CN100537727C - A kind of solid alcohol fuel and preparation method thereof - Google Patents
A kind of solid alcohol fuel and preparation method thereof Download PDFInfo
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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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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 239000007787 solid Substances 0.000 title claims abstract description 93
- 239000000446 fuel Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 31
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 30
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008117 stearic acid Substances 0.000 claims abstract description 29
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- 238000000034 method Methods 0.000 claims description 22
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
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- Liquid Carbonaceous Fuels (AREA)
Abstract
Description
技术领域 technical field
本发明涉及一种固体燃料,具体涉及一种便携、安全、易于储存和运输的高热值固体醇燃料及其制备方法。The invention relates to a solid fuel, in particular to a portable, safe, easy-to-store and transport high-calorific-value solid alcohol fuel and a preparation method thereof.
背景技术 Background technique
固体燃料作为一种可随身携带、安全方便、经济实惠的餐饮热源已经广泛应用于军用和民用。在军用热源上,乌洛托品固体燃料由于在常温下有较大的强度,便于贮藏,而且热值很高,因而至今仍然作为单兵作战所需燃料,在国外或国内部队中被广泛使用。该产品为白色固体状,可户外使用,携带方便、不易挥发。但是,由于其化学性质的特点(分子式为(CH2)6N4),燃烧时易产生对人体及环境有害的氮氧化合物,且不易充分燃烧,会产生大量黑烟,污染加热用具,给重复使用带来不便,特别是在高原缺氧情况下,燃烧质量低,很难发挥固体燃料的优点,并且原料乌洛托品的价格较高,市场竞争力差。As a portable, safe, convenient, and economical food and beverage heat source, solid fuel has been widely used in military and civilian applications. As a heat source for military use, because of its high strength at room temperature, urotropine solid fuel is easy to store and has a high calorific value, so it is still used as fuel for individual combat and is widely used in foreign or domestic troops. . The product is white solid, can be used outdoors, is easy to carry, and is not volatile. However, due to its chemical properties (molecular formula (CH 2 ) 6 N 4 ), it is easy to produce nitrogen oxides that are harmful to the human body and the environment when burning, and it is not easy to burn fully, and it will produce a lot of black smoke, pollute heating appliances, and give Repeated use brings inconvenience, especially in the case of plateau hypoxia, the combustion quality is low, it is difficult to give full play to the advantages of solid fuel, and the price of raw material urotropine is relatively high, and the market competitiveness is poor.
另一方面,在民用热源上,现已出现了很多种新型燃料固体酒精,较传统的木炭,其具有一点即燃、火焰大小均匀、火焰温度均匀、火焰偏差小,没有粉尘和炭灰飘落,安全清洁,使用方便高雅,携带方便等优点,广泛应用于火锅燃料及野外热源。目前文献介绍最新的固体酒精燃料(固体酒精燃料生产工艺的改进,王茂元等,应用科技,2002年4月,Vol.29,No.4,P52-53),利用工业酒精、氢氧化钠、硬脂酸、石蜡、硝酸铜为主要原料加工而成。这样制备得到的固体燃料产品,仍然存在很多不足:其一,熔点相对低不能在较高温度下保存很长时间;其二,在制备过程中,容易就发生了局部凝胶现象,很难实现工业化的连续生产;其三,在气压低,氧气不足的条件下,燃烧真空度不够,持续时间较短,不能在高海拔环境中使用。因此,不能满足军用固体醇燃料的装备要求。On the other hand, in civil heat sources, many new types of fuel solid alcohol have appeared. Compared with traditional charcoal, it has the characteristics of instant combustion, uniform flame size, uniform flame temperature, small flame deviation, and no dust and charcoal falling. Safe and clean, easy to use and elegant, easy to carry and other advantages, it is widely used in hot pot fuel and outdoor heat source. Current literature introduces the latest solid alcohol fuel (improvement of solid alcohol fuel production process, Wang Maoyuan, etc., Applied Science and Technology, April 2002, Vol.29, No.4, P52-53), using industrial alcohol, sodium hydroxide, hard alcohol, etc. Fatty acid, paraffin, and copper nitrate are processed as main raw materials. The solid fuel product prepared in this way still has many deficiencies: first, the melting point is relatively low and cannot be stored for a long time at a higher temperature; Industrialized continuous production; third, under the condition of low air pressure and insufficient oxygen, the combustion vacuum degree is not enough and the duration is short, so it cannot be used in high altitude environment. Therefore, can not satisfy the equipment requirement of military solid alcohol fuel.
