CN100537727C - A kind of solid alcohol fuel and preparation method thereof - Google Patents

A kind of solid alcohol fuel and preparation method thereof Download PDF

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CN100537727C
CN100537727C CNB200610114233XA CN200610114233A CN100537727C CN 100537727 C CN100537727 C CN 100537727C CN B200610114233X A CNB200610114233X A CN B200610114233XA CN 200610114233 A CN200610114233 A CN 200610114233A CN 100537727 C CN100537727 C CN 100537727C
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solid
alcohol fuel
solid alcohol
fuel
alcohol
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CN1944603A (en
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张晓娟
刘嘉喜
钱平
郝利民
杨文领
杜铁平
王昶
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Quartermaster Research Institute of General Logistics Department of CPLA
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Abstract

The invention discloses a kind of solid alcohol fuel, it is by industrial spirit 90.73%, stearic acid 4.76%, and NaOH 0.62%, paraffin 1.30%, distilled water 2.59% is percentage ratio by weight, is prepared from two steps under 70 ℃ constant temperature.Solid alcohol fuel of the present invention, have easily light, combustion heat value height, no black smoke, free from extraneous odour, burning back residue is few, shelf lives is long, does not soften characteristics such as separation, especially under vacuum anoxybiotic condition, still can keep flameholding, flame is vigorous, has good combustionproperty, still can burn in the plateau of more than 6300 meter of height above sea level or mountain region environment.The more common solid fuel of solid alcohol fuel of the present invention has the wider scope of application, uses in the high altitude anoxia area to have clear superiority, and be the first-selected thermal source of highlands household, travelling, motion or soldier's field exercise and plateau mountain operations.

Description

A kind of solid alcohol fuel and preparation method thereof
Technical field
The present invention relates to a kind of solid fuel, be specifically related to a kind of portable, safely, be easy to high heating value solid alcohol fuel that stores and transport and preparation method thereof.
Background technology
Solid fuel as a kind ofly carry, safe ready, economical and practical food and drink thermal source be widely used in dual-use.On military thermal source, the urotropine solid fuel be convenient to storage, and calorific value is very high, thereby so far still as the required fuel of individual combat, is widely used abroad or in the domestic army owing at normal temperatures bigger intensity is arranged.This product is a white solid, can outdoor use, and easy to carry, not volatile.But, since the characteristics of its chemical property (molecular formula is (CH 2) 6N 4), easily produce during burning human body and the deleterious oxynitrides of environment, and be difficult for fully burning, can produce a large amount of black smokes, pollute the heating apparatus, make troubles to repeated use, particularly under the high altitude anoxia situation, burning quality is low, is difficult to the solid-fuelled advantage of performance, and the price of raw material urotropine is higher, and the market competitiveness is poor.
On the other hand, on civilian thermal source, a variety of New-type fuel solid alcohols have now appearred, more traditional charcoal, it has firing-burning, flame size is even, flame temperature is even, the flame deviation is little, does not have dust and charcoal ash to descend slowly and lightly, safely cleaning, elegance easy to use, advantage such as easy to carry is widely used in fuel for chafing dish and open-air thermal source.Document is introduced up-to-date solid alcohol fuel (improvement of Productive Technology of Solid Alcohol, Wang Maoyuan etc., applicating technology at present, in April, 2002, Vol.29, No.4, P52-53), utilize industrial spirit, sodium hydroxide, stearic acid, paraffin, cupric nitrate to process for main raw material.The solid fuel product for preparing so still exists a lot of not enough: one, fusing point are low relatively can not be preserved for a long time under comparatively high temps; Its two, in preparation process, the topical gel phenomenon has just taken place easily, be difficult to realize industrialized continuous production; Its three, low at air pressure, under the oxygen condition, the burning vacuum tightness not enough, the time length is shorter, can not use in high altitude environment.Therefore, can not satisfy the Equipment Requirement of military solid alcohol fuel.
Summary of the invention
The purpose of this invention is to provide a kind of have easily light, combustion heat value height, no black smoke, free from extraneous odour, burning back residue is few, the following shelf lives of hot conditions is long, characteristics such as softening separation and the solid alcohol fuel that is suitable for using in the hypoxic plateau environment.
Another object of the present invention provides the preparation method of this solid alcohol fuel.
Solid alcohol fuel of the present invention, its by following component by weight percentage ratio form:
Industrial spirit 90.73%,
Stearic acid 4.76%,
NaOH 0.62%,
Paraffin 1.30%,
Distilled water 2.59%.
Wherein, the mass concentration of described industrial spirit is 95%.
The invention provides a kind of preparation method of solid alcohol fuel, according to above-mentioned assembly, all operate under 70 ℃ and carry out, 55.7% of stearic acid, paraffin and industrial spirit heated and stirring and refluxing in there-necked flask, sodium hydroxide, distilled water and 44.3% industrial spirit are heated in Erlenmeyer flask, then the solution in the Erlenmeyer flask is slowly injected there-necked flask, mixed solution continues 70 ℃ of heated and stirred, be poured in the container while hot, even, the translucent gelatinous solid that naturally cooling, coagulation forming obtain is solid alcohol fuel.
