KR20200122490A - The solid or gel alcohol fuels and their preparation to prevent flameout - Google Patents

Abstract

The present invention relates to a method for preparing solid and gel alcohol fuels, especially has an advantage of exhibiting excellent effects in preventing flameout by adding trioxane derivatives and triacetin to solid and gel alcohol fuels such as methanol, ethanol isopropanol, etc. A solid alcohol fuel composition or a gel alcohol fuel composition according to an aspect of the present invention has high stability during movement.

Description

The solid or gel alcohol fuels and their preparation to prevent flameout}

The present specification relates to an alcohol fuel composition in the form of a solid or a gel, and in particular, to an alcohol fuel composition in the form of a solid or a gel exhibiting an excellent effect on preventing off in cold winter.

Conventional alcohol fuels such as methanol, ethanol, and isopropanol have a gel type and a solid.

In the gel type, acidic substances such as polyacrylic acid and bases such as diisopropanolamine and triisopropanolamine are added to alcohols such as methanol, ethanol, and isopropanol by hydrogen bonding and acid/base bonding of acid and base in a small amount of water. It is a method of stabilizing alcohol by making a gel by chelation and confining a large amount of alcohol inside the chelation frame.

In addition, solid alcohol fuels are made by adding a little water to organic acids such as lauric acid, palmitic acid, stearic acid, and mixed fatty acids including soybean fatty acids derived from soybean oil, and adding a little water to form a solid solid. do. Both of these work by the same mechanism.

When moving or storing, the gel is stabilized rather than liquid alcohol, but the more stabilized alcohol fuel is a solid type. The big advantage of the solid type is that if it is spilled over accidentally while moving, the solid hardly spreads to the surroundings, and the stability of storage as well as the evaporation of alcohol is slower than that of the gel.

Alcohol Fuel Looking at the existing prior art, Korean Publication 1992-0018199 and Korean Patent 0156372 describe a method of making a gel alcohol fuel by adding alcohol having 1-6 carbon atoms, polyoxyethylene alkylamine, acrylic polymer silicate compound, and water. .

In Korean Patent 10-0738811 and Korean Patent 10-1315993, amines with more amine compounds are used in 1-6 alcohols, various acid compounds of carboxyvinyl polymer are added, and a little metal is added to improve physical properties. It describes the method.

Korean Patent No. 10-1535603, Korean Patent No. 10-1626104, and Korean Patent Laid-Open Patent No. 10-2017-0012993 describe a manufacturing method for adding and adding amines and acid compounds that chelate in a more variety.

In addition, the most recent Korean Patent No. 10-1942281 of January 2019 describes a manufacturing method that can increase the amount of calories by using vegetable glycerin ester fatty acids, dispersants and water.

On the other hand, there has not been much technology development for solid alcohol fuels that are harder than gel fuels, and solid fuels have a disadvantage in that they often turn off slightly more than gel fuels.

Therefore, in the solid and gel form, particularly in the solid form of alcohol fuel composition, the solid alcohol fuel is a new alcohol fuel composition that improves the prevention of turn-off and increases the amount of heat, and the gel alcohol fuel composition is a new alcohol fuel composition for improving the efficiency of increasing calories. There is a need for research on

Korean Patent Publication No. 10-1992-0018199 Korean Patent Registration No. 10-0156372 Korean Patent Registration No. 10-0738811 Korean Patent Registration No. 10-1315993 Korean Patent Registration No. 10-1535603 Korean Patent Registration No. 10-1626104 Korean Patent Publication No. 10-2017-0012993 Korean Patent Registration No. 10-1942281

Accordingly, the present inventors have conducted research to solve the above problems, and as a result of the solid alcohol fuel, a novel solid or gel-type alcohol fuel composition capable of improving efficiency such as prevention of turning off and increasing calories, and gel alcohol fuels It is intended to be invented and provided.

One aspect of the present invention, in the alcohol fuel composition, characterized in that it comprises a trioxane derivative and triacetin, to provide an alcohol fuel composition for preventing off.

In one aspect of the present invention, the alcohol fuel composition is to provide an alcohol fuel composition in a gel form.

In one aspect of the present invention, the alcohol fuel composition is to provide an alcohol fuel composition in a solid form.

The object of the present invention is not limited to the object mentioned above. The object of the present invention will become more apparent from the following description, and will be realized by the means described in the claims and combinations thereof.

