EP0258426B1 - Process for producing an additive for lubricants and for aqueous heating agents and fuels - Google Patents

Process for producing an additive for lubricants and for aqueous heating agents and fuels Download PDF

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Publication number
EP0258426B1
EP0258426B1 EP87902076A EP87902076A EP0258426B1 EP 0258426 B1 EP0258426 B1 EP 0258426B1 EP 87902076 A EP87902076 A EP 87902076A EP 87902076 A EP87902076 A EP 87902076A EP 0258426 B1 EP0258426 B1 EP 0258426B1
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Prior art keywords
additive
cane sugar
lubricants
pct
fuel
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German (de)
French (fr)
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EP0258426A1 (en
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Kurt Bertram
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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
    • C10L10/00—Use of additives to fuels or fires for particular purposes
    • C10L10/02—Use of additives to fuels or fires for particular purposes for reducing smoke development
    • 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
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • 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
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/32—Liquid carbonaceous fuels consisting of coal-oil suspensions or aqueous emulsions or oil emulsions
    • C10L1/328—Oil emulsions containing water or any other hydrophilic phase
    • 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
    • C10L10/00—Use of additives to fuels or fires for particular purposes
    • C10L10/08—Use of additives to fuels or fires for particular purposes for improving lubricity; for reducing wear
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
    • C10M145/40—Polysaccharides, e.g. cellulose

Definitions

  • the invention relates to a process for the preparation of an additive for lubricants and for aqueous fuel systems and heating agents, in which an alkaline aqueous solution of an inverted cane sugar as the main component with a content of a hydrocarbon and an alcohol is heated and cooled thereon, and the uses mentioned above.
  • the invention was based on the object of improving the method mentioned at the outset in such a way that it enables simple and flexible production of the desired process product.
  • this object is achieved in that cane sugar of an inversion sugar of about 55 to 75% is used and heated to about 75 to 100 ° C. until a roton color tone is formed.
  • the essence of the invention is therefore that no fully inverted cane sugar is used, but that a degree of inversion of approximately 55 to 75%, particularly preferably approximately 60 to 70% and particularly preferably approximately 66% leads to the desired results .
  • a degree of inversion of approximately 55 to 75%, particularly preferably approximately 60 to 70% and particularly preferably approximately 66% leads to the desired results .
  • Particularly favorable properties are obtained in the process product if it is kept at about boiling temperature, in particular about 100 ° C., for some time in order to adjust the red color mentioned.
  • the temperature of 100 ° C should not be exceeded if possible. After heating, it is cooled to room temperature.
  • the starting material for the product produced according to the invention is always a concentrated aqueous solution of the sugar cane of the degree of inversion mentioned.
  • the concentration of this cane sugar should advantageously be at least 50% by weight, in particular close to the degree of saturation. Particularly favorable results are obtained when about 60 to 75% by weight of the partially inverted cane sugar is obtained in the aqueous starting medium. In practice, a concentration of 72% by weight has been found to be very useful.
  • This solution is then made weakly alkaline by means of organic or inorganic bases, such as sodium hydroxide solution, potassium hydroxide solution, and / or calcium hydroxide, or else by protolysis of salts which have an alkaline action, in particular carboxylates and salts of weak acids with strong bases, such as sodium acetate and sodium carbonate.
  • organic or inorganic bases such as sodium hydroxide solution, potassium hydroxide solution, and / or calcium hydroxide
  • salts which have an alkaline action in particular carboxylates and salts of weak acids with strong bases, such as sodium acetate and sodium carbonate.
  • aqueous solution of the partially inverted cane sugar preferably a few parts per thousand of a hydrocarbon, in particular about 2 to 25 parts by weight
  • This hydrocarbon can be a variety of materials. In particular, it should be a liquid hydrocarbon.
  • the invention is not subject to any significant restrictions here. Different petroleum fractions of aliphatic and / or aromatic origin can be involved.
  • Examples are unleaded petrol, petroleum, light petrol, ligroin, heavy petrol, light oil, gas oil (diesel oil or Hiezöl), cyclic hydrocarbons (naphthenes) and their fractions in the form of cyclopentane and cyclohexane as well as petroleum fractions, which have an intermediate position between “paraffinic” and take the “naphthenic” petroleum.
  • a compound is added to the aqueous solution of the partially inverted sugar cane, which shows alcoholic character, in particular a lower primary, secondary or tertiary mono- or polyhydric alcohol.
  • the focus here is on methanol, ethanol, propanol, butanol, glycol and glycerin.
  • These compounds are advantageously used in an amount such that about 5 to 100 parts by weight per 1000 parts by weight of the solution of the partially inverted cane sugar. Parts of it are omitted. The range from about 10 to 60 parts by weight is considered to be particularly preferred. Very particularly favorable results are regularly obtained when about 50 parts by weight of the alcohol, aldehyde and / or ketone account for 1000 parts by weight of the liquid sugar.
  • the function of these connections has not yet been clearly clarified. They may have the function of a dispersion mediator. For this it is necessary that they are readily soluble in the aqueous solution of the partially inverted cane sugar.
  • the compounds detailed above meet this requirement.
  • gypsum CaSO 4 .1 / 2 H 2 O
  • Traces are sufficient for this.
  • trace amounts of 10 2 to 10 4 are understood to be ppm.
  • the addition of gypsum does not improve the special suitability of the flammable aqueous mixtures described in detail below. Rather, it leads to a reduction in small amounts of toxic substances when the aqueous mixtures are burned. At these temperatures, gypsum breaks down into calcium oxide and sulfur trioxide. The decay products cause the elimination of unwanted toxins in the course of the combustion process.
  • the product obtained on the basis of the method according to the invention described above shows the interesting and, compared to the prior art, improved property of delivering together with hydrocarbons, alcohols and water in a combustible mixture which can be used as fuel in any combustion system, in particular in engines of motor vehicles. It is only added to the mixtures of water, alcohol and petrol in comparatively small amounts. The amount of water is essential for whether this mixture is used as "normal gasoline” or as "super fuel”. The knock resistance decreases with an increased water content.
  • This fuel meets the requirements specified in DIN 51 600 Regular petrol, ie its knock resistance is sufficient to be used as a petrol engine in motor vehicles which are run on normal petrol in general
  • the product described above can be converted into a "super fuel” if only about 1/4 of the Such a product is equivalent to a super fuel that meets the requirements of the aforementioned DIN regulation, depending on the operating conditions of various heating systems l, and the like can be calculated using simple experiments the optimal mix for such purposes determined.
  • lubricant is to be understood as much as possible here.
  • lubricating oils for machining such as cutting and drilling oils
  • oils for plastic non-cutting deformation such as those e.g. be used in the cold rolling process.
  • the filter effect of air filters in motor vehicles and also in combustion systems is increased significantly if the filter materials are impregnated with the additive.
  • This effect can be increased if, in addition to the above-described measures of the process according to the invention or subsequently, the process is carried out in such a way that the mixture having the red hue is added to excess water and stored for several days with the exclusion of air at room temperature, the product obtained in this way having a low Amount of egg yolk, especially chicken egg yolk (as a protein-containing nutrient base or nutrient for microorganisms), and stored again for several days at room temperature.
  • about 30 g of the additive were mixed with 4 water. The entire mass was then kept airtight at room temperature for 16 days.
  • microorganisms had arisen.
  • phosphorus proteids could be detected in the mass obtained.
  • the mass obtained in this way can be used particularly well as an impregnating agent for air filters in motor vehicles and incineration plants.
  • the effect is increased in that a lower alcohol, such as methanol, ethanol, propanol and / or butanol or also glycol or glycerin, is incorporated into this additive, it being possible for two parts of the additive to account for about 1 part of alcohol.
  • the CO value is therefore reduced by approximately 95% for the MTS fuel. Another advantage is that it does not require any special means to increase knock resistance, especially no lead compounds. If the filters of motor vehicles are now treated with the additive 7, in particular in accordance with the above-described further procedure (additional treatment with special proteins), then the reduction in the CO value by about 1/3 can be determined in conventional super fuels.
  • the impregnation mentioned can significantly reduce the CO value.
  • the test drives with the individual vehicles showed that the MTS fuel and the normal super fuel used for comparison were absolutely comparable in terms of performance.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Liquid Carbonaceous Fuels (AREA)
  • Lubricants (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Beans For Foods Or Fodder (AREA)
  • Detergent Compositions (AREA)
  • Pyridine Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