Among the above-mentioned preparation method, all operate in bath temperature and be in 70 ℃ the Water Tank with Temp.-controlled and carry out.
Described preparation method's concrete operations are:
The first step, stearic acid is dissolved in alcohol:
1. fixedly the bath temperature of Water Tank with Temp.-controlled is 70 ℃, and the mixing speed of electric mixer is 250r/min.
2. take by weighing 55.7% in stearic acid, paraffin and the industrial spirit respectively, add in the there-necked flask successively.Electric mixer, thermometer and reflux condensing tube are installed on there-necked flask then;
3. there-necked flask is heated in water-bath and stir, a small amount of alcohol of evaporation is got back in the there-necked flask behind the reflux condensation mode pipework condensation, till the colourless solution of being dissolved into homogeneous transparent.
In second step, sodium hydroxide is dissolved in alcohol:
1. distinguish 44.3% of weighing sodium hydroxide, distilled water and industrial spirit, join in the Erlenmeyer flask successively;
2. also Erlenmeyer flask is heated the identical time under condition same as described above with the time, until making it become the solution of homogeneous transparent;
The 3rd step, solution in the Erlenmeyer flask is slowly injected there-necked flask, mixed solution continues 70 ℃ of heated and stirred, 2 minutes reaction times, be poured into while hot in the container then, allow its naturally cooling, coagulation forming, pack, just can obtain the very high gelatinous solid alcohol fuel of even, translucent intensity.
Adopt the solid alcohol fuel of the inventive method preparation, have easily light, combustion heat value height, no black smoke, free from extraneous odour, burning back residue is few, at high temperature (as more than 50 ℃) shelf lives long, do not soften characteristics such as separation, especially under vacuum anoxybiotic condition, still can keep flameholding, flame is vigorous, has good combustionproperty, still can burn in the plateau of more than 6300 meter of height above sea level or mountain region environment, be that other like products can't be realized.The more common solid fuel of solid alcohol fuel of the present invention has the wider scope of application, having clear superiority at hot environment and the use of high altitude anoxia area, is the first-selected thermal source of desert area and highlands household, travelling, motion or soldier's field exercise and plateau mountain operations.
Description of drawings
Fig. 1 is the quantitative relationship curve between average combustionvelocity and the burn pot diameter in the solid alcohol combustion experiment.
Embodiment
A kind of good solid alcohol fuel should have easily light, combustion heat value height, no black smoke, free from extraneous odour, burning back residue is few, is convenient to store, characteristics such as softening separation.Also should have better economic in addition, raw material is easy to get, and technology is simple, and cost is low, is suitable for suitability for industrialized production.
Solid alcohol fuel of the present invention is a main raw material by Fatty Alcohol(C12-C14 and C12-C18), sodium stearate, dispersion agent, is to make Fatty Alcohol(C12-C14 and C12-C18) be frozen into needed burning block (being called the convenient fuel piece again) under the effect of gelifying agent sodium stearate.Softening when utilizing stearic acid to be heated, the character of solidifying again after the cooling is wrapped in Fatty Alcohol(C12-C14 and C12-C18) in the mesh skeleton of stearic acid sodium salt firmly.Since the stearic acid sodium salt cost an arm and a leg and market on be difficult for having bought.The present invention adopts at a certain temperature for this reason, stearic acid and sodium hydroxide hybrid reaction is made sodium stearate, thereby greatly reduce the cost of solid alcohol fuel.In solid fuel, add certain amount of dispersant, can change the microtexture of gel, increase solid-fuelled physical strength, improve solid-fuelled stability, because used dispersion agent also is a kind of hydrocarbon polymer, do not influence solid-fuelled combustioncharacteristics, and can make and burn more lastingly and can discharge very high heat energy, in actual applications safe ready more.
The used main raw material of the present invention has:
Industrial alcohol (containing alcohol 95 %): molecular formula CH 3CH 2OH, formal name used at school ethanol is commonly called as alcohol, and colourless transparent liquid has aroma smell, volatile, and is inflammable, and combustion heat value is 29.67kJ/g.Specific refractory power 1.3651, surface tension (20 ℃) 22.8mN/m, viscosity (20 ℃) 1.41mPas, vapour pressure (20 ℃) 5.732kPa, specific heat capacity (23 ℃) 2.58J/ (g ℃), 12.8 ℃ of flash-points, relative density 0.816,78.15 ℃ of boiling points, zero pour-114 ℃, 793 ℃ of spontaneous ignition temperatures.Ethanol is the main component of fuel in the present invention, and low price is easy to get.
Stearic acid: molecular formula CH 3(CH 2) 16COOH, the formal name used at school octadecanoic acid.White has glossy foliated lamellar solid.Molecular weight 284.48,67~70 ℃ of fusing points, 376.1 ℃ of boiling points (decomposition), 232 ℃ (2.0kPa), and relative density (20/4 ℃) 0.9408, specific refractory power 1.4299 (80 ℃), combustion heat value is 42.98kJ/g.Slowly volatilization under 90-100 ℃.Water-soluble hardly (20 ℃ time, only dissolve 0.00029g in 100 ml waters) are dissolved in alcohol, and acetone is soluble in ether, chloroform, benzene, tetracol phenixin, dithiocarbonic anhydride, amyl acetate-n and toluene etc.The commodity stearic acid is actually the mixture of 45% stearic acid and 55% Palmiticacid, and contains a small amount of oleic acid, slightly fatty smell.These product have pungency, and are nontoxic.As the main component of gel, be the important carrier that contains fuel alcohol in the present invention.