In order to achieve the above object, the present invention provides a means of solving the following problems.

The present invention comprises a fatty acid having 10 to 20 carbon atoms, soybean fatty acid derived from soybean oil, based on 100 parts by weight of a lower alcohol having 1 to 5 carbon atoms such as methanol, ethanol, isopropanol, and n-propanol in order to achieve the above object. 0.1 to 5 parts by weight of organic or inorganic acids of mixed fatty acids or polyacrylic acid, inorganic bases such as potassium hydroxide, calcium hydroxide, sodium hydroxide, or organic or inorganic bases of organic amines such as diisopropanolamine and triisopropanolamine Parts, and 0.1 to 5 parts by weight of water, and trioxane, trimethyltrioxane, triethyltrioxane, tripropyltrioxane, 1,3,5-triisopropyltrioxane, etc. It provides a solid alcohol or gel alcohol fuel production method comprising 0.1 to 5 parts by weight of an oxane derivative and 0.1 to 5 parts by weight of triacetin.

One aspect of the present invention provides an alcohol fuel composition for preventing off, comprising a trioxane derivative and triacetin in the alcohol fuel composition.

In one aspect of the present invention, the trioxane derivative is contained in an amount of 0.1% to 10% by weight based on the total weight of the composition, and the triacetin is contained in an amount of 0.1% to 10% by weight based on the total weight of the composition. It provides an alcohol fuel composition for preventing.

In one aspect of the present invention, the trioxane derivative and the triacetin are included in a weight ratio of 1:0.5 to 2, providing an alcohol fuel composition for preventing off.

In one aspect of the present invention, the trioxane derivative is 1,2,3-trioxane derivative; It provides a 1,2,4-trioxane derivative and any one or more of 1,3,5-trioxane derivative, an alcohol fuel composition for preventing off.

In one aspect of the present invention, the trioxane derivative provides an alcohol fuel composition for preventing off-off, wherein an alkyl group having 1 to 6 carbon atoms is substituted with one or more of 0 to 3 carbon groups of a trioxan ring.

In one aspect of the present invention, the composition is an alcohol having 1 to 5 carbon atoms; Organic or inorganic acids selected from fatty acids having 10 to 20 carbon atoms, fatty acids derived from soybean oil, and polyacrylic acids; Organic or inorganic bases selected from potassium hydroxide, calcium hydroxide, sodium hydroxide, and amines having 1 to 8 carbon atoms; Trioxane derivatives; And triacetin; containing, it provides an alcohol fuel composition for preventing off.

In one aspect of the present invention, based on 100 parts by weight of the alcohol, the organic or inorganic acid is 0.1 to 5 parts by weight, the organic or inorganic base is 0.05 to 3 parts by weight, the trioxane derivative is 0.1 to 5 parts by weight, the Triacetin is contained in an amount of 0.1 to 5 parts by weight, providing an alcohol fuel composition for preventing off.

In one aspect of the present invention, the alcohol is 80 to 98% by weight based on the total weight of the composition; 0.1 to 2% by weight of the organic or inorganic acid; The inorganic or organic acid is 0.05 to 1% by weight; The trioxane derivative is 0.1 to 2% by weight; And the triacetin is 0.1 to 2% by weight; Provides an alcohol fuel composition for preventing the off contained.

In one aspect of the present invention, the alcohol fuel composition is an alcohol fuel composition in a solid form or an alcohol fuel composition in a gel form, providing an alcohol fuel composition for preventing off.

In another aspect of the present invention, in the method for preparing an alcohol fuel composition for preventing any one of the above, (a) adding and stirring alcohol, an organic or inorganic acid, and an organic or inorganic base; And (b) adding and heating a trioxane derivative and triacetin after the step (a) and heating it.

In another aspect of the present invention, the method provides a method for preparing an alcohol fuel composition for preventing off-off, further comprising: (c) leaving the heated mixture to room temperature after step (b).

The solid alcohol fuel composition or the gel alcohol fuel composition according to an aspect of the present invention is superior in preventing the light-off phenomenon compared to the existing alcohol fuel composition.

The solid alcohol fuel composition or gel alcohol fuel composition according to an aspect of the present invention has a higher calorific value than conventional products.

The solid alcohol fuel composition or gel alcohol fuel composition according to an aspect of the present invention has high stability during movement and almost no fire risk in case of a leakage accident.