PCT No. PCT/EP87/00044 Sec. 371 Date Sep. 15, 1987 Sec. 102(e) Date Sep. 15, 1987 PCT Filed Jan. 30, 1987 PCT Pub. No. WO87/04717 PCT Pub. Date Aug. 13, 1987.A process for producing an additive for lubricants and for aqueous fuel mixtures and heating media is described, in which an alkaline aqueous solution of an inverted cane sugar as the main component and containing a hydrocarbon and an alcohol is heated and then cooled. Use is made of inverted cane sugar with a degree of inversion of approximately 50 to 80% and is heated to approximately 75 DEG to 100 DEG C. until a red shade forms. The additive obtained in this way, mixed with alcohol, water and gasoline, can be used as an excellent fuel and as a substitute for normal gasoline and even superfuel. A corresponding mixture can also be used as a heating medium. The characteristics of lubricants can be improved by incorporating this additive. In addition, the effectiveness of air filters of motor vehicles and internal combustion systems can be improved by impregnating the filter material with the described additive.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung eines Zusatzstoffes für Schmiermittel sowie für wässrige Kraftstoffsysteme und Heizmittel, bei dem eine alkalische wässrige Lösung eines invertierten Rohrzuckers als Hauptbestandteil mit einem Gehalt an einem Kohlenwasserstoff und einem Alkohol erwärmt und darauf abgekühlt wird sowie die oben angesprochenen Verwendungsmöglichkeiten.The invention relates to a process for the preparation of an additive for lubricants and for aqueous fuel systems and heating agents, in which an alkaline aqueous solution of an inverted cane sugar as the main component with a content of a hydrocarbon and an alcohol is heated and cooled thereon, and the uses mentioned above.