Sodium hydroxide: molecular formula NaOH, popular name caustic soda, caustic soda, caustic soda etc., molecular weight 40.00, density: 2.130g/cm 3, fusing point: 318 ℃, boiling point: 1390 ℃.Relative density is 2.130.The sodium hydroxide of pure product is water white crystal.Do not burn, but enough thermal ignition combustible matls may take place in easy the contact with water or moisture of solid.Industrial goods sodium hydroxide contains small amount of sodium chloride and yellow soda ash, is the White-opalescent solid.There are bulk, sheet, granular and bar-shaped etc., general designation solid caustic soda in the commercially available prod.The product popular name liquid caustic soda of solution state.The impurity of institute's sodium chloride-containing one class is more than solid caustic soda in the liquid caustic soda.Sodium hydroxide solution has strong basicity, skin, fabric, paper etc. is had the intensive corrosive nature, so will pay special attention to safety in use.In the present invention as stearic acid saponification reaction, the highly effective solidifying agent of formation gel.
Paraffin: polymer hydro carbons mixture is odorless, tasteless white solid when impure (then be yellow).Density rises with fusing point and increases, and is generally 0.88~0.915g/cm3,50~70 ℃ of fusing points, and 300~550 ℃ of boiling points, combustion heat value are 47.55kJ/g.Water insoluble, solubleness is very low in alcohol and ketone, is soluble in tetracol phenixin, trichloromethane, ether, benzene, paraffin ether, the various mineral oil of dithiocarbonic anhydride and the most of vegetables oil, and along with fusing point raises, solubleness reduces usually.Belong to saturated hydrocarbons, chemical property is stable, is difficult for reacting with bases, mineral acid and halogen.Meet hot melt, meet then combustion decomposition of high heat.As the dispersion agent of saponification reaction process, can suppress the caking that local saponification reaction forms in the present invention, improve the characteristic of the homogeneous distribution of gel.
Experimental principle:
Stearic acid with following reaction will take place after sodium hydroxide mixes:
Figure C200610114233D00061
The sodium stearate that reaction generates is the polar molecule of a long carbochain, is difficult for molten under the room temperature in alcohol.At a certain temperature, sodium stearate can be evenly dispersed in the liquid alcohol, then forms gelling system after the cooling, can tie up the alcohol molecular beam between interconnective macromole, makes alcohol be stagnant condition, thereby has obtained the alcohol of solid state.Gelation process is a noncrystalline process, so,, promote the stable of gelation process to carry out as far as possible in order to reduce the ununiformity of gelation process, guarantee that alkanol molecule stably is bound in the gelinite, so it is very important to add an amount of dispersion agent in the mixture of gelifying agent and alcohols.The effect of dispersion agent mainly is to make stearic lipophilic group under the avidity of dispersion agent hydro carbons hydrocarbon polymer, make and be uniformly dispersed, avoid sodium salt local excessive, solidify caking, form the solution of uniform stearic acid sodium salt and Fatty Alcohol(C12-C14 and C12-C18), then by reducing temperature, make solution slowly form the gel state of stearic acid sodium salt, liquid Fatty Alcohol(C12-C14 and C12-C18) homogeneous is dispersed among the reticulated structure of gel, form solid alcohol fuel with higher hardness and good stability.
The processing condition of preparation solid alcohol fuel of the present invention are: configure the mixing speed of electric mixer, the water-bath of Water Tank with Temp.-controlled is raised to 70 ℃; The reactor there-necked flask that a certain amount of raw material will be housed again places water-bath to heat certain hour; Simultaneously, under identical bath temperature, the Erlenmeyer flask that a certain amount of raw material is housed is heated the identical time; Then the solution in the Erlenmeyer flask is injected there-necked flask, hybrid reaction certain hour; At last product is poured in the container while hot, can be obtained as white as polished jade, the good solid alcohol of hardness behind the naturally cooling.
The preparation of embodiment 1, solid alcohol fuel
Raw material: paraffin 1.3 grams, stearic acid 4.76 grams, consumption 0.62 gram of NaOH, industrial spirit 90.73 grams, distilled water 2.59 grams.
Adopt two-step approach to prepare solid alcohol fuel, experimental procedure is:
The first step is dissolved stearic acid in alcohol.Concrete operations are as follows:
1. fixedly the bath temperature of Water Tank with Temp.-controlled is 70 ℃, and the mixing speed of electric mixer is 250r/min.
2. take by weighing stearic acid, paraffin and 50.55 gram industrial spirit respectively, add in the there-necked flask successively.Electric mixer, thermometer and reflux condensing tube are installed on there-necked flask then.
