Title of Invention

"A PROCESS FOR THE PREPARATION OF MICROEMULSIFIED FUEL"

Abstract

A microemulsified fuel is prepared from diesel oil and water, using a surfactant formed insitu by the reaction of an liphatic amine, an unsaturated fatty acid and a €4 to C6 saturated alcohol as consurfactant. NOx. This microemulsion has lower CO and NC^emissions and is thermodynamically stable. This microemulsion can be used in the diesel engines without any modifications needed in the engine and also fuel reduces soot content of the exhaust produced from the engine.

Full Text

FIELD OF INVENTION This invention relates to a process for the preparation of low-emission micro-emulsified diesel fuel. PRIOR ART Strategies for reducing emissions from diesel engines include engine redesign, after-treatment (various combinations of catalysts and emission control compounds); modifications of fuel production processes, and direct addition of emission control compounds to fuels. The emission control potential of engine redesign is limited by physical constraints and by combustion chemistry. Similar constraints limit emission control by catalytic converters. The dispersal of water into fuel has been explored to decrease fuel inflammability, decrease temperature of combustion, reduce particulate emissions resulting from combustion and/or to reduce levels of NOx emissions resulting from combustion. According to one of the processes known in the art as per US Patents 4,451, 265, emulsion or micro-emulsion diesel fuel is prepared by transforming the composition containing diesel fuel, lower alcohols and water with the aid of a surfactant or mixture of surfactants like N,N-dimethylethanolamine, Soyabean acids, etc. A disadvantage of the above method is that large surfactant quantities are generally needed to obtain emulsions or micro-emulsions to the disadvantage of cost. Another disadvantage of the above method is that such emulsions or micro-emulsions are stable over a limited temperature range which is too narrow for practical purposes. Still another disadvantage of the above method is that these emulsions are able to incorporate only a limited quantity of water which is generally less than the optimum quantity, which would produce the least/best smoke emission and nitrogen dioxide reduction during combustion. According to another process known in the art (US Patent 4,347,061), micro-emulsion of diesel fuel is prepared by emulsifying three components namely diesel fuel, lower alcohols and water, in a homogeniser or in an ultrasonic generator. In addition to the disadvantages mentioned earlier, the above process has the further disadvantage that it increases the production cost and complexity in commercial production. According to yet another process known in the art (US Patent 4,083,698), water-in-oil emulsion is prepared by mixing a hydrocarbon fuel, water, a lower alcohol (methanol, ethanol, etc.) and a multi-component surfactant system comprising of an ammonium or sodium long chain-fatty acid salt, or a mixture thereof; a free unsaturated long-chain fatty acid, or a mixture of free unsaturated organic acid and a free saturated long-chain fatty acid and a non-ionic surfactant typified by ethylene oxide condensation products and esterification products of a fatty acid with ethylene oxide. A disadvantage of the above method is that when ethanol or methanol are used as co-surfactant, tolerance of water gets reduced therefore phased separation occurs easily affecting the stability. Another disadvantage of the above method is that large quantity of surfactant are generally needed to obtain emulsion or micro-emulsions, to the disadvantage of cost. According to yet another process known in the art (US Patent 2,892,694), water-emulsified motor fuel is prepared by means of a detergent type emulsifier comprising the reaction product of alkyl-4-sulfophthalate and ammonia or an amine. According to still another process known in the art (Application No. 06/256,206), a diesel fuel micro-emulsion containing relatively high levels of water and alcohol is stabilised by means of a two-component surfactant system comprising of N,N-dimethyl ethanol amine and a long chain fatty acid substance. However, the disadvantage of the above two processes is that increasing the levels of surfactant which is necessitated by the higher leuels of ethanol and water,,,has the effect of- increasing the feels viscosity which will in turn affect the engine performance, OBJECTS OF PRESENT INVENTION The primary object of the present invention is to provide a micro-emulsified diesel fuel and a process for preparation thereof \vhere-in the emulsified diesel fuel obtained can be used in diesel engine without any modification in the diesel engine. Another object of the present invention is to provide a micro-emulsified diesel fuel by blending diesel fuel with water using surfactant and co-surfactant where-in the efficiency of the fuel emulsion obtained is comparable to commercial diesel. Still another object of the present invention is to provide a micro-emulsified diesel fuel and a process for preparation thereof which does not require costly and highly purified chemicals but uses easily available materials. Yet another object of the present invention is to provide a micro-emulsified diesel fuel and a process for preparation thereof where-in the formation of surfactant takes place in-situ. Further object of the present invention is to provide a micro-emulsified diesel fuel and a process for preparation thereof which requires relatively small processing time of 10 to 30 minutes. Yet further object of the present invention is to provide a micro-emulsified diesel fuel and a process for preparation thereof which is cost-effective as it does not require any expensive processing equipment. Still further object of the present invention is to provide a micro-emulsified diesel fuel composition which can reduce the soot content of the exhaust. Even further object of the present invention is to provide a micro-emulsified diesel fuel composition which keeps the level of pollutants within acceptable limits. Still further object of the present invention is to provide a micro-emulsified diesel fuel composition which has a good storage stability with good shelf life of more than one year. Yet further object of the present invention is to provide a micro-emulsified diesel fuel composition which has thermal stability over a temperature range from 14 to 65 degree Celsius. Still further object of the present invention is to provide a micro-emulsified diesel fuel composition which is thcriiiodynamically stable so that even though the temperature is raised to any temperature above 65 degree Celsius or lowered below 14 degree Celsius in a closed system, when the emulsion returns in the range of 14 to 65 degree Celsius, it regains its original property without getting destroyed. Even further object of the present invention is to provide a micro-emulsified diesel fuel composition which is non-corrosive to engine parts, as well as storage container materials. Even further object of the present invention is to provide a micro-emulsified diesel fuel composition which does not adversely affect the flash point of the fuel. STATEMENT OF INVENTION According to this invention there is provided a process for the preparation of microemulsified fuel comprising of mixing components A and B wherein: a) Component A is a mixture of a saturated 2 to 10% of aliphatic alcohol as herein described a cosurfactant, 70 to 90% diesel oil and 2 to 30% of an unsaturated long chain fatty acid as herein described as one of the constituent of the surfactant system, b) Component B being a mixture of 0.5 to 20% distilled water with 0.25 to 3% of an amine as herein described as the other constituent of the surfactant system. This invention provides a micro-emulsified diesel fuel composition and a process for preparation thereof. The process involves blending of diesel fuel with water using surfactant and co-surfactant. The process has the advantage in terms of time, energy saving and elimination of expensive processing equipment. The process comprises the preparation of the two components -Component 'A' and component 'B' and these two components are mixed together using a mechanical stirrer at ambient temperature and mixing is continued till a clear homogenous micro-emulsion is obtained. The preparation of Component VA^ involves mixing of a saturated aliphatic alcohol as a co-surfactant, commercial high speed diesel oil and an unsaturated long chain fattv_acid as one of the constituent of surfactant system. The saturated aliphatic alcohol as cosurfactant is having the general formula, CnHm+iOH, such as n-butyl alcohol, iso-butyl alcohol, cetyl alcohol, amyl alcohol, hexyl alcohol, or a mixture of C4 to C6 alcohols containing at least 2 to 3 alcohols in equimolar quantities etc., n-butyl alcohol being preferred over others. The unsaturated long chain fatty acid is having general formula CnH2n.xCOOH like oleic acid, linoleic acid, linolenic acid, recinolic acid, etc. Or a mixture of oleic acid and linoleic acid in equimolar quantities, preferably oleic acid. The preparation of Component 'B' involves mixing of distilled water with an