Das Verfahren der eingangs beschriebenen Art ist aus der DE-A-32 05 594 bekannt. Nach den konkreten Angaben dieser Druckschrift wird eine Mischung aus 50%iger Natronlauge, Petroleum, Essigsäure, Glyzerin, einem Ethanol/Propanol-Gemisch sowie als Hauptmasse aus einem vollständig invertierten Flüssigzucker, insbesondere einem auf Rohrzucker zurückgehenden Flüssigzucker, 10 Minuten lang auf einer Temperatur von etwa 60 bis 65°C gehalten. Nach dem Abkühlen bildet sich ein Mittel, das, Gemischen aus Wasser, Alkohol und Benzin (z.B. im Volumenverhältnis 1:5:4) in einer Menge von einigen Promille zugegeben, eine Flüssigkeit liefert, die in beliebigen Verbrennungsanlagen aber auch in Verbrennungsmotoren von Kraftfahrzeugen eingesetzt werden kann. Dieses Verfahren führt zwar zu vorteilhaften Ergebnissen, erfordert jedoch eine sorgfältige Abstimmung der genannten Einzelbestandteile. So sollen besonders günstige Ergebnisse mit einem Zusatzstoff erhalten werden, der wie folgt hergstellt wird: zunächst wird ein Gemisch aus 20 bis 45 Gew.-% 50%iger Natronlauge, 3 bis 15 Gew.-% Petroleum, 3 bis 15 Gew.-% 5%iger Essigsäure, 25 bis 80 Gew.-% Glyzerin und 20 bis 45 Gew.-% eines Gemisches aus Ethanol und Propanol hergestellt. Anschließend wird dieses Gemisch mit der 10- fachen Menge eines 75%igen invertierten, wässrigen Flüssigzuckers (Rohrzucker) gemischt. Dieses wird zu dem wirksamen Zusatzstoff wässriger Kraftstoffe etc. in der beschreibenen Weise erhitzt. Die Wirksamkeit eines derartigen Zusatzstoffes soll durch Zugabe von Spuren von Calciumsulfathalbhydrat (CaS04' 1/2 H20) gesteigert werden können.The method of the type described above is known from DE-A-32 05 594. According to the specific information in this publication, a mixture of 50% sodium hydroxide solution, petroleum, acetic acid, glycerin, an ethanol / propanol mixture and, as the main mass, a completely inverted liquid sugar, in particular a liquid sugar derived from cane sugar, is kept at a temperature of 10 minutes for 10 minutes kept at about 60 to 65 ° C. After cooling, an agent is formed which, when added to mixtures of water, alcohol and petrol (for example in a volume ratio of 1: 5: 4) in an amount of a few parts per thousand, provides a liquid which can be used in any combustion system but also in internal combustion engines of motor vehicles can be. Although this method leads to advantageous results, it requires careful coordination of the individual components mentioned. Particularly favorable results are to be obtained with an additive which is prepared as follows: first, a mixture of 20 to 45% by weight 50% sodium hydroxide solution, 3 to 15% by weight petroleum, 3 to 15% by weight 5% acetic acid, 25 to 80 wt .-% glycerol and 20 to 45 wt .-% of a mixture of ethanol and propanol. This mixture is then mixed with 10 times the amount of a 75% inverted, aqueous liquid sugar (cane sugar). This is heated to the active additive of aqueous fuels etc. in the manner described. The effectiveness of such an additive should be increased by adding traces of calcium sulfate hemihydrate (CaS04 '1/2 H 2 0).

Der Erfindung lag die Aufgabe zugrunde, das eingangs genannte Verfahren so zu verbessern, daß es eine einfache und flexiblere Herstellung des angestrebten Verfahrenserzeugnisses ermöglicht.The invention was based on the object of improving the method mentioned at the outset in such a way that it enables simple and flexible production of the desired process product.

Erfindungsgemäß wird diese Aufgabe dadurch gelöst, daß Rohrzucker eines Inversionszuckers von etwa 55 bis 75% verwendet und bis zur Ausbildung eines roton Farbtons auf etwa 75 bis 100°C erhitzt wird.According to the invention, this object is achieved in that cane sugar of an inversion sugar of about 55 to 75% is used and heated to about 75 to 100 ° C. until a roton color tone is formed.

Das Wesen der Erfindung besteht demzufolge darin, daß kein vollständig invertierter Rohrzucker eingesetzt wird, sondern ein solcher eines Inversionsgrades von etwa 55 bis 75%, besonders bevorzugt von etwa 60 bis 70% und besonders bevorzugt ein solcher von etwa 66% zu den gewünschten Ergebnissen führt. Es zeigt sich im Zusammenhang mit der Wahl eines solchen partiell invertierten Rohrzuckers als zwingend erforderlich, das Erhitzen der Ausgangsmischung so lange fortzusetzen, bis sich ein roter Farbton eingestellt hat. Auch diese bedeutsame Angabe läßt sich aus dem Stand der Technik nicht herleiten. Dabei ist es von Vorteil, daß sich dieser rote Farbton möglichst schnell einstellt, was durch Erhitzen des Ausgangsgemisches auf eine Temperatur von mehr als etwa 75°C oder vorzugsweise mehr als etwa 80°C, insbesondere mehr als 90°C erreicht werden kann. Besonders günstige Eigenschaften werden bei dem Verfahrenserzeugnis erhalten, wenn es auf etwa Siedetemperatur, insbesondere etwa 100°C einige Zeit gehalten wird, um den erwähnten roten Farbton einzustellen. Die Temperatur von 100°C sollte möglichst nicht überschritten werden. Nach dem Erhitzen wird auf Raumtemperatur abgekühlt.The essence of the invention is therefore that no fully inverted cane sugar is used, but that a degree of inversion of approximately 55 to 75%, particularly preferably approximately 60 to 70% and particularly preferably approximately 66% leads to the desired results . In connection with the choice of such a partially inverted cane sugar, it is imperative to continue heating the starting mixture until a red color has appeared. This important statement cannot be derived from the prior art either. It is advantageous that this red color is established as quickly as possible, which can be achieved by heating the starting mixture to a temperature of more than about 75 ° C. or preferably more than about 80 ° C., in particular more than 90 ° C. Particularly favorable properties are obtained in the process product if it is kept at about boiling temperature, in particular about 100 ° C., for some time in order to adjust the red color mentioned. The temperature of 100 ° C should not be exceeded if possible. After heating, it is cooled to room temperature.