3. there-necked flask is heated in water-bath and stir, a small amount of alcohol of evaporation is got back in the there-necked flask behind the reflux condensation mode pipework condensation, till the colourless solution of being dissolved into homogeneous transparent.
Second step, sodium hydroxide to be dissolved in alcohol, concrete operations are as follows:
1. weighing sodium hydroxide and distilled water join in the Erlenmeyer flask respectively, make it dissolving, and then add 40.18 grams
Industrial spirit.
2. simultaneously also heated and stirred until the solution that becomes homogeneous transparent.
The 3rd step, solution in the Erlenmeyer flask is slowly injected there-necked flask, mixed solution continues 70 ℃ of heated and stirred, 2 minutes reaction times, be poured into while hot in the container then, allow its naturally cooling, coagulation forming, pack, just can obtain the very high gelatinous solid alcohol of even, translucent intensity.
Embodiment 2: the influence of each factor during the preparation solid alcohol fuel
The present embodiment The effect has the factor of influence to the solid alcohol fuel quality product.The heating in water bath time is 10min in this experiment, and the hybrid reaction time is 2min, mechanical stirring rotating speed 250r/min.Wherein alcohol (alcohol 1) consumption is 50.55g in the there-necked flask, and alcohol in the Erlenmeyer flask (alcohol 2) consumption is 40.18g (whole material benchmark is 100g).
One, Temperature Influence
Based on stearic fusing point is 67~70 ℃, temperature t=60 ℃ of experiment, 65 ℃, 70 ℃, 75 ℃ as four levels, to investigate the influence of temperature to experiment and product.
Experiment desired raw material consumption is as follows:
The consumption of experimental raw when table 1-1 investigates temperature factor
Figure C200610114233D00071
Wherein, alcohol 1 is the consumption in the there-necked flask, and alcohol 2 is the consumption in the Erlenmeyer flask, and promptly used alcohol accounts for 90.73% altogether in raw material.
This experiment has been investigated the influence of temperature to product performance by changing the temperature of water bath with thermostatic control, and the conclusion that draws sees the following form:
Concrete experimental phenomena when table 1-2 investigates temperature factor
Figure C200610114233D00081
As can be seen, existing partly solidified in reactor when temperature lower (promptly 60 ℃, 65 ℃) from table 1-2, this integrally curing influence to the back is very big, has had a strong impact on the quality of product; And when temperature too high (promptly 75 ℃), owing near the alcoholic acid boiling point, cause the alcohol reflux amount excessive, local leading solidified phenomenon has taken place also, the same with the low excessively situation of temperature also is a kind of unstable operation.So the index in every respect of the product when temperature is 70 ℃ has all reached standard, has satisfied the requirement of quartermaster equipment exhibition area.
Two, the influence of dispersant dosage
In this experiment, the consumption of fixing other raw materials is constant, only changes the consumption of dispersion agent paraffin, chooses five levels, with the variation of the investigating dispersant dosage influence (whole material benchmark is 100g) to quality product.
This experiment experimentizes respectively under above-mentioned experimental level by changing the consumption of dispersion agent, can draw to draw a conclusion:
Concrete experimental phenomena when table 2 is investigated dispersant dosage
Figure C200610114233D00082
As can be seen from Table 2, the adding of an amount of dispersion agent is very big to the influence of product hardness.Do not add dispersion agent, the product quality is softer, and gel particle is big, and hardness is low, poor stability; If add an amount of dispersion agent, then the hardness of product is improved, can cut arbitrarily, make different shape, as white as polished jade, higher transparency is arranged, this is because an amount of dispersion agent has affinity to stearic hydro carbons group, can avoid local phenomenon of solidifying, play extremely effectively dissemination because of acid base concentration is too high.But when dispersion agent was too much, because deliquescent difference is prone to demixing phenomenon, and solidifying agent was prone to muddy phenomenon after adding.When the add-on of dispersion agent was 1.30g, products obtained therefrom performance index in every respect met the requirements most.
Three, the influence of hardener dose
According to the acid-base reaction of stearic acid and sodium hydroxide as can be known, the consumption of solidifying agent sodium hydroxide directly influences the reaction mol ratio of stearic acid and sodium hydroxide, and this experiment is keeping carrying out different experiments under the constant situation of alcohol and stearic amount.Change the amount of sodium hydroxide earlier, it is adjusted to a suitable mol ratio.After the optimum amount of solidifying agent has been decided, keep the amount of solidifying agent constant, and then adjust the amount of alcohol, by a series of like this exploration and experimental study, determine the best solidifying agent and the amount of alcohol.
In this experiment, the consumption of fixing other raw materials is constant, NaOH and stearic mol ratio 0.73: 1,0.83: 1,0.92: 1,1.02: 1,1.12: 1 as five levels, with the variation of investigating hardener dose influence (whole material benchmark is 100g) to quality product.