The solid alcohol fuel composition or gel alcohol fuel composition according to an aspect of the present invention has the advantage of being able to provide thermal power for heat insulation or emergency emergency use during events or training in concrete curing, home, office, outdoor, etc.

The effects of the present invention are not limited to the effects mentioned above. It should be understood that the effects of the present invention include all effects that can be inferred from the following description.

1 is a solid alcohol fuel (A) prepared by Example 3 of the present invention and a gel alcohol fuel (B) prepared by Example 33.

Unless otherwise specified, all numbers, values, and/or expressions expressing ingredients, reaction conditions, and content of ingredients used herein are the variety of measurements that occur in obtaining such values, among other things, in which these numbers are essentially different. Since they are approximations that reflect uncertainty, they should be understood as being modified in all cases by the term "about". In addition, when numerical ranges are disclosed herein, these ranges are continuous and, unless otherwise indicated, include all values from the minimum value of this range to the maximum value including the maximum value. Furthermore, when this range refers to an integer, all integers from the minimum value to the maximum value including the maximum value are included, unless otherwise indicated.

In the present specification, when a range is described for a variable, it will be understood that the variable includes all values within the stated range, including the stated endpoints of the range. For example, a range of "5 to 10" includes values of 5, 6, 7, 8, 9, and 10, as well as any subranges such as 6 to 10, 7 to 10, 6 to 9, 7 to 9, etc. Inclusive, and it will be understood to include any values between integers that are reasonable in the scope of the stated range, such as 5.5, 6.5, 7.5, 5.5 to 8.5 and 6.5 to 9, and the like. Also, for example, the range of "10% to 30%" is 10% to 15%, 12% to 10%, 11%, 12%, 13%, etc., as well as all integers including up to 30%. It will be understood to include any subranges such as 18%, 20% to 30%, and the like, and include any values between reasonable integers within the scope of the stated range, such as 10.5%, 15.5%, 25.5%, and the like.

Hereinafter, the present invention will be described in detail.

The mechanism of immobilization of solid alcohol fuel and gel alcohol fuel can be explained by the same principle that alcohol such as methanol is inserted into the cage formed by the reaction of acid and base. In this case, the strength of the solid fuel and the viscosity of the gel are weakened or strengthened. It is an important and very difficult problem to use a calorie enhancer according to the alcohol fuel composition to enhance the caloric value of alcohol, and it can be controlled according to what kind of organic or inorganic acid is used and what kind of organic or inorganic base is used.

The biggest difference between the solid alcohol fuel or gel alcohol fuel according to the present invention and the conventional alcohol fuel having a technical advantage is trioxane, trimethyltrioxane, triethyltrioxane, tripropyltrioxane, Trioxane derivatives such as 1,3,5-triisopropyltrioxane are added, and trioxane is added to enhance caloric value at the same time.

To explain this in more detail,

Typical solid alcohol fuel manufacturing methods include 0.1-5 parts by weight of stearic acid, 0.05-5 parts by weight of sodium hydroxide, 0.1-5 parts by weight of water, and trioxane in 100 parts by weight of alcohol such as methanol, ethanol, isopropanol or n-propanol. 0.1-5 parts by weight of triacetin and 0.1-5 parts by weight of triacetin can be added to prepare solid and gel alcohol fuel, which requires 2-3 hours of reflux.

As a typical method for producing a gel alcohol fuel, 0.1-5 parts by weight of polyacrylic acid, 0.05-3 parts by weight of triisopropanolamine, 0.1-5 parts by weight of water, triisopropanolamine, 0.1-5 parts by weight of water, and 100 parts by weight of alcohol such as methanol, ethanol, isopropanol or n-propanol. 0.1-5 parts by weight of oxane and 0.1-5 parts by weight of triacetin can be added to prepare a gel alcohol fuel. In this case, strong stirring using Homervikser is required.

Or, 0.1-5 parts by weight of mixed fatty acids containing myristic acid, palmitic acid, stearic acid, soybean fatty acid derived from soybean oil, 0.05-5 parts by weight of sodium hydroxide in 100 parts by weight of alcohol such as methanol, ethanol, isopropanol or n-propanol Part, 0.1-5 parts by weight of water, 0.1-5 parts by weight of trioxane, and 0.1-5 parts by weight of triacetin can be added to prepare a solid and gel alcohol fuel.