Ausgangsmaterial für das erfindungsgemäß erzeugte Erzeugnis ist stets eine konzentrierte wässrige Lösung des Rohrzuckers des genannten Inversionsgrades. Hierbei sollte die Konzentration dieses Rohrzuckers vorteilhafterweise mindestens 50 Gew.-% betragen, insbesondere nahe an den Sättigungsgrad gehen. Besonders günstige Egebnisse werden erhalten, wenn in dem wässrigen Ausgangsmedium etwa 60 bis 75 Gew.-% des partiell invertierten Rohrzuckers erhalten sind. In der Praxis hat sich eine Konzentration von 72 Gew.-% als sehr nützlich gezeigt. Diese Lösung wird nun mittels organischer oder anorganischer Basen, wie Natronlauge, Kalilauge, und/oder Calciumhydroxid, oder auch durch Protolyse alkalische wirkende Salze, insbesondere Carboxylate sowie Salze schwacher Säeren mit starken Basen, wie Natriumacetat und Natriumcarbonat, schwach alkalisch eingestellt. Dabei hat es sich gezeigt, daß der erstrebenswerte schwach alkalische Bereich, insbesondere eines pH-Wertes von etwa 8 bis 10, mit besonderem Vorteil durch Zugabe von alkalische puffenden Carboxylaten, insbesondere von Natriumacetat, durch deren Pufferwirkung konstant gehalten wird.The starting material for the product produced according to the invention is always a concentrated aqueous solution of the sugar cane of the degree of inversion mentioned. The concentration of this cane sugar should advantageously be at least 50% by weight, in particular close to the degree of saturation. Particularly favorable results are obtained when about 60 to 75% by weight of the partially inverted cane sugar is obtained in the aqueous starting medium. In practice, a concentration of 72% by weight has been found to be very useful. This solution is then made weakly alkaline by means of organic or inorganic bases, such as sodium hydroxide solution, potassium hydroxide solution, and / or calcium hydroxide, or else by protolysis of salts which have an alkaline action, in particular carboxylates and salts of weak acids with strong bases, such as sodium acetate and sodium carbonate. It has been shown that the desirable, weakly alkaline range, in particular a pH of about 8 to 10, is kept particularly constant by the addition of alkaline puffing carboxylates, in particular sodium acetate, through their buffering action.

Des weiteren werden etwa 1000 Gew.-Teile der wässrigen Lösung des partiell invertierten Rohrzuckers vorzugsweise einige Promille eines Kohlenwasserstoffs, insbesondere etwa 2 bis 25 Gew.-Teile, zugesetzt. Bei diesem Kohlenwasserstoff kann es sich um verschiedene Materialien handeln. Es sollte insbesondere ein flüssiger Kohlenwasserstoff sein. Hier unterliegt die Erfindung keinen wesentlichen Beschränkungen. Es kann sich dabei um verschiedene Erdölfraktionen aliphatischer und/oder aromatischer Herkunft handeln. Beispiele sind Rohbenzin, Petroleum, Leichtbenzin, Ligroin, Schwerbenzin, Leuchtöl, Gasöl (Dieselöl bzw. Hiezöl), cyclische Kohlenwasserstoffe (Naphthene) und deren Fraktionen in Form von Cyclopentan und Cyclohexan sowie Erdölfraktionen, die bezüglich ihrer Zusammensetzung eine Mittelstellung zwischen "paraffinischen" und den "naphthenischen" Erdölen einnehmen.Furthermore, about 1000 parts by weight of the aqueous solution of the partially inverted cane sugar, preferably a few parts per thousand of a hydrocarbon, in particular about 2 to 25 parts by weight, are added. This hydrocarbon can be a variety of materials. In particular, it should be a liquid hydrocarbon. The invention is not subject to any significant restrictions here. Different petroleum fractions of aliphatic and / or aromatic origin can be involved. Examples are unleaded petrol, petroleum, light petrol, ligroin, heavy petrol, light oil, gas oil (diesel oil or Hiezöl), cyclic hydrocarbons (naphthenes) and their fractions in the form of cyclopentane and cyclohexane as well as petroleum fractions, which have an intermediate position between "paraffinic" and take the "naphthenic" petroleum.

Schließlich wird der wässrigen Lösung des partiell invertierten Rohrzuckers eine Verbindung beigegeben, die alkoholischen Charakter zeigt, insbesondere ein niederer primärer, sekundärer oder tertiärer ein- oder mehrwertiger Alkohol. Hier stehen Methanol, Ethanol, Propanol, Butanol, Glykol und Glyzerin im Vordergrund. Diese Verbindungen werden vorteilhafterweise in einer solchen Menge eingesetzt, daß auf 1000 Gew.-Teile der Lösung des partiell invertierten Rohrzuckers etwa 5 bis 100 Gew.-Teile hiervon entfallen. Der Bereich von etwa 10 bis 60 Gew.- Teilen gilt als besonders bevorzugt. Ganz besonders günstige Ergebnisse werden regelmäßig dann erhalten, wenn etwa 50 Gew.-Teile des Alkohols, Aldehyds und/oder Ketons auf 1000 Gew.-Teile des Flüssigzuckers entfallen. Die Funktion dieser Verbindungen ist noch nicht eindeutig geklärt. Möglicherweise haben sie die Funktion eines Dispersionsvermittlers. Hierzu ist es erforderlich, daß sie in der wässrigen Lösung des partiell invertieren Rohrzuckers gut löslich sind. Die oben im einzelnen genannten Verbindungen erfüllen dieses Erfordernis.Finally, a compound is added to the aqueous solution of the partially inverted sugar cane, which shows alcoholic character, in particular a lower primary, secondary or tertiary mono- or polyhydric alcohol. The focus here is on methanol, ethanol, propanol, butanol, glycol and glycerin. These compounds are advantageously used in an amount such that about 5 to 100 parts by weight per 1000 parts by weight of the solution of the partially inverted cane sugar. Parts of it are omitted. The range from about 10 to 60 parts by weight is considered to be particularly preferred. Very particularly favorable results are regularly obtained when about 50 parts by weight of the alcohol, aldehyde and / or ketone account for 1000 parts by weight of the liquid sugar. The function of these connections has not yet been clearly clarified. They may have the function of a dispersion mediator. For this it is necessary that they are readily soluble in the aqueous solution of the partially inverted cane sugar. The compounds detailed above meet this requirement.