Concrete experimental phenomena when table 3 is investigated hardener dose
Figure C200610114233D00091
As can be seen from Table 3, the adding of an amount of solidifying agent is also very big to the influence of quality product.Solidifying agent is NaOH and less water, and wherein mainly to act on be to make NaOH be in ionic condition to less water, makes it more abundant fully with stearic reaction, thereby obtains required gelifying agent stearic acid sodium salt.The consumption of NaOH adds too much or is very few, does not all reach expected effect.So when the add-on of solidifying agent was 0.62g, products obtained therefrom performance index in every respect met the requirements most.
Four, the influence of water content in the alcohol
In general, the purity of industrial alcohol 〉=95% (mass percent).If water content is too much in the alcohol, because water to the dissolution characteristics of sodium salt, can destroy the intensity of gel, will produce a very large impact the quality of product, and can reduce the combustion heat value of product, influence the use properties of solid alcohol fuel.
In this experiment, the purity of alcohol is investigated index as one, be about to the shared mass fraction 1%, 3%, 5%, 7%, 9% of water in the raw material alcohol as five levels, with the influence (whole material benchmark is 100g) of the water content of investigating alcohol to quality product.
Each amounts of components of experiment desired raw material is shown in table 2-4:
This experiment as variable, experimentizes the purity (being the water ratio in the alcohol) of alcohol, and it is as follows to obtain experimental result:
The consumption of experimental raw when table 4-1 investigates water ratio in the alcohol
Figure C200610114233D00101
Wherein, alcohol 1 is the consumption in the there-necked flask, and alcohol 2 is the consumption in the Erlenmeyer flask, and promptly used alcohol accounts for 90.73% altogether in raw material.
Concrete experimental phenomena when table 4-2 investigates alcohol purity factor
As can be seen, water content is very big to the quality product influence in the alcohol from table 4-2.When the water content of alcohol is very few, existing local solidification phenomenon in reactor; When the water content of alcohol is too high, owing to the dissolution characteristics of water to sodium salt, the intensity of gel will be destroyed, and the quality of product is subjected to very big influence, and the combustion heat value of product can reduce.So, when the water content of alcohol is 5%, prepared product best results.
Determine that by above experiment optimum process condition of the present invention and proportioning raw materials are: 70 ℃ of service temperatures, the chemical composition of solid alcohol fuel is respectively by weight, dispersion agent 1.30%, stearic acid 4.76%, the consumption 0.62% of NaOH, mass concentration is 95% industrial spirit 90.73%, distilled water 2.59%.Adopt the solid alcohol fuel smooth in appearance of this explained hereafter smooth, as white as polished jade, the gel particle uniform and delicate, hardness is big, stability is high, and resistance toheat is good, and quality is even, the easy-formation packing is particularly suitable for medium-sized and small enterprises and family and produces, and has vast market prospect.
The performance test of embodiment 3, solid alcohol fuel
Used solid alcohol fuel of the present invention all adopts embodiment 2 optimization processing condition and proportioning raw materials to prepare among this embodiment.To be main raw material with industrial spirit 500ml, sodium hydroxide 2.5g, stearic acid 14.5g, paraffin 4.0g, water 10g form with processes similarly to Example 2 for the analogous products (reference substance 1) of contrast, raw material.To the military solid fuel of urotropine (reference substance 2) in the same old way available from the new international health product company limited in east, Beijing.
1, the fusing point of solid alcohol fuel experiment:
Experimental technique: carry out a stable thermostatic water-circulator bath, concrete operation steps is as follows:
Before the mensuration, earlier bath temperature is reduced to 40 ℃, the fine taper bottle of putting into sample is fixed in water bath, slowly heating.Every 20min, once heat up at the beginning, intensification amplitude at every turn is 4 ℃, keeps 20min then, examines Erlenmeyer flask, and no abnormal phenomenon takes place.Continue elevated temperature, when bath temperature reaches 48 ℃, every 30min, once heat up, intensification amplitude at every turn is 1 ℃, keeps 30min then, examines phenomenon in the Erlenmeyer flask.Sample begins to occur slump and moistening phenomenon in Erlenmeyer flask, but also drop of liquid down occurs, and this shows that sample has begun fusing, and writing down at this moment, temperature is fusing point.
Fusing point test has the multiple data at least twice, measures the Erlenmeyer flask that all must more renew each time.
After repeating twice experiment, can determine that the actual temperature of water bath is 52 ℃, is 52 ℃ so confirm as the fusing point of solid alcohol fuel under 51 ℃ of the design temperatures of water bath.
For this reason by experimental result as can be known, the solid alcohol fuel fusing point that makes under optimum process condition of the present invention is 52 ℃, has good physicals, can store for a long time, is easy to carry or transports.The fusing point of the reference substance of measuring with quadrat method 1 is 50 ℃.
2, the combustion experiment of solid alcohol fuel
The combustion experiment method is as follows, on electronic balance, put heat-proof device, put the small vessels that will heat then in the above, put into solid fuel, ignition, regularly write down the amount of combustion time and solid fuel minimizing, can calculate the average combustionvelocity of incendiary speed and combustion processes, can also calculate the residue rate of combustion processes by these data.
The calculation formula of residue rate is as follows:
Figure C200610114233D00121
Experimental result is referring to table 5.