Or 100 parts by weight of alcohol such as methanol, ethanol, isopropanol or n-propanol 0.1-5 parts by weight of stearic acid, inorganic bases such as sodium hydroxide, potassium hydroxide or calcium hydroxide, or organic bases such as triisopropanolamine and diisopropanolamine 0.05 -5 parts by weight, 0.1-5 parts by weight of water, 0.1-5 parts by weight of trioxane, 0.1-5 parts by weight of triacetin, and a solid and gel alcohol fuel can be prepared.

Or 100 parts by weight of alcohol such as methanol, ethanol, isopropanol or n-propanol 0.1-5 parts by weight of stearic acid, 0.05-5 parts by weight of sodium hydroxide, 0.1-5 parts by weight of water, trioxane, trimethyltrioxane, triethyltri 0.1-5 parts by weight of trioxane derivatives such as oxane, tripropyltrioxane, and 1,3,5-triisopropyltrioxane, and 0.1-5 parts by weight of triacetin can be added to prepare solid and gel alcohol fuel.

Totally mixed fatty acids containing myristic acid, palmitic acid, stearic acid, soybean fatty acid derived from soybean oil, or 0.1-5 parts by weight of polyacrylic acid, sodium hydroxide, in 100 parts by weight of alcohol such as methanol, ethanol, isopropanol or n-propanol, Potassium hydroxide or calcium hydroxide Diisopropanolamine or triisopropanolamine 0.05-5 parts by weight, water 0.1-5 parts by weight, trioxane, trimethyltrioxane, triethyltrioxane, tripropyltrioxane, 1,3,5-triisopropyl It is characterized in that 0.1-5 parts by weight of trioxane derivatives such as trioxane and 0.1-5 parts by weight of triacetin are added to prepare solid and gel alcohol fuel.

The gel and solid and gel alcohol fuel produced as described above can provide firepower for emergency and emergency use during events or training in concrete curing, home, office, outdoor, etc., and can be used for various purposes other than the above. Do.

Hereinafter, various aspects of the present invention will be described.

One aspect of the present invention provides an alcohol fuel composition for preventing off, comprising a trioxane derivative and triacetin in the alcohol fuel composition.

In the present invention, the trioxane derivative is 1,2,3-trioxane; 1,2,3-trioxane derivatives; 1,2,4-trioxane; 1,2,4-trioxane derivatives; 1,3,5-trioxane; And 1,3,5-trioxane derivatives. The 1,2,3-trioxane derivatives; In the 1,2,4-trioxane derivative and the 1,3,5-trioxane derivative, an alkyl group having 1 to 6 carbon atoms may be substituted with one or more of 0 to 3 carbon groups of a trioxan ring.

In one aspect of the present invention, the trioxane derivative is contained in an amount of 0.1% to 10% by weight based on the total weight of the composition, and the triacetin is contained in an amount of 0.1% to 10% by weight based on the total weight of the composition. It provides an alcohol fuel composition for preventing. When the trioxane derivative and the triacetin satisfy the above range, when the fuel is burned, the flame is constant throughout the combustion time, the non-extinguishing prevention effect is excellent, and the calorific value is excellent.

In one aspect of the present invention, the trioxane derivative and the triacetin are included in a weight ratio of 1:0.5 to 2, providing an alcohol fuel composition for preventing off. When the trioxane derivative and the triacetin satisfy the above range, when the fuel is burned, the flame is constant throughout the combustion time, the non-extinguishing prevention effect is excellent, and the calorific value is excellent.

In one aspect of the present invention, the trioxane derivative is 1,2,3-trioxane derivative; It provides a 1,2,4-trioxane derivative and any one or more of 1,3,5-trioxane derivative, an alcohol fuel composition for preventing off.

In one aspect of the present invention, the trioxane derivative provides an alcohol fuel composition for preventing off-off, wherein an alkyl group having 1 to 6 carbon atoms is substituted with one or more of 0 to 3 carbon groups of a trioxan ring.

In one embodiment, the trioxane derivative is 1,2,3-trioxane, 1,2,4-trioxane, 1,3,5-trioxane, an alkyl group having 1 to 6 carbon atoms to the carbon group of the trioxane ring 1,2,3-trioxane substituted with any one or more of 0 to 3, 1,2,4- wherein the alkyl group having 1 to 6 carbon atoms is substituted with any one or more of 0 to 3 carbon groups of the trioxan ring Trioxane and 1,3,5-trioxane in which an alkyl group having 1 to 6 carbon atoms is substituted with any one or more of 0 to 3 carbon groups of a trioxan ring.