Auch im Rahmen des vorstehend beschriebenen bekanntenen Verfahrens soll es sich als vorteilhaft erwiesen haben, zusätzlich geringe Menge Gips (CaS04 . 1/2 H20) beizumengen. Hierzu reichen Spuren aus. Unter "Spuren" sollen Mengen von 102 bis 10-4 ppm verstanden werden. Der Zusatz von Gips verbessert allerdings nicht die spezielle Eignung der nachfolgend noch detailliert beschreibenen brennbaren wässrigen Gemische. Vielmehr führt er zur Reduzierung geringer Anteile toxischer Stoffe, wenn die wässrigen Gemische verbrannt werden. Bei diesen Temperaturen zerfällt Gips in Calciumoxid und Schwefeltrioxid. Die Zerfallprodukte bedingen die Ausschaltung unerwünschter Toxine im Verlaufe des Verbrennungsvorganges.Also in the context of the known method described above, it should have proven to be advantageous to additionally add a small amount of gypsum (CaSO 4 .1 / 2 H 2 O). Traces are sufficient for this. By "trace" amounts of 10 2 to 10 4 are understood to be ppm. However, the addition of gypsum does not improve the special suitability of the flammable aqueous mixtures described in detail below. Rather, it leads to a reduction in small amounts of toxic substances when the aqueous mixtures are burned. At these temperatures, gypsum breaks down into calcium oxide and sulfur trioxide. The decay products cause the elimination of unwanted toxins in the course of the combustion process.

Das anhand des vorstehend beschriebenen erfindungsegmäßen Verfahrens erhaltene Erzeugnis zeigt die interessante und gegenüber dem Stand der Technik verbesserte Eigenschaft, zusammen mit Kohlenwasserstoffen, Alkoholen und Wasser in brennbares Gemisch zu liefern, das als Kraftstoff in beliebigen Verbrennungsanlagen, insbesondere in Motoren von Kraftfahrzeugen eingesetzt werden kann. Dabei wird es den Gemischen aus Wasser, Alkohol und Benzin nur in vergleichsweise geringen Mengen beigefügt. Die Menge des Wasseranteils ist wesentlich dafür, ob dieses Gemisch als "Normalbenzin" oder als "Super-Kraftstoff" eingesetzt wird. Bei erhöhtem Wasseranteil sinkt der Klopffestigkeit. So has es sich gezeigt, daß ein Gemisch aus etwa 1 Gew.-Teil Wasser, 5 Gew.-Teilen Ethanol und 4 Gew.-Teilen Benzin, versetzt mit etwa 0,1 Gew.-Teil Zusatzstoff (z.B. aus 5 g Natriumhydroxid, 5 g Petroleum, 0,001 g Natriumacetat, 38 g Glyzerin, 27 g Ethanol und 1000 g 75%igen invertierten Rohrzuckers (Inversionsgrad 66%) 10 1 Normalkraftstoff bzw. "Normalbenzin" liefern. Dieser Kraftstoff erfüllt die Anforderungen, die gemäß DIN 51 600 an Normalbenzin gestellt werden, d.h. seine Klopffestigkeit reicht aus, um als Ottokraftstbff in Kraftfahrzeugen eingesetzt zu werden, die an sich mit Normalbenzin, betrieben werden. Das oben beschriebene Erzeugnis läßt sich in einem "Super-Kraftstoff" überführen, wenn lediglich etwa 1/ 4 des genannten Wasseranteils eingesetzt wird. Dabei kommt ein solches Erzeugnis einem Super-Kraftstoff gleich, der den Anforderungen nach der genannten DIN-Vorschrift genügt. In Abhängigkeit von den Betriebsbedingungen verschiedener Verbennungsanlagen von Heizöl und dergleichen läßt sich anhand einfacher Versuche die optimale Mischung für derartige Zwecke ermitteln.The product obtained on the basis of the method according to the invention described above shows the interesting and, compared to the prior art, improved property of delivering together with hydrocarbons, alcohols and water in a combustible mixture which can be used as fuel in any combustion system, in particular in engines of motor vehicles. It is only added to the mixtures of water, alcohol and petrol in comparatively small amounts. The amount of water is essential for whether this mixture is used as "normal gasoline" or as "super fuel". The knock resistance decreases with an increased water content. It has been shown that a mixture of about 1 part by weight of water, 5 parts by weight of ethanol and 4 parts by weight of gasoline, mixed with about 0.1 part by weight of additive (for example from 5 g of sodium hydroxide, Deliver 5 g of petroleum, 0.001 g of sodium acetate, 38 g of glycerin, 27 g of ethanol and 1000 g of 75% inverted cane sugar (degree of inversion 66%) 10 1 normal fuel or "normal gasoline". This fuel meets the requirements specified in DIN 51 600 Regular petrol, ie its knock resistance is sufficient to be used as a petrol engine in motor vehicles which are run on normal petrol in general The product described above can be converted into a "super fuel" if only about 1/4 of the Such a product is equivalent to a super fuel that meets the requirements of the aforementioned DIN regulation, depending on the operating conditions of various heating systems l, and the like can be calculated using simple experiments the optimal mix for such purposes determined.

Darüberhinaus hat es sich gezeigt, daß das Additiv auch zu einer vorteilhaften Verbesserung der Schmiereigenschaft von Schmiermitteln führt. Der Begriff "Schmiermittel" soll hier weitestgehend verstanden werden. Als Schmiermittel kommen insbesondere in Frage: Schmieröle für die spanabhebende Verarbeitung, wie Schneid- und Bohröle, und Öle für die plastische spanlose Verformung, wie sie z.B. beim Kaltwalzprozeß eingesetzt werden.In addition, it has been shown that the additive also leads to an advantageous improvement in the lubricating properties of lubricants. The term "lubricant" is to be understood as much as possible here. The following are particularly suitable as lubricants: lubricating oils for machining, such as cutting and drilling oils, and oils for plastic non-cutting deformation, such as those e.g. be used in the cold rolling process.