amine as other constituent of surfactant system. The amine is like monoethanolamine, triethanolamine, ethylenediamine, diethylenetriamine, 1,1-dimethyI 2-hydroxy ethylamine, butyl amine etc. Or a mixture thereof in equimolar quantities preferably ethylene diamine. In the process of the present invention, surfactant is prepared by the reaction of aliphatic amine of Component *Byunsaturated fatty acid of Component 'A' and_saturated alcohol. This preparation of surfactant takes place insitu__and instantaneously, at room temperature, thus eliminating the need for any costly equipment other than just a mecBanical stirrer. The fuel micro-emulsion of the present invention can incorporate larger quantity of water with the use of relatively smaller amount of surfactant. The fuel composition obtained by this invention is as efficient as commercial diesel and does not require any modification in diesel engine. The micro-emulsified diesel fuel composition of the present invention is thermodynamically stable over a wide temperature range from 14 degree to 65 degree Celsius, reduces the soot content of the exhaust and also reduces the CO and NO, levels thereby keeping the level of pollutants within the acceptable limits. The microetmulsified diesel can be stored under ambient conditions in normal diesel containers. DESCRIPTION OF PROCESS The process of the present invention involves preparation of two components - Component 'A' and Component 'B' and their mixing with mechanical stirring as per steps as foliows:- (A) Preparation of the Components (i) Preparation of Component 'A* Component 'A' comprises of the following ingredients:- (a) A saturated aliphatic alcohol, having the general formula CJHbn+iOH, such as n-butyl alcohol, iso-butyl alcohol, cetyl alcohol, amyl alcohol, hexyl alcohol, etc.or a mixture of C4 to C6 alcohols containing at least two alcohols in equimolar quantities. Of these, n-butyl alcohol is the preferred one. (b) Commercially available High Speed Diesel oil. (c) Unsaturated long chain fatty acid, having general formula CnH2n-xCOOH like oleic acid, linoleic acid, linolenic acid, recinolic acid, or a mixture of oleic acid and linoleic acid in equimolar quantities in equimolar quantities. Of these, oleic acid is the preferred one. For preparation of Component 'A', 2 to 10% by t volume, preferably 2 to 3 %Jby volume of alcohol, is mixed i with 70jo_90% preferably 80Jo 85 % by volume of ^.r & 1 commercial diesel oil. To this, 2jo_30% preferably 3 to 5% by volume of long chain unsaturated fatty acid is added. These are mixed with mechanical stirrer, at 80-100 rpm, at ambient temperature, for 1-2 minutes, when clear solution is formed. (ii) Preparation of Component 'B1 The Component 'Bf comprises of the following ingredients:- (a) Amine, like monoethanolamine, triethanolamine, ethylene diamine, diethylene triamine, 1,1-dimethyl 2-hydroxy ethylamine, butyl amine, etc. Of which the preferred ones are ethylene diamine and butyl amine or a mixture thereof in equimolar quantities. (b) Water, that is, distilled water. For preparation of component 'B', 0.25 to 3% preferably OJjtoJ[y5%_,by volume of amine is mixed with JOJ?_to 20% preferably^ to 10% by volume of water. These are mixed with mechanical stirrer, at 80-100 rpm, at ambient temperature, for 1-2 minutes, when clear solution is formed. (B) Preparation of Microemulsified Fuel Composition Component A is taken in a container. To this Component-B is added slowly, with mechanical stirring, at 80-100 rpm, at ambient temperature, for 8-10 minutes, resulting in a clear and transparent microemulsion, which is slightly darker than the original diesel. After addition of component B, stirring is continued, till clear homogenous liquid is obtained. Vigorous stirring is to be avoided to keep the frothing tendency of diesel to the minimum, at the same time, ensuring homogenous mixing. Table I gives the comparative properties of commercial diesel and microemulsified fuel. Table -I Comparative Properties Of Commercial Diesel And Microemulsified Fuel Of Present Invention (Table Removed) The above table shows that the essential quality of viscosity remains in the prescribed range. The flash point of the microemulsified fuel has come down to 35 degree Celsius, which will help in the quick engine startup. The turbidity of the microemulsified fuel remains very less, below 20NTU. The appearance of the microemulsified fuel is clear and transparent. The particle size of emulsion is below 0.2 microns, thus justifying it to be a microemulsion. The smoke test reveals that the smoke content is drastically reduced as compared to