In one aspect of the present invention, the composition is an alcohol having 1 to 5 carbon atoms; Organic or inorganic acids selected from fatty acids having 10 to 20 carbon atoms, fatty acids derived from soybean oil, and polyacrylic acids; Organic or inorganic bases selected from potassium hydroxide, calcium hydroxide, sodium hydroxide, and amines having 1 to 8 carbon atoms; Trioxane derivatives; And triacetin; containing, it provides an alcohol fuel composition for preventing off.

In one embodiment, the amine having 1 to 8 carbon atoms is monomethylamine, dimethylamine, trimethylamine, monoethylamine, diethylamine, triethylamine, monopropylamine, dipropylamine, tripropylamine, monobutylamine , Dibutylamine, tributylamine, monopentylamine (amylamine), dipentylamine, tripentylamine, monohexylamine, dihexylamine, trihexylamine, monomethanolamine, dimethanolamine, trimethanolamine, mono Ethanolamine, diethanolamine, triethanolamine, and the like can be used.

In one aspect of the present invention, based on 100 parts by weight of the alcohol, the organic or inorganic acid is 0.1 to 5 parts by weight, the organic or inorganic base is 0.05 to 3 parts by weight, the trioxane derivative is 0.1 to 5 parts by weight, the Triacetin is contained in an amount of 0.1 to 5 parts by weight, providing an alcohol fuel composition for preventing off. When the component contained in the composition satisfies the above range, when the fuel is burned, the flame is constant throughout the combustion time, the non-extinguishing prevention effect is excellent, and the calorific value is excellent.

In one aspect of the present invention, the alcohol is 80 to 98% by weight based on the total weight of the composition; 0.1 to 2% by weight of the organic or inorganic acid; The inorganic or organic acid is 0.05 to 1% by weight; The trioxane derivative is 0.1 to 2% by weight; And the triacetin is 0.1 to 2% by weight; Provides an alcohol fuel composition for preventing the off contained. When the component contained in the composition satisfies the above range, when the fuel is burned, the flame is constant throughout the combustion time, the non-extinguishing prevention effect is excellent, and the calorific value is excellent.

In one embodiment, the composition may contain 1 to 20% by weight of water based on the total weight of the composition.

In one aspect of the present invention, the alcohol fuel composition is an alcohol fuel composition in a solid form or an alcohol fuel composition in a gel form, providing an alcohol fuel composition for preventing off.

In one aspect of the present invention, the gel-type alcohol fuel may further include a scattering inhibitor. As the anti-scattering agent, a porous material having adsorption capacity for acids and alkalis is preferable. For example, inorganic porous materials such as activated carbon, silica gel, alumina, activated clay, charcoal, clay minerals, and diatomaceous earth; Natural polymers such as dextran and agarose; Synthetic polymers such as polyacrylamide, hydrophilic vinyl polymer, and polystyrene can be used. In particular, activated carbon such as granular activated carbon or crushed activated carbon, diatomaceous earth or silica gel is preferably used. The amount of the porous material used is 0.1 to 5% by weight, preferably 0.25 to 1% by weight, based on the total weight of the fuel composition. If the amount of the porous material is too small, the scattering prevention effect may decrease, and if too much, the combustion efficiency may decrease.

In addition, the gel-type alcohol fuel according to an aspect of the present invention may further include an ultraviolet absorber. As the ultraviolet absorber, benzophenones, benzoic acids, cinnamic acids, salicylic acids, and the like can be used. Benzophenones include 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid, 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid sodium, And hydroxy substituted benzophenones such as dihydroxybenzophenone, dihydroxydimethoxybenzophenone, sodium dihydroxydimethoxybenzophenone disulfonate, and tetrahydroxybenzophenone. Examples of the benzoic acids include paraaminobenzoic acid esters such as paraaminobenzoic acid and ethyl paraaminobenzoate, N-substituted paraaminobenzoic acid esters such as amyl paradimethylbenzoate and octyl paradimethylbenzoate. Examples of cinnamic acids include 4-methoxycinnamic acid-2-ethoxyethyl, diisopropyloxycycinamide methyl, paramethoxycinnamic acid-2-ethylhexyl glyceryl, paramethoxycinnamic acid isopropyl, di Alkyloxy substituted cinnamic acids, such as isopropyloxy cinnamic acid ester, etc. are mentioned. Examples of salicylic acids include salicylic acid esters such as phenyl salicylate, octyl salicylate, and dipropylene glycol salicylate. The content of the ultraviolet absorber is 1 to 1000 ppm, preferably 10 to 500 ppm, based on the total weight of the fuel composition. If the content of the ultraviolet absorber is too small, the ultraviolet absorption efficiency may decrease, and if it is too large, the combustion efficiency may decrease.