Besonders überraschen muß es, daß die Filterwirkung von Luftfiltern von Kraftfahrzeugen sowie auch von Verbrennungsanlagen ganz deutlich gesteigert wird, wenn die Filtermassen mit dem Zusatzstoff imprägniert werden. Diese Wirkung läßt sich steigern, wenn über die vorstehend beschreibenen Maßnahmen des erfindungsgemäßen Verfahrens hinaus bzw. nachfolgend so verfahren wird, daß das den roten Farbton aufweisende Gemisch in überschüssiges Wasser gegeben und mehrere Tage unter Luftabschluß bei Raumtemperatur aufbewahrt, das hierbei erhaltene Produkt mit einer geringen Menge Eidotter, insbesondere Hühnereidotter (als eiweißhaltige Nährbodengrundlage bzw. Nährmittel für Mikroorganismen), versehen und erneut mehrere Tage bei Raumtemperatur aufbewahrt wird. So wurden in einem Einzelfall etwa 30 g des Zusatzstoffes mit 4 Wasser gemischt. Die gesamte Masse wurde dann 16 Tage lang luftdicht verschlossen bei Raumtemperatur aufbewahrt. Anhand mikrobiologischer Untersuchungen konnte festgestellt werden, daß Mikroorganismen entstanden waren. Es kann also von einer Art Nährlösung gesprochen werden. Gab man zu dieser Nährlösung Hühnereidotter, dann schien das Mikrobenwachstum weiter begünstigt zu werden. Dabei stellt es sich heraus, daß der biologische Prozeß nach etwa 23 Tagen abgeschlossen war. In der erhaltenen Masse ließen sich unter anderem Phosphorproteide nachweisen. Die derartig erhaltene Masse läßt sich besonders gut als Imprägniermittel von Luftfiltern von Kraftfahrzeugen und Verbrennungsanlagen einsetzen. Der Effekt wird dadurch gesteigert, daß diesem Zusatzstoff ein niederer Alkohol, wie Methanol, Ethanol, Propanol und/oder Butanol oder auch Glykol oder Glyzerin, einverleibt wird, wobei zwei Teile Zusatzstoff auf etwa 1 Teil Alkohol entfallen können.It must be particularly surprising that the filter effect of air filters in motor vehicles and also in combustion systems is increased significantly if the filter materials are impregnated with the additive. This effect can be increased if, in addition to the above-described measures of the process according to the invention or subsequently, the process is carried out in such a way that the mixture having the red hue is added to excess water and stored for several days with the exclusion of air at room temperature, the product obtained in this way having a low Amount of egg yolk, especially chicken egg yolk (as a protein-containing nutrient base or nutrient for microorganisms), and stored again for several days at room temperature. In an individual case, about 30 g of the additive were mixed with 4 water. The entire mass was then kept airtight at room temperature for 16 days. On the basis of microbiological tests, it was found that microorganisms had arisen. One can speak of a kind of nutrient solution. If egg yolk was added to this nutrient solution, microbial growth appeared to be further promoted. It turns out that the biological process was complete after about 23 days. Among other things, phosphorus proteids could be detected in the mass obtained. The mass obtained in this way can be used particularly well as an impregnating agent for air filters in motor vehicles and incineration plants. The effect is increased in that a lower alcohol, such as methanol, ethanol, propanol and / or butanol or also glycol or glycerin, is incorporated into this additive, it being possible for two parts of the additive to account for about 1 part of alcohol.

Worauf die mit der Erfindung erzielbaren Erfolge tatsächlich zurückgehen, laßt sich im einzelnen noch nicht sagen. Es ist zu vermuten, daß der eingesetzte Rohrzucker des genannten Inversionsgrades unter den geschilderten Verfahrensbedingungen gewißen mikrobiologischen Abläufen unterliegt, die zur Bildung spezieller Mikroorganismen führen. Für die Ausführbarkeit der Erfindung sind diese technologischen Gesichtspunkte jedoch nicht bedeutsam.It is not yet possible to say in detail what the successes that can be achieved with the invention actually go back. It can be assumed that the cane sugar of the degree of inversion mentioned is subject to certain microbiological processes under the described process conditions, which lead to the formation of special microorganisms. However, these technological aspects are not important for the feasibility of the invention.

Wird anhand des Zusatzstoffes ein Kraftstoff hergestellt, dann zeigt sich dieser gegenüber den Super-Kraftstoffen nach DIN 51 600 unter veilfältigen Gesichtspunkten überlegen. Dies gilt insbesondere für den Anteil von umweltbelastenden Schadstoffen. Dies zeigt sich durch die Gegenüberstellung des Mehrkomponententreibstoffes aus 200 ml Wasser, 0,4 g Zusatzstoff, 3000 ml Isopropylalkohol und 700 ml Superbenzin (MTS-Treibstoff) und normalen Superbenzin einer Oktanzahl von mehr als 98.

  • Superkraftstoff bei 480 U/min/CO-Wert 3,5 Vol.-%;
  • MTS-Kraftstoff "CO-Wert 0,2 Vol.-%.
  • (MTS=Mehrkomponententreibstoff).
If a fuel is produced using the additive, then this is superior to the super fuels according to DIN 51 600 in a variety of ways. This applies in particular to the proportion of polluting pollutants. This is shown by the comparison of the multi-component fuel from 200 ml water, 0.4 g additive, 3000 ml isopropyl alcohol and 700 ml Super gasoline (MTS fuel) and normal super gasoline with an octane number of more than 98.
  • Super fuel at 480 rpm / CO value 3.5% by volume;
  • MTS fuel "CO value 0.2 vol .-%.
  • (MTS = multi-component fuel).

Der CO-Wert wird demzufolge bei dem MTS-Kraftstoff um etwa 95% herabgesetzt. Sein weiterer Vorteil liegt darin, daß er keine besonderen Mittel zur Steigerung der Klopffestigkeit, insbesondere auch keine Bleiverbindungen benötigt. Werden nun die Filter von Kraftfahrzeugen mit dem Zusatzstoff, 7 insbesondere gemäß der vorstehend geschilderten weriteren Verfahrensweise behandelt (zusätzliche Behandlung mit speziellen Eiweißen), dann läßt sich bei üblichen Super-Kraftstoffen die Herabsetzung des CO-Wertes um etwa 1/3 feststellen.The CO value is therefore reduced by approximately 95% for the MTS fuel. Another advantage is that it does not require any special means to increase knock resistance, especially no lead compounds. If the filters of motor vehicles are now treated with the additive 7, in particular in accordance with the above-described further procedure (additional treatment with special proteins), then the reduction in the CO value by about 1/3 can be determined in conventional super fuels.