diesel. The CO content, after free burning is below that of commercial diesel, while the CQa. content is more than than that of commercial fuel. The N0x content is also seen to have reduced. The invention will now be illustrated with the following working example which is intended to further illustrate the working of the invention and is not intended to imply any limitation on the scope of the present invention. WORKING EXAMPLE For preparation of 1 litre of microemulsified diesel fuel, component A was prepared by taking 30 ml of n-Butyl alcohol, (C4H9OH) and mixing with 830ml of high speed diesel oil. To this 40 ml of Oleic acid (CH3(CH2)7CHStrCH(CH2)7COOH) was added and mixed by mechanical stirring at 100 rpm at ambient temperature for 2 mins, when clear solution is formed. Component B was prepared by mixing 5 ml of Ethylene diamine with 95 ml of distilled water and mixfd by mechanical stirring at 100 rpm at ambient temperature for 2 minnvhen clear solution is formed. For preparation of micro-emulsified fuel, component A was taken in a container. To this, component B was added slowly, with mechanical stirring at 100 rpm at ambient temperature for 10 minutes, resulting in a clear and transparent microemulsion, which is slightly darker than the original diesel. After addition of component B, stirring was continued, till clear homogenous liquid was obtained. EVALUATION 1 litre of microemulsified fuel was tested using a generator of Power lite Ltd. (India). The diesel engine used is 1500 rpm, 3.5 kW/bhp. The AC generator used is 2kVA, 2kW, 50 Hz, 1500 rpm. The generator was allowed to run till the fuel was fully consumed. A sample of the exhaust gas was collected at ambient .temperature in a 10 litre Glass gas sampler and tested with for the concentration of the gases. Similar experiment was conducted with the diesel blank. The comparative results obtained are given in Table II. Table-II (Table Removed) The Table above shows that the time required to utilise both the fuels remains the same. The temperature of the exhaust gas was seen to be lower in the microemulsified fuel than in the diesel fuel. The carbon monoxide content is seen to have decreased in the microemulsified as compared to commercial diesel. Jhe carbon dioxide content has increased in the microemulsified fuel as compared to commercial diesel indicating better combustion. WE CLAIM; 1. A process for the preparation of microemulsified fuel comprising of mixing components A and B wherein: a) Component A is a mixture of a saturated 2 to 10% of aliphatic alcohol as herein described a cosurfactant, 70 to 90% diesel oil and 2 to 30% of an unsaturated long chain fatty acid as herein described as one of the constituent of the surfactant system, b) Component B being a mixture of 0.5 to 20% distilled water with 0.25 to 3% of an arnine as herein described as the other constituent of the surfactant system. 2. A process as claimed in claim 1 wherein saturated aliphatic alcohol as a cosurfactant is such as n-butyl alcohol, iso-butyl alcohol, amyl alcohol, hexyl alcohol, cetyl alcohol, or a mixture of C4 to Ce alcohols containing at least 2 or 3 alcohols in equimolar quantities, preferably n-butyl alcohol. 3. A process as claimed in claim 1 wherein diesel oil is commercial high speed diesel oil. 4. A process as claimed in claim 1 wherein unsaturated long chain fatty acid is oleic acid, linoleic acid, linolenic acid, or a mixture of oleic acid and linoleic acid in equimolar quantities. 5. A process as claimed in claim 1 wherein amine, taken is ethylene diamine, monoethanolamine, 1-1, 1-dimethyl, 2-hydroxy-ethylamine, butyl amine, diethylene triamine, triethanol amine, or a mixture of these amines in equimolar quantities preferably ethylene diamine or butylamine or a mixture thereof in equimolar quantities. 6. A process as claimed in claim 1 wherein commercial diesel is 80 to 85% by volume. 7. A process as claimed in claim 1 wherein unsaturated fatty acid is 3 to 5% by volume. 8. A process as claimed in claim 1 wherein saturated aliphatic alcohol is 2 to 3% by volume. 9. A process as claimed in claim 1 wherein amine is 0.3 to 0.5% by volume. 10. A process as claimed in claim 1 wherein distilled water content is 9 to 10% by volume. A process for preparation of microemulsifled fuel substantially as herein described and illustrated in the example.

Documents:

580-del-2000-abstract.pdf

580-del-2000-claims.pdf

580-del-2000-correspondence-others.pdf

580-del-2000-correspondence-po.pdf

580-del-2000-description (complete).pdf

580-del-2000-form-1.pdf

580-del-2000-form-19.pdf

580-del-2000-form-2.pdf

580-del-2000-gpa.pdf