Experiment 1 Experiment 2 Experiment 3 Experiment 4 Experiment 5 Experiment 6
Tray for combustion quality (g) 53.86 27.16 26.70 24.49 8.35 12.83
The diameter of tray for combustion (cm) 5.948 3.960 3.520 2.964 2.520 2.024
Total mass (g) before the burning 69.61 34.26 34.39 30.25 22.98 15.47
Burning back total mass (g) 54.84 27.61 27.19 24.85 18.65 13.00
Average combustionvelocity (g/s) 0.035 0.017 0.012 0.009 0.007 0.005
The last extinction time (min) 7’ 6’26” 10’53” 11’10” 11’56” 9’55”
Residue rate (%) 6.22 6.34 6.37 6.25 6.48 6.44
State of combustion Flame is vigorous stable; Smoke-free and tasteless is nontoxic Flame is vigorous stable; Smoke-free and tasteless is nontoxic Flame is vigorous stable; Smoke-free and tasteless is nontoxic Flame is vigorous stable; Smoke-free and tasteless is nontoxic Flame is vigorous stable; Smoke-free and tasteless is nontoxic Flame is vigorous stable; Smoke-free and tasteless is nontoxic
By the The above results analysis as can be known, the combustion vessel of different diameter, solid alcohol fuel combustionvelocity therein is different.Under the condition of identical burning consumption, the area of container, promptly diameter is big more, and burned flame is prosperous more, and liberated heat is high more during burning, thereby combustionvelocity is just fast more, and the average combustionvelocity of solid alcohol fuel is along with the minimizing of diameter reduces.And when tray for combustion diameter hour, level of residue is higher relatively, and this is that complete inadequately during burning, the residue that obtains is many slightly naturally because the Fatty Alcohol(C12-C14 and C12-C18) that volatilizes during burning contacts fully inadequately with airborne oxygen.
In conjunction with above six groups of average combustionvelocities of being drawn of experiment, utilize non-linear regression can obtain quantitative relationship curve between combustionvelocity and the diameter, as shown in Figure 1.Curvilinear equation is Y=0.013X 1.833, relation conefficient is 0.9932.Illustrate that dependency is fine, wherein Y represents combustionvelocity, and unit is g/s, and X is expressed as the diameter of container, and unit is cm.
This equation explanation, the area of combustionvelocity and combustion vessel is not linear.Under same experimental conditions, the combustionvelocity of solid alcohol fuel in different combustion vessels is different.From the transmission ofenergy angle, burning area is excessive, and power loss is just big more, so will come reasonably to determine the size of combustion vessel according to heated container bottom area.Quantitative relationship between this combustionvelocity and the diameter has disclosed aptitude to burn.Know also that by regression curve the average combustionvelocity when solid alcohol fuel burns can also calculate the consumption of solid alcohol fuel under the different time simultaneously in the combustion vessel of each different area.
3, the water of solid alcohol fuel heating experiment
Experimental technique and combustion experiment are similar, 400g cold water frame be equipped with 13.8 the gram solid alcohol fuels tray for combustion on, after lighting, regularly write down the temperature of combustion time and water, water temperature raises and the relation of combustion time in the time of can drawing solid alcohol fuel and add the hot water experiment by these data.Wherein 400g water boils one bag of needed water yield of instant noodles just during field work.
After reaching boiling, the service requirements of field work has been satisfied in energy sustained combustion at least 3 minutes.
Similar approach is with the test of heating up water of the military solid fuel of urotropine.The result shows that when combustion vessel was arranged, combustionvelocity obviously descended, and firepower is less, under the colder situation of envrionment temperature, is difficult to water is boiled; The urotropine of no combustion vessel can also sustained combustion more than 3 minutes after reaching boiling, has satisfied the service requirements of field work.Experimentation is observed the military solid fuel of urotropine needs 40 seconds from the whole burning of lighting a fire, and is difficult for lighting, and extinguishes easily.
Under this description of test combustion conditions, the middle concentration of oxygen of environment and the transmission speed of oxygen are very important, and solid alcohol fuel combustionproperty is just better under the same conditions, even under anoxybiotic condition a little, also can fully burn, compare with the military solid fuel of urotropine, more can adapt to the highlands.
In addition, when incendiary experiment can also be seen the urotropine solid fuel ignition, because of poisonous, sharp aroma gas purgings such as oxynitrides, severe contamination environment, when in indoor or tent, burning especially, very big to the harm of human body.Burn under these two kinds of conditions, net result can see, is heated residual a large amount of coal smoke grey black on the hot face of container, is difficult to remove, and makes troubles to repeated use, thereby reduced the characteristics of solid fuel convenience.
4, the storage of solid alcohol fuel experiment
In order to investigate the storage requirement of solid alcohol fuel, at high temperature solid alcohol fuel is carried out repeatedly heating in water bath experiment, by to the examining of phenomenon, thereby obtain the temperature limitation of storing solid alcohol fuel.
The experimental technique and the fusing point test of storing experiment are similar, and the concrete operations step is as follows:
1. the solid alcohol fuel that will now do directly solidifies in there-necked flask, treat completion of cure after, the temperature of setting water bath with thermostatic control is 44 ℃, there-necked flask is fixed in the water-bath heats.