In another aspect of the present invention, in the method for preparing an alcohol fuel composition for preventing any one of the above, (a) adding and stirring alcohol, an organic or inorganic acid, and an organic or inorganic base; And (b) adding and heating a trioxane derivative and triacetin after the step (a) and heating it.

In another aspect of the present invention, the method provides a method for preparing an alcohol fuel composition for preventing off-off, further comprising: (c) leaving the heated mixture to room temperature after step (b).

Hereinafter, the present invention will be described in more detail through specific examples. The following examples are only examples to aid understanding of the present invention, and the scope of the present invention is not limited thereto.

[Examples and Comparative Examples]

Example 1

Condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of methanol, 5g of water, 3g of myristic acid, 0.52g of sodium hydroxide were added to reflux for 1 hour, and 2.5g of 1,3,5-trioxane , Add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 2

Install a condenser, mechanical stirrer, and thermometer in a 1L 3-neck round bottom flask, add 500g of methanol, 5g of water, 3.4g of palmitic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-trioxane 2.5 g, add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 3

Install a condenser, mechanical stirrer, and thermometer in a 1L 3-neck round bottom flask, add 500g of methanol, 5g of water, 3.74g of stearic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and 2.5g of 1,3,5-trioxane , Add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 4

Condenser, mechanical stirrer, and thermometer are installed in a 1L 3-necked round bottom flask, 500g of methanol, 5g of water, 3.5g of soybean fatty acid, 0.52g of sodium hydroxide are added to reflux for 1 hour, and 2.5g of 1,3,5-trioxane , Add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 5

Condenser, mechanical stirrer, and thermometer are installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3g of myristic acid, 0.52g of sodium hydroxide are added to reflux for 1 hour, and 2.5g of 1,3,5-trioxane , Add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 6

Condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.4g of palmitic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, followed by 1,3,5-trioxane 2.5 g, add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 7

Condenser, mechanical stirrer, and thermometer are installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.74g of stearic acid, 0.52g of sodium hydroxide are added to reflux for 1 hour, and 2.5g of 1,3,5-trioxane , Add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 8

Install a condenser, mechanical stirrer, and thermometer in a 1L 3-neck round bottom flask, add 500g of ethanol, 5g of water, 3.5g of soybean fatty acid, 0.52g of sodium hydroxide, reflux for 1 hour, and 2.5g of 1,3,5-trioxane , Add 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 9

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of methanol, 5g of water, 3g of myristic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-trioxane 5g, Add 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 10

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of methanol, 5g of water, 3.4g of palmitic acid, and 0.52g of sodium hydroxide were added to reflux for 1 hour, and then 1,3,5-trioxane 5g , Add 5g of triacetin and boil for another hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 11

A condenser, mechanical stirrer, and thermometer were installed in a 1L three-necked round bottom flask, and 500g of methanol, 5g of water, 3.74g of stearic acid, and 0.52g of sodium hydroxide were added to reflux for 1 hour, and then 1,3,5-trioxane 5g, Add 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 12

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of methanol, 5g of water, 3.5g of soybean fatty acid, 0.52g of sodium hydroxide were added to reflux for 1 hour, and then 1,3,5-trioxane 5g, Add 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 13

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3g of myristic acid, 0.52g of sodium hydroxide were added to reflux for 1 hour, and then 1,3,5-trioxane 5g, Add 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 14

Condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.4g of palmitic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-trioxane 5g , Add 5g of triacetin and boil for another hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 15

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.74g of stearic acid, 0.52g of sodium hydroxide were added to reflux for 1 hour, and then 1,3,5-trioxane 5g, Add 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 16

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, and 500g of ethanol, 5g of water, 3.5g of soybean fatty acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour and then 1,3,5-1,3, Add 5g of 5-triisopropyltrioxane and 5g of triacetin and boil for 1 hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 17

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of methanol, 5g of water, 3g of myristic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-1,3, Add 2.5 g of 5-triisopropyltrioxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 18

