably in a continuous stirrer. The process may equally well be applied to dry coal dust, similarly by the addition of the requisite amount of bitumen emulsion at room temperature - elevated temper-::
~740~Z
atures generally produce worse results - and by brief, intensive mixing suitably in a worm-screw kneader designed for continuous operation. This process yields a granulate which is fully comparable to the above-described granulate formed in the aqueous phase. In the dry process as well, the chemical nature of the emulsifier has an effect, in addition to the consistency and origin of the emulsified bitumen. Under equal conditions the preferred alkaline naphthenate emulsions yield a better granulate, i.e., one having more uniform grain distribution and, in particular, less fine grains (below 0.2 mm) and coarse grains (over 5 mm), as the following comparative test shows.
Air-dry coal dust was intimately mixed in a kneader designed for continuous operation with 10% by weight of bitumen emulsion (approximately 50% by weight of bitumen).
The speed of the kneading screw was set at 105 rpm~
resulting in an average residence time in the trough of 5 minutes. The bitumen emulsion was sprayed on in the first tenth part of the mixing section. The screen analyses of the untreated coal dust (A) were compared with those of the dried granulates, which had been prepared, on the one hand, with a special bitumen emulsion as described above containing a commercial-grade emulsifier (B) and, on the other hand, with acorresponding emulsion which had been prepared in the described manner with approximately 3% by weight of alkaline naphthenate (C).
It is evident that the granulate C contains far less of the undesirable fine and coarse grains than the granulate B.
A B C
below 0.2 mm 52% 4% 2%
0.2-0.5 mm 35% 21% 14%
0.5-1.0 mm 10% 43% 38%
1.0-2.0 mm 2~ 21% 28%
The present invention relates to a process for the agglomeration of fines, in particular coal fines, in slurry or powder form by means of a mineral oil product dispersed in water.
The process can, e.g., be applied to aqueous coal slurries or coal fines containing waste water from the washing treatment and in that case facilitates the sub-sequent separation of the water in a known manner, for example by centrifugation; it can likewise be applied to concentrated slurries or dry dust. In each case the process yields an excellent granular, non-dusty product.
The invention therefore relates to a process for the agglomeration of fines in slurry or powder form by means of a mineral oil product dispersed in water, characterized in that from 5-15% by weight, based on anhydrous fines, of a bitumen emulsion is added to the fines, the bitumen having a penetration at 25C below 5 and a Conradson value over 35. In the preferred em-bodiment ~ the process a bitumen emulsion is utilized which contains as emulsifier a minor proportion, prefer-ably 1-10% by weight based on the proportion of bitumen, of alkaline metal naphthenate.
Preferred fines are coal fines, although this process can also be used for the agglomeration of other fines, such as coke fines, iron fines, sponge iron fines from steel works, ores, such as iron ores. If desirable the ~o7~0~2 granules can be briquetted. Heat treatments can be applied as well. In general 3 mineral fines are preferred.
The recovery and utilization of the portion of fines, in particular those obtained during the production and preparation of coal has always been a problem for the mining industry. With the increasing mechanization in the fields of working and transport the output of fines is growing, as a result of which this problem is being aggravated. The effluents from the washing treatment entrain a lot of coal dust and have to be purified in settling basins and/or centrifuges. The resultant slurries are partly worked up further, at any rate dewatered by means of centrifuges or vacuum filters and nevertheless only yield a dusty, low-grade coal with limited applications.
The same applies to the more or less dry coal dust which is additionally obtained in major quantities.
Several processes are known which facilitate the separation of water from the coal slurries. For example, in the Convertol process and in the newer Olifloc process, mineral oil fractions, namely light or heavy fuel oil, are admixed to the slurries. They act simultaneously as flotation agents for the working-up treatment and as flocculation agents for dewatering the slurries. However, the incorporation of the mineral oil requires special equipment, and the addition of mineral oil has no detect-able effect on the consistency o' the resultant coal fines.
~' .
~ : ' ~7408Z
This also applies to the Esso Research Engineering Company's process (U.K. patent specifications 1,041,547 and 1,123,597), in which relatively low-boiling hydro-carbons are used as pure flotation agents. In this process the addition of liquid surfactants, such as long-chain alcohols, is also suggested. It is then obvious to employ the mineral oil fraction in dispersed form from the beginning, as is in fact known from the process according to U.K. patent specification 1,351,986. This process, however, is not intended for coal fines but for the sludges obtained during bi~ogical sewage purification.
Whereas these known processes are based on liquids which are not water-miscible and which selectively wet coal particles, it has now been found that the corre-sponding flocculation effect can also be achieved with solid bitumen. An admixture of approximately 5-15% by weight, based on anhydrous fines, of bitumen emulsion to the coal fines-containing waste waters or slurries produces a satisfactory flocculation, as a result of which the subsequent removal of water, for example by means of screen-type centrifuges, can be appreciably facilitated.
Suitable bitumens have a Ring and Ball softening point of at least 100C. Although straight-run bitumen can be used, the residue from a thermal cracking treat-1(~74~8Z
ment, brought to the stated specification by high-vacuum distillation, is preferred.