2. at the beginning every 1h, once heat up, intensification amplitude at every turn is 2 ℃, keeps 1h then, examines there-necked flask, the dry no moisture of sample surfaces, and also no abnormal phenomenon takes place.
3. continue elevated temperature, when bath temperature reaches 48 ℃, every 2h, once heat up, intensification amplitude at every turn is 1 ℃, keeps 2h, examines phenomenon in the there-necked flask.When temperature was 51 ℃, phenomenon was as shown in table 6 in the there-necked flask, was still keeping metastable state under this temperature.
4. when temperature rose to 52 ℃, behind the maintenance 1h, sample surfaces had oozed out a little liquid in the there-necked flask, and drop also appears in a bottle wall, and take out there-necked flask this moment, still had the liquid existence after the room temperature cooling.
5. hence one can see that, the temperature limitation value of the solid alcohol fuel storage requirement of this experiment development is 51 ℃, if envrionment temperature is higher than 51 ℃, solid alcohol fuel may be subjected to temperatures involved and the liquid alcohol that is wrapped in the high-molecular gel is oozed out, thereby cause the solid alcohol fuel downgrade.
When being 51 ℃, table 6 temperature stores experimental phenomena
Figure C200610114233D00131
Figure C200610114233D00141
As shown in Table 6, after heating half an hour, solid alcohol fuel with position that glass wall contacts on ooze out the liquid film of minute quantity, this is owing to contain a certain amount of moisture in the products material, and water is not lipophilic group, and through heat, the moisture at wall place easily oozes out from solid alcohol fuel.Through concrete test as can be known, cooling back solid alcohol fuel still can return to original state again, therefore to the quality influence of product seldom.After heating one hour, solid alcohol fuel surface drying, dripless; Through one hour, the solid alcohol fuel surface still kept dry again.This shows that solid alcohol fuel stores in order under this temperature, just can be under this temperature after certain packing long storage, this is because the gel component in the solid fuel of gel state is the stearate by the saponification reaction formation of soda acid, composition is very stable, can time to time change, as long as under suitable storage temperature, can preserve 3 years.
Continue attemperation, the storage temperature of solid alcohol fuel should be in ultimate temperature below 51 ℃ as can be known by repeatedly testing repeatedly.And the relative comparison product 1 storage temperature limit is 49 ℃, surpasses this limit, then can not keep good physical property.Usually solid alcohol fuel is stored at normal temperatures and is got final product, but under Special Circumstances such as desert Environment, hot environment, solid alcohol fuel of the present invention still has good performance index, therefore, product of the present invention time of guaranteeing the quality is long, be convenient to long-term deposit and long-distance transport, not only be suitable for hotel's catering industry, but also be suitable for tourism, field work and army's camp and field training.
5, the vacuum combustion experiment of solid alcohol fuel
This experiment is used to verify product of the present invention state of combustion under anoxic environment.
This experiment is to carry out in vacuum drying oven, regulates air absolute magnitude in the vacuum drying oven, the true nature environment when burning under plateau climate with simulated solid fuel by inflation valve and vacuum pump.
1. take by weighing the solid alcohol fuel of 1.57g, in diameter is the tray for combustion (tray for combustion of diameter minimum) of 2.024cm, light, treat to put into vacuum drying oven behind the flameholding, fasten loft drier, make in the whole loft drier air content certain, do not change with external environment;
2. with the power connection of vacuum pump, the absolute magnitude of air changes in the vacuum drying oven at this moment, thereby the reading of vacuum meter also changes, when the air absolute magnitude reduces gradually, the reading of vacuum meter constantly increases, and regulates inflation valve, and vacuum tightness is increased with stable speed, the combustion processes of sample is stable, is convenient to observe phenomena and record data;
3. examine the combustion phenomena of sample, note the variation of vacuum meter reading simultaneously, when sample extinguishes, write down the vacuum tightness of this moment under a certain vacuum tightness, be the gained experimental data;
4. for guaranteeing the reliability of experimental data, repeated experiments 3 times is got its mean value;
Equally, take by weighing the reference substance 1 of 1.57g respectively, the reference substance 2 urotropine solid fuels of 1.60g carry out parallel laboratory test under the same conditions.Because urotropine burns extremely insufficiently in tray for combustion, so urotropine is not adopted tray for combustion, directly lights in glass dish, treat flameholding after, put into loft drier.
The concrete phenomenon of vacuum burning contrast experiment of solid alcohol fuel and reference substance is as shown in table 7:
Table 7 vacuum combustion experiment recorder
Figure C200610114233D00151
Through observation shows that the solid alcohol fuel firing-burning is put into vacuum drying oven, connect vacuum-pump power supply, originally flame is very weak, treat that the air content of vacuum drying oven is stable after, flameholding, flame is vigorous, when experiment proceeded to the later stage, flame weakened again gradually, until extinguishing; The main fuel of reference substance 1 also is an alcohol, during burning and solid alcohol fuel combustion phenomena of the present invention basic identical; Reference substance 2 urotropines extremely are difficult for lighting, need light earlier, treat to put into vacuum drying oven again behind the flame stabilization, connect vacuum-pump power supply then, thereby flame is just very big at the beginning, after treating that the air content of vacuum drying oven is stable, burning also tends towards stability, and flame is vigorous, when experiment proceeds to the later stage, flame begins to weaken gradually, until extinguishing
Can draw solid alcohol fuel and the reference substance different burning behaviors when the anoxic by the vacuum combustion experiment, vacuum values according to the experimental result gained, again in conjunction with the conversion relation of vacuum tightness and sea level elevation, be 12 meters of every risings, normal atmosphere reduces 1mmHg, therefore by simple computation, just can draw the maximum value of the sea level elevation when fuel is flammable under the high altitude anoxia condition.