Install a condenser, mechanical stirrer, and thermometer in a 1L 3-neck round bottom flask, add 500g of methanol, 5g of water, 3.4g of palmitic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-1,3 Add 2.5 g of ,5-triisopropyltrioxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 19

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of methanol, 5g of water, 3.74g of stearic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 2.5 g of oxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 20

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of methanol, 5g of water, 3.5g of soybean fatty acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 2.5 g of oxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 21

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of ethanol, 5g of water, 3g of myristic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 2.5 g of oxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 22

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.4g of palmitic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-triisopropyl Add 2.5 g of trioxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 23

Condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.74g of stearic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-triisopropyltri Add 2.5 g of oxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 24

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of ethanol, 5g of water, 3.5g of soybean fatty acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 2.5 g of oxane and 2.5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 25

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of methanol, 5g of water, 3g of myristic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 5 g of oxane and 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 26

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of methanol, 5g of water, 3.4g of palmitic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-triisopropyl Add 5g of trioxane and 5g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 27

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of methanol, 5g of water, 3.74g of stearic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 5 g of oxane and 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 28

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of methanol, 5g of water, 3.5g of soybean fatty acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 5 g of oxane and 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 29

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of ethanol, 5g of water, 3g of myristic acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 5 g of oxane and 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 30

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.4g of palmitic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-triisopropyl Add 5g of trioxane and 5g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 31

Condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, 500g of ethanol, 5g of water, 3.74g of stearic acid, 0.52g of sodium hydroxide were added and refluxed for 1 hour, and then 1,3,5-triisopropyltri Add 5 g of oxane and 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 32

In a 1L 3-neck round bottom flask, install a condenser, mechanical stirrer, and thermometer, add 500g of ethanol, 5g of water, 3.5g of soybean fatty acid, and 0.52g of sodium hydroxide, reflux for 1 hour, and then 1,3,5-triisopropyltri Add 5 g of oxane and 5 g of triacetin and boil for an additional hour (between 65-75 ^o C). It was allowed to stand at room temperature for 1-2 hours to cure to prepare a solid alcohol fuel.

Example 33

A homer mixer was installed in a 2L beaker, and methanol 500g, water 5g, polyacrylic acid 3g, triisopropanolamine 2g, 1,3,5-trioxane 2.5g, and triacetin 2.5g were added and stirred for 2 hours. It was allowed to stand at room temperature for 1-2 hours to cure to prepare a gel alcohol fuel.

Comparative Example 1

A condenser, mechanical stirrer, and thermometer were installed in a 1L 3-necked round bottom flask, and 500g of methanol, 5g of water, 3.74g of stearic acid, and 0.52g of sodium hydroxide were added and refluxed for 2 hours. It was allowed to stand at room temperature for 1-2 hours to harden to prepare a solid alcohol fuel.

Comparative Example 2

A Homer mixer was installed in a 2L beaker, and 500g of methanol, 5g of water, 3g of polyacrylic acid, and 2g of triisopropanolamine were added and stirred for 2 hours. It was allowed to stand at room temperature for 1-2 hours to cure to prepare a gel alcohol fuel.

[Experimental Example]

Fig. 1(A) shows the shape of the solid alcohol fuel prepared according to Example 3, and Fig. 1(B) shows the gel alcohol fuel prepared according to Example 33.

In addition, the components of Example 3, Example 33, Comparative Example 1, and Comparative Example 2 are summarized as follows.

Unit(g) Example 3 Example 33 Comparative Example 1 Comparative Example 2 Methanol 500 500 500 500 water 5 5 5 5 Stearic acid 3.74 - 3.74 - Polyacrylic acid - 3 - 3 Sodium hydroxide 0.52 - 0.52 - Triisopropanolamine - 2 - 2 1,3,5-trioxane 2.5 2.5 - - Triacetin 2.5 2.5 - -

As described above, the calorie test of the alcohol fuel prepared according to Example 3, Example 33, Comparative Example 1, and Comparative Example 2 was measured using a caloriemeter and shown in Table 2, and the calorific value of pure methanol was also measured.

Example 3 Example 33 Comparative Example 1 Comparative Example 2 Pure methanol Calorific value
(cal/g) 5,600 5,500 4,870 5,010 4,850 Comparison of pure methanol heat increase rate (%) 15.5 11.8 0.4 3.2 -

Solid or gel alcohol fuels prepared by adding trioxane derivatives and triacetin have a higher burning temperature of 10-30 ^o C than solid or gel alcohol fuels prepared by conventional methods that do not use trioxane derivatives and triacetin. It does not turn off and generates up to 15.5% more calories than pure methanol for the caloric reinforcing effect of trioxane derivatives and triacetin.