Die Erfindung soll nachfolgend anhand verschiedener Beispiele noch näher erläutert werden.The invention will be explained in more detail below with the aid of various examples.

Beispiel 1example 1

Zunächst wurde ein Zusatzstoff wie folgt hergestellt: Mischen und Erhitzen von

  • 25 g 50 proz. Natronlauge
  • 5 g Leuchtpetroleum (Siedebereich 150-250°C)
  • 5 g 25 proz. Essigsäure
  • 30 g Glycerin (DAB VII)
  • 25 g Ethanol (96 %ig)
  • 1 g Calciumsulfathalbhydrat
  • 1000 g 75 proz. Saccharoselösung (Inversionsgrad 66%)
First, an additive was made as follows: mixing and heating
  • 25 g 50 percent Caustic soda
  • 5 g of light petroleum (boiling range 150-250 ° C)
  • 5 g 25 percent acetic acid
  • 30 g glycerin (DAB VII)
  • 25 g ethanol (96%)
  • 1 g calcium sulfate hemihydrate
  • 1000 g 75 percent Sucrose solution (degree of inversion 66%)

(etwa 10 min. bis zur Einstellung eines roten Farbtons auf etwa 100°C erhitzt).(heated to about 100 ° C for about 10 minutes until a red color is reached).

2 g des.:im Beispiel beschriebenen Zusatzstoffes wurden mit 1 I Leitungswasser gemischt. 3 I Isopropanol wurden darauf mit 200 ml dieser Lösung versetzt und verrührt. Die erhaltenen 3,2 I wurden dann mit 7 I Super-Kraftstoff einer Realkauf-Tankstelle gut vermischt. Das so hergestellte Treibstoffgemisch von 10,2 I wurde darauf in einen vorher vollständig entleerten Tank eines VW-Kastenwagens (Typ 21, 50 PS sowie 1570 ccm Hubraum) als Testfahrzeug gefüllt. Das Testfahrzeug wurde dann 50 km lang gefahren. Das Farverhalten konnte als auszeichnet beziechnet werden Es zeigten sich bezüglich der Fahrleistungen keine Unterschiede gegenüber üblichem Superbenzin.2 g of the additive described in the example were mixed with 1 liter of tap water. 3 l of isopropanol were then mixed with 200 ml of this solution and stirred. The 3.2 liters obtained were then mixed well with 7 liters of super fuel from a Realkauf petrol station. The fuel mixture of 10.2 l produced in this way was then filled into a previously completely emptied tank of a VW van (type 21, 50 hp and 1570 cc capacity) as a test vehicle. The test vehicle was then driven for 50 km. The color behavior could be referred to as excellent. There were no differences in driving performance compared to standard super gasoline.

Beispiel 2Example 2

Das unter Beispiel 1 bereits beschriebene Additiv wurde mit Superkraftstoff anhand verschiedener Autotypen im Hinblick auf den CO-Wert überprüft. Die Messungen wurden mit einem IR-Abgastester MHC 220 (hergestellt und vertrieben von der Firma Hermann Electronic) ausgeführt. An der Motoreinstellung der Testfahrzeuge wurde während der Überprüfung keine Veränderung vorgenommen. Testfahrzeug waren ein Open Ascona (Hubraum 1,6 und 75 PS) sowie ein Mercedes 200 (94 PS). Ber der Überprüfung anhand des Mercedes 200 wurde bei zwei Messungen auch die Steigerung der Wirksamkeit des Luftfilters durch Imprägnierung mit dem Mittel getestet. Im einzelnen ergaben sich folgende Ergebnisse:

  • 1) Open Ascona
    • a) normaler Superkraftstoff
      • 800 U/min. CO-Wert 2,0 Vol.-%
      • 1600 U/min. CO-Wert 2,0 Vol.-%
      • 4800 U/min. CO-Wert 3,5 Vol.-%
    • b) Messung mit erfindungsgemäßen MTS-Kraftstoff gemäß Beispiel 1
      • 800 U/min, CO-Wert 0,2 Vol.-%,
      • 1600 U/min. CO-Wert 0,5 Vol.-%,
      • 4800 U/min. CO-Wert 0,2 Vol.-%,
The additive already described in Example 1 was checked with super fuel using various types of cars with regard to the CO value. The measurements were carried out using an MHC 220 IR emission tester (manufactured and sold by Hermann Electronic). No changes were made to the engine settings of the test vehicles during the review. Test vehicles were an Open Ascona (displacement 1.6 and 75 hp) and a Mercedes 200 (94 hp). After checking with the Mercedes 200, the effectiveness of the air filter was also tested in two measurements by impregnation with the agent. The individual results were as follows:
  • 1) Open Ascona
    • a) normal super fuel
      • 800 rpm. CO value 2.0% by volume
      • 1600 rpm. CO value 2.0% by volume
      • 4800 rpm. CO value 3.5% by volume
    • b) Measurement with MTS fuel according to the invention according to Example 1
      • 800 rpm, CO value 0.2 vol.%,
      • 1600 rpm. CO value 0.5 vol .-%,
      • 4800 rpm. CO value 0.2 vol%,

Der MTS-Kraftstoff lieferte demzulfolge eine Reduzierung des CO-Wertes um etwa 95%.