The advantage of the process according to the invention resides in that the dewatered fines, in particular coal fines, agglomerate or granulate durably and are thereby more versatile and more readily applic-able than the coal dust obtained in the customary manner.
For example, the flotation concentrate from a hard-coal washing treatment was, on the one hand, dewatered in the conventional manner over vacuum filters (A), and, on the other hand, prior to dewatering was agglomerated by the addition of 15% by weight, based on anhydrous coal, of a special bitumen emulsion (B). The emulsiom contained approximately 50% by weight of a bitumen having a PEN/25 of 1-2 and a Conradson value of 40. The screen analysis produced the following results:
A B
below 0.2 mm 69% 5%
0.2-0.6 mm 24~ 19%
0.6-2.0 mm 4% 18%
over 2.0 mm 3% 58%
It was further found that the chemical nature of the emulsifier contained in the bitumen emulsion plays a role in the process. Especially the agglomerate formed in aqueous slurries can vary in its microscopic structure from spongy to coarse- grained. This process is affected 1~74~1BZ
very considerably by the emulsifier. A granulated micro-structure means better settling of the agglomerated slurry, more rapid and more complete dewatering in the centrifuge and, in particular, a considerable increase in the filtering rate, in the event of the slurry being dewatered over vacuum filters.
Most emulsifiers generally used for bitumen emulsions, which emulsifiers essentially comprise alkaline soaps of higher fatty acids, are only moderately suitable in this respect. On the other hand, very good results were ob-tained with a special emulsion which had been prepared with, e.g., 3% by weight, based on the proportion of bitumen, of alkaline metal naphthenate. The naphthenates in question are the salts of the higher molecular naph-thenic acids, which preferably have approximately thesame boiling range as the lubricating oil fractions.
Generally, in the vacuum distillation of naphthenic mineral oil these acids are neutralized in the column using caustic soda or caustic potash solution and with-drawn as a side-fraction. The raw product contains, for example, approximately 50% of unsaponifiable material, 25%
of alkaline naphthenate and 25% of water and excess alkali.
The naphthenate is suitably employed in the raw state, being dispersed with the calculated amount of water and the calculated amount of bitumen without further additives being incorporated in this dispersion in a known manner.
1~740~Z
By way of example, filtration tests were carried out with a coal slurry containlng 20% by weight of dry matter having a grain composition as indicated above (A). This was compared with the same slurry, agglomer-ated with 15~ by weight, based on dry matter, of a specialbitumen emulsion as described above (B); this emulsion contained a commercial-grade emulsifier consisting essentially of alkaline soaps of higher fatty acids.
In the further comparison a corresponding emulsion was used which had been prepared with approximately 3% by weight of alkaline naphthenate in the described manner (C). The following table shows the times in seconds in which under identical conditions identical amounts of filtrate had passed.
A B C
20 ml of filtrate 34 117 11 sec.
40 ml of filtrate 56 226 20 sec.
60 ml of filtrate 86 _ 33 sec.
The present process may be applied to more or less aqueous coal slurries. In each case it is sufficient to add the requisite amount of bitumen emulsion at room temperature to the slurry and mix intensively for a brief period, suitably in a continuous stirrer. The process may equally well be applied to dry coal dust, similarly by the addition of the requisite amount of bitumen emulsion at room temperature - elevated temper-::
~740~Z
atures generally produce worse results - and by brief, intensive mixing suitably in a worm-screw kneader designed for continuous operation. This process yields a granulate which is fully comparable to the above-described granulate formed in the aqueous phase. In the dry process as well, the chemical nature of the emulsifier has an effect, in addition to the consistency and origin of the emulsified bitumen. Under equal conditions the preferred alkaline naphthenate emulsions yield a better granulate, i.e., one having more uniform grain distribution and, in particular, less fine grains (below 0.2 mm) and coarse grains (over 5 mm), as the following comparative test shows.
Air-dry coal dust was intimately mixed in a kneader designed for continuous operation with 10% by weight of bitumen emulsion (approximately 50% by weight of bitumen).
The speed of the kneading screw was set at 105 rpm~
resulting in an average residence time in the trough of 5 minutes. The bitumen emulsion was sprayed on in the first tenth part of the mixing section. The screen analyses of the untreated coal dust (A) were compared with those of the dried granulates, which had been prepared, on the one hand, with a special bitumen emulsion as described above containing a commercial-grade emulsifier (B) and, on the other hand, with acorresponding emulsion which had been prepared in the described manner with approximately 3% by weight of alkaline naphthenate (C).
It is evident that the granulate C contains far less of the undesirable fine and coarse grains than the granulate B.
A B C
below 0.2 mm 52% 4% 2%
0.2-0.5 mm 35% 21% 14%
0.5-1.0 mm 10% 43% 38%
1.0-2.0 mm 2~ 21% 28%
2.0-3.2 mm 1% 3% 9%
3.2-5.0 mm - 3% 6%
over 5.0 mm - 5~ 3%
It should be mentioned that the preferred special emulsion, containing a bitumen having a PEN/25C below 5 and a Conradson value over 35, as well as alkaline -naphthenate as emulsifier, is not a standard product, does not conform to any standard and is not suitable for most applications, for examp~e in road construction.