In addition, 18 L of solid alcohol fuel and gel alcohol fuel were prepared according to Examples 3 and 33 and burned for 8-10 hours. As a result, solid alcohol fuel and gel alcohol fuel containing trioxane derivative and triacetin were flamed throughout the burning time. While this was constant and did not turn off, the solid alcohol fuel and gel alcohol fuel prepared by the conventional methods of Comparative Examples 1 and 2 had a result that the flame was not constant and turned off leaving a little amount. Among them, the solid alcohol fuel prepared by Comparative Example 1 was turned off leaving a greater amount than the gel alcohol fuel, and the results are shown in Table 3.

Example 3 Example 33 Comparative Example 1 Comparative Example 2 18L methanol fuel production, turning off during combustion Does not turn off in the middle Does not turn off in the middle Off in the middle Off in the middle Burning time Ride for 8 hours and 40 minutes. Only dried solid remains after burning Ride for 8 hours and 35 minutes. Only dried solid remains after burnt Turns off after 7 hours ride. About 20cm remaining Turns off after 7 hours and 30 minutes ride. About 15cm remaining

In the above, the present invention has been described with reference to the embodiments, experimental examples, and drawings of the present invention, but those of ordinary skill in the art to which the present invention pertains to the present invention in other specific forms without changing the technical spirit or essential features. It will be appreciated that it can be implemented. Therefore, it should be understood that the embodiments described above are illustrative in all respects and not limiting.

Claims (11)

In the alcohol fuel composition,
An alcohol fuel composition for preventing off, comprising a trioxane derivative and triacetin.
The method of claim 1,
The trioxane derivative is included in an amount of 0.1% to 10% by weight based on the total weight of the composition,
The triacetin is contained in an amount of 0.1% to 10% by weight based on the total weight of the composition, an alcohol fuel composition for preventing off.
The method of claim 1,
The trioxane derivative and the triacetin are contained in a weight ratio of 1:0.5 to 2, alcohol fuel composition for preventing off.
The method of claim 1,
The trioxane derivatives include 1,2,3-trioxane derivatives; Any one or more of 1,2,4-trioxane derivatives and 1,3,5-trioxane derivatives, alcohol fuel composition for preventing off.
The method of claim 1,
In the trioxane derivative, an alkyl group having 1 to 6 carbon atoms is substituted with any one or more of 0 to 3 carbon groups of a trioxan ring.
The method of claim 1,
The composition is an alcohol having 1 to 5 carbon atoms;
Organic or inorganic acids selected from fatty acids having 10 to 20 carbon atoms, fatty acids derived from soybean oil, and polyacrylic acids;
Organic or inorganic bases selected from potassium hydroxide, calcium hydroxide, sodium hydroxide, and amines having 1 to 8 carbon atoms;
Trioxane derivatives; And
Triacetin; containing, an alcohol fuel composition for preventing off.
The method of claim 6,
Based on 100 parts by weight of the alcohol
0.1 to 5 parts by weight of the organic or inorganic acid, 0.05 to 3 parts by weight of the organic or inorganic base, 0.1 to 5 parts by weight of the trioxane derivative, and 0.1 to 5 parts by weight of the triacetin, alcohol fuel for preventing off Composition.
The method of claim 6,
Based on the total weight of the composition
The alcohol is 80 to 98% by weight;
0.1 to 2% by weight of the organic or inorganic acid;
The inorganic or organic acid is 0.05 to 1% by weight;
The trioxane derivative is 0.1 to 2% by weight; And
The triacetin is 0.1 to 2% by weight; alcohol fuel composition for preventing off contained.
The method of claim 1,
The alcohol fuel composition is an alcohol fuel composition in a solid form or an alcohol fuel composition in a gel form, an alcohol fuel composition for preventing off.
In the manufacturing method of the alcohol fuel composition for preventing the turn off of claims 1 to 9,
(a) adding an alcohol, an organic or inorganic acid, and an organic or inorganic base and stirring; And
(b) adding and heating a trioxane derivative and triacetin after the step (a) and heating;
The method of claim 10,
The method further comprises the steps of (c) leaving the heated mixture to room temperature after step (b).

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