  • 2) Versuch mit Mercedes 200
    • a) Messung mit normalen Superkraftstoff (Originalluftfilter)
      • 700 U/min. CO-Wert 2,2 Vol.-%
      • 4500 U/min. CO-Wert 1,2 Vol.-%
    • b) Messung mit normalen Superkraftstoff, bei dem die Filtermasse mit dem in Beispiel 1
      • beschriebenen
      • Zusatzstoff imprägniert wurde
      • 700 U/min. CO-Wert 1,5 Vol.-%
      • 4500 U/min. CO-Wert 0,8 Vol.-%
    • c) Messung mit MTS-Kraftstoff (Originalluftfilter)
      • 700 U/min. CO-Wert 0,25 Vol.-%
      • 4500 U/min. CO-Wert 0,20 Vol.-%
    • d) Messung mit MTS-Kraftstoff und mit einem mit dem Zusatzstoff imprägniertem Luftfilter
      • 700 U/min. CO-Wert 0,20 Vol.-%
      • 4500 U/min. CO-Wert 0,18 Vol.-%
As a result, the MTS fuel delivered a reduction in the CO value of around 95%.
  • 2) Trial with Mercedes 200
    • a) Measurement with normal super fuel (original air filter)
      • 700 rpm. CO value 2.2% by volume
      • 4500 rpm. CO value 1.2 vol%
    • b) Measurement with normal super fuel, in which the filter mass with that in Example 1
      • described
      • Additive was impregnated
      • 700 rpm. CO value 1.5% by volume
      • 4500 rpm. CO value 0.8 vol .-%
    • c) Measurement with MTS fuel (original air filter)
      • 700 rpm. CO value 0.25 vol .-%
      • 4500 rpm. CO value 0.20 vol.%
    • d) Measurement with MTS fuel and with an air filter impregnated with the additive
      • 700 rpm. CO value 0.20 vol.%
      • 4500 rpm. CO value 0.18 vol .-%

Durch die genannte Imprägnierung kann der CO-Wert noch merklich herabgesetzt werden. Die Probefahrten mit den einzelen Fahrzeugen zeigten, daß der MTS-Kraftstoff sowie der zum Vergleich herangezogen normale Superkraftstoff bezüglich der Leistung absolut vergleichbar waren.The impregnation mentioned can significantly reduce the CO value. The test drives with the individual vehicles showed that the MTS fuel and the normal super fuel used for comparison were absolutely comparable in terms of performance.

Claims (3)

1. A method of producing an additive for lubricants, as well as for aqueous fuel mixtures and heating agents, in which an alkaline aqueous solution of an invert cane sugar (the main constituent) containing a hydrocarbon and an alcohol is heated and then cooled, characterised in that invert cane sugar having a degree of inversion of about 55 to 75% is used and is heated to about 75-100° until the formation of a red coloration.
2. A method according to Claim 1, characterised in that cane sugar having a degree of inversion of about 66% is used.
3. A method according to Claim 1 or 2, characterised in that the resulting red-coloured mixture is added to an excess of water and kept for a number of days at room temperature with exclusion of air, and the resulting product is mixed with a small quantity of egg-yolk and kept for more days at room temperature.
EP87902076A 1986-02-03 1987-01-30 Process for producing an additive for lubricants and for aqueous heating agents and fuels Expired - Lifetime EP0258426B1 (en)

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DE3603207 1986-02-03

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US6843916B2 (en) 2002-07-16 2005-01-18 The Lubrizol Corporation Slow release lubricant additives gel
US7384896B2 (en) 2002-07-16 2008-06-10 The Lubrizol Corporation Controlled release of additive gel(s) for functional fluids
US7534747B2 (en) 2003-06-25 2009-05-19 The Lubrizol Corporation Gels that reduce soot and/or emissions from engines
US8022021B2 (en) 2007-02-05 2011-09-20 The Lubrizol Corporation Low ash controlled release gels
US8109287B2 (en) 2001-08-24 2012-02-07 Cummins Filtration Ip, Inc. Controlled release of additives in fluid systems
US8425772B2 (en) 2006-12-12 2013-04-23 Cummins Filtration Ip, Inc. Filtration device with releasable additive

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US8109287B2 (en) 2001-08-24 2012-02-07 Cummins Filtration Ip, Inc. Controlled release of additives in fluid systems
US6843916B2 (en) 2002-07-16 2005-01-18 The Lubrizol Corporation Slow release lubricant additives gel
US7384896B2 (en) 2002-07-16 2008-06-10 The Lubrizol Corporation Controlled release of additive gel(s) for functional fluids
US7417012B2 (en) 2002-07-16 2008-08-26 The Lubrizol Corporation Slow release lubricant additives gel
US7799745B2 (en) 2002-07-16 2010-09-21 The Lubrizol Corporation Slow release lubricant additives gel
US8076273B2 (en) 2002-07-16 2011-12-13 The Lubrizol Corportion Slow release lubricant additives gel
US8299000B2 (en) 2002-07-16 2012-10-30 The Lubrizol Corporation Slow release lubricant additives gel
US7534747B2 (en) 2003-06-25 2009-05-19 The Lubrizol Corporation Gels that reduce soot and/or emissions from engines
US8425772B2 (en) 2006-12-12 2013-04-23 Cummins Filtration Ip, Inc. Filtration device with releasable additive
US8022021B2 (en) 2007-02-05 2011-09-20 The Lubrizol Corporation Low ash controlled release gels

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EP0231906A1 (en) 1987-08-12
DE3603207A1 (en) 1987-08-06
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HU200484B (en) 1990-06-28
US4828574A (en) 1989-05-09
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BR8705768A (en) 1988-02-09
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CA1285387C (en) 1991-07-02
DK519087D0 (en) 1987-10-02
DK519087A (en) 1987-10-02
AU588097B2 (en) 1989-09-07
EP0258426A1 (en) 1988-03-09
NO874049L (en) 1987-12-02
SU1577704A3 (en) 1990-07-07
ATE54933T1 (en) 1990-08-15
NO874049D0 (en) 1987-09-28
FI874229A (en) 1987-09-25
HUT44068A (en) 1988-01-28
AU7160587A (en) 1987-08-25
FI874229A0 (en) 1987-09-25

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