(1) solid alcohol fuel
For solid alcohol fuel, vacuum tightness is 0.07Mpa during fray-out of flame.
Because 1mmHg=133Pa=0000133MPa,
Can be scaled the pressure value P under the anaerobic environment 1=0.07/0.000133=526.32mmHg
Then the sea level elevation value under this pressure is H 1=52632 * 12=6315.84m
Thereby reach a conclusion: under hypoxic plateau environment, the maximum value that solid alcohol fuel can the incendiary sea level elevation is about 6300m.
(2) reference substance
For two kinds of reference substances, vacuum tightness is 0.06Mpa during fray-out of flame.
Because 1mmHg=133Pa=0.000133MPa,
Can be scaled the pressure value P under the anaerobic environment 2=0.06/0.000133=451.13mmHg
Then the sea level elevation value under this pressure is H 2=451.13 * 12=5413.56m
Thereby reach a conclusion: under hypoxic plateau environment, the maximum value that reference substance fuel can the incendiary sea level elevation is about 5400m.
Can learn that by above contrast experiment under vacuum anoxybiotic condition, solid alcohol fuel of the present invention has clear superiority, under high altitude anoxia rigorous environment like this, still can keep flameholding, flame is vigorous, has good combustionproperty.Reference substance then has deficiency slightly, and under same envrionment conditions, combustion flame is not prosperous, the combustion processes instability, and incendiary vacuum tightness ultimate value is also lower, and the combustionproperty of its each side all is not so good as solid alcohol fuel.By data calculated as can be known, solid alcohol fuel still can burn in the plateau of more than 6300 meter of height above sea level or mountain region environment, reference substance then can only height above sea level below 5400 meters the plateau or the mountain region environment in use.Obviously, solid alcohol fuel of the present invention is more suitable for being used for the high altitude anoxia area, has clear superiority, is the first-selected thermal source of plateau soldier's field exercise and plateau mountain operations, can be widely used in modernized quartermaster equipment exhibition area.

Claims (4)

1, a kind of solid alcohol fuel, its by following component by weight percentage ratio form:
Industrial spirit 90.73%,
Stearic acid 4.76%,
NaOH 0.62%,
Paraffin 1.30%,
Distilled water 2.59%;
The mass concentration of described industrial spirit is 95%.
2, a kind of preparation method of solid alcohol fuel, according to the described component of claim 1, all operate under 70 ℃ and carry out, 55.7% of stearic acid, paraffin and industrial spirit heated and stirring and refluxing in there-necked flask, sodium hydroxide, distilled water and 44.3% industrial spirit are heated in Erlenmeyer flask, then the solution in the Erlenmeyer flask is slowly injected there-necked flask, mixed solution continues 70 ℃ of heated and stirred, be poured in the container while hot, even, the translucent gelatinous solid that naturally cooling, coagulation forming obtain is solid alcohol fuel.
3, the preparation method of solid alcohol fuel according to claim 2 is characterized in that, all operates in bath temperature and be in 70 ℃ the Water Tank with Temp.-controlled to carry out.
4, the preparation method of solid alcohol fuel according to claim 3 is characterized in that, concrete operations are:
The first step, stearic acid is dissolved in alcohol:
1. fixedly the bath temperature of Water Tank with Temp.-controlled is 70 ℃, and the mixing speed of electric mixer is 250r/min.
2. take by weighing 55.7% in stearic acid, paraffin and the industrial spirit respectively, add in the there-necked flask successively.Electric mixer, thermometer and reflux condensing tube are installed on there-necked flask then;
3. there-necked flask is heated in water-bath and stir, a small amount of alcohol of evaporation is got back in the there-necked flask behind the reflux condensation mode pipework condensation, till the colourless solution of being dissolved into homogeneous transparent.
In second step, sodium hydroxide is dissolved in alcohol:
1. distinguish 44.3% of weighing sodium hydroxide, distilled water and industrial spirit, join in the Erlenmeyer flask successively;
2. also Erlenmeyer flask is heated the identical time under condition same as described above with the time, until making it become the solution of homogeneous transparent;
The 3rd step, solution in the Erlenmeyer flask is slowly injected there-necked flask, mixed solution continues 70 ℃ of heated and stirred, 2 minutes reaction times, be poured into while hot in the container then, allow its naturally cooling, coagulation forming, pack, just can obtain the very high gelatinous solid alcohol fuel of even, translucent intensity.
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