In the case ~ coal fines the agglomerated product is ready for use, e.g., for burning in power station boilers.
.
over 5.0 mm - 5~ 3%
It should be mentioned that the preferred special emulsion, containing a bitumen having a PEN/25C below 5 and a Conradson value over 35, as well as alkaline -naphthenate as emulsifier, is not a standard product, does not conform to any standard and is not suitable for most applications, for examp~e in road construction.
In the case ~ coal fines the agglomerated product is ready for use, e.g., for burning in power station boilers.
.
Claims
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for the agglomeration of fines in slurry or powder form by means of a mineral oil product dispersed in water, characterized in that from 5-15% by weight, based on anhydrous fines, of a bitumen emulsion is added to the fines, the bitumen having a penetration at 25°C below 5 and a Conradson value over 35.
2. A process as claimed in claim 1, wherein the bitumen emulsion contains from 1 to 10% by weight, based on the proportion of bitumen, of alkaline metal naphthenate.
3. A process as claimed in claim 1 or 2, wherein the fines are coal fines.
4. Agglomerates whenever prepared according to the process of
claim 1.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2459349A DE2459349C2 (en) | 1974-12-16 | 1974-12-16 | Process for agglomerating finely divided coal in sludge or powder form |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1074082A true CA1074082A (en) | 1980-03-25 |
Family
ID=5933509
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA240,491A Expired CA1074082A (en) | 1974-12-16 | 1975-11-26 | Process for the agglomeration of fines, in particular coal fines |
Country Status (7)
Country | Link |
---|---|
JP (1) | JPS592527B2 (en) |
BE (1) | BE836628A (en) |
CA (1) | CA1074082A (en) |
DE (1) | DE2459349C2 (en) |
FR (1) | FR2295120A1 (en) |
GB (1) | GB1473269A (en) |
ZA (1) | ZA757801B (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1575413A (en) * | 1976-12-03 | 1980-09-24 | Shell Int Research | Method for agglomeration of coal fines |
JPS5725392A (en) * | 1980-07-23 | 1982-02-10 | Hitachi Ltd | Storage of coal |
AT376147B (en) * | 1980-12-15 | 1984-10-10 | Gergely Gerhard | METHOD AND DEVICE FOR GRANULATING A POWDER MIXTURE |
JPS58167690A (en) * | 1982-03-27 | 1983-10-03 | Mitsui Eng & Shipbuild Co Ltd | Fluidization and discharge of granulated coal and apparatus therefor |
GB2138441A (en) * | 1983-04-18 | 1984-10-24 | British Gas Corp | Briquetting coal |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE508570C (en) * | 1927-04-04 | 1930-10-02 | Frank Ford Tapping | Process for briquetting powdery materials, especially fuels |
AT162039B (en) * | 1946-01-18 | 1949-01-10 | Walter Dipl Ing Otto | Process for the production of briquettes from lignite. |
DE885088C (en) * | 1951-06-19 | 1953-08-03 | Kamillo Dr-Ing Konopicky | Process for breaking up fine coal |
CH315099A (en) * | 1951-06-28 | 1956-07-31 | Eloed Egon Prof Ing Dr | Process for the production of briquettes from coal |
DE1571703B2 (en) * | 1966-08-31 | 1973-03-01 | Metallgesellschaft AG, 6000 Frank fürt | PROCESS FOR MANUFACTURING COCKSHOLE BODIES |
GB1351986A (en) * | 1971-07-15 | 1974-05-15 | Shell Int Research | Dewatering of aqueous suspensions of organic waste material |
GB1388371A (en) * | 1972-04-14 | 1975-03-26 | Shell Int Research | Separation process for solid material |
-
1974
- 1974-12-16 DE DE2459349A patent/DE2459349C2/en not_active Expired
-
1975
- 1975-11-26 CA CA240,491A patent/CA1074082A/en not_active Expired
- 1975-12-15 ZA ZA757801A patent/ZA757801B/en unknown
- 1975-12-15 BE BE162732A patent/BE836628A/en not_active IP Right Cessation
- 1975-12-15 GB GB5124875A patent/GB1473269A/en not_active Expired
- 1975-12-15 FR FR7538325A patent/FR2295120A1/en active Granted
- 1975-12-15 JP JP50148556A patent/JPS592527B2/en not_active Expired
Also Published As
Publication number | Publication date |
---|---|
BE836628A (en) | 1976-06-15 |
ZA757801B (en) | 1976-11-24 |
DE2459349C2 (en) | 1986-04-10 |
FR2295120A1 (en) | 1976-07-16 |
AU8754475A (en) | 1977-06-23 |
FR2295120B1 (en) | 1980-01-25 |
GB1473269A (en) | 1977-05-11 |
JPS592527B2 (en) | 1984-01-19 |
JPS5186086A (en) | 1976-07-28 |
DE2459349A1 (en) | 1976-06-24 |
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Legal Events
Date | Code | Title | Description |
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MKEX | Expiry |