发明内容 Contents of the invention
本发明的目的是提供一种具有易点燃、燃烧热值高、无黑烟、无异味,燃烧后残渣少,高温条件下储存期长,不软化分离等特点并适于高原缺氧环境中使用的固体醇燃料。The purpose of the present invention is to provide a kind of fuel oil that has the characteristics of easy ignition, high combustion calorific value, no black smoke, no peculiar smell, less residue after combustion, long storage period under high temperature conditions, no softening and separation, and is suitable for use in plateau anoxic environment. solid alcohol fuel.
本发明的另一目的是提供这种固体醇燃料的制备方法。Another object of the present invention is to provide the preparation method of this solid alcohol fuel.
本发明的固体醇燃料,其由以下组分按重量百分数组成:Solid alcohol fuel of the present invention, it is made up of following component by weight percentage:
工业酒精 90.73%,Industrial alcohol 90.73%,
硬脂酸 4.76%,Stearic acid 4.76%,
NaOH 0.62%,NaOH 0.62%,
石蜡 1.30%,Paraffin 1.30%,
蒸馏水 2.59%。Distilled water 2.59%.
其中,所述工业酒精的质量浓度为95%。Wherein, the mass concentration of said industrial alcohol is 95%.
本发明提供一种固体醇燃料的制备方法,按照上述组配,全部操作在70℃下进行,将硬脂酸、石蜡和工业酒精的55.7%在三口烧瓶中加热并搅拌回流,将氢氧化钠、蒸馏水和44.3%工业酒精在锥形瓶中加热,然后将锥形瓶中的溶液缓慢注入三口烧瓶中,混合后的溶液继续在70℃加热搅拌,趁热将其倒入容器中,自然冷却,凝固成型得到的均匀、半透明的凝胶状固体即为固体醇燃料。The invention provides a method for preparing solid alcohol fuel. According to the above composition, all operations are carried out at 70°C. 55.7% of stearic acid, paraffin and industrial alcohol are heated in a three-necked flask, stirred and refluxed, and sodium hydroxide , distilled water and 44.3% industrial alcohol are heated in the conical flask, and then the solution in the conical flask is slowly injected into the three-necked flask, and the mixed solution is continued to be heated and stirred at 70°C, poured into the container while it is hot, and cooled naturally , The uniform, translucent gel-like solid obtained by solidification and molding is solid alcohol fuel.
上述制备方法中,全部操作在水浴温度为70℃的恒温水槽中进行。In the above preparation method, all operations are carried out in a constant temperature water tank with a water bath temperature of 70°C.
所述制备方法具体操作为:The specific operations of the preparation method are:
第一步,将硬脂酸在酒精中溶解:In the first step, stearic acid is dissolved in alcohol:
①固定恒温水槽的水浴温度为70℃,电动搅拌器的搅拌转速为250r/min。①The temperature of the water bath in the fixed constant temperature water tank is 70°C, and the stirring speed of the electric stirrer is 250r/min.
②分别称取硬脂酸、石蜡和工业酒精中的55.7%,依次加入三口烧瓶中。然后在三口瓶上安装电动搅拌器、温度计和回流冷凝管;② Weigh 55.7% of stearic acid, paraffin and industrial alcohol respectively, and add them into a three-necked flask in turn. Then install an electric stirrer, a thermometer and a reflux condenser on the there-necked flask;
③将三口瓶在水浴中加热并搅拌,蒸发的少量酒精经回流冷凝管冷凝后回到三口烧瓶中,直至溶解成均匀透明的无色溶液为止。③Heat and stir the three-necked flask in a water bath. A small amount of evaporated alcohol is condensed by the reflux condenser and returned to the three-necked flask until it dissolves into a uniform and transparent colorless solution.
第二步,将氢氧化钠在酒精中溶解:In the second step, dissolve sodium hydroxide in alcohol:
①分别称取氢氧化钠、蒸馏水和工业酒精的44.3%,依次加入到锥形瓶中;① Weigh 44.3% of sodium hydroxide, distilled water and denatured alcohol respectively, and add them in the Erlenmeyer flask successively;
②同时间也将锥形瓶在与上述相同条件下加热相同时间,直至使其成为均匀透明的溶液;② At the same time, heat the Erlenmeyer flask under the same conditions as above for the same time until it becomes a uniform and transparent solution;
第三步,将锥形瓶中的溶液缓慢注入三口烧瓶中,混合后的溶液继续在70℃加热搅拌,反应时间2分钟,然后趁热将其倒入容器中,让其自然冷却,凝固成型,密封包装,便可得到均匀、半透明的强度很高的凝胶状固体醇燃料。The third step is to slowly inject the solution in the Erlenmeyer flask into the three-necked flask, and continue to heat and stir the mixed solution at 70°C for 2 minutes, then pour it into the container while it is hot, let it cool naturally, and solidify into shape , sealed packaging, you can get a uniform, translucent high-strength gel-like solid alcohol fuel.
采用本发明方法制备的固体醇燃料,具有易点燃、燃烧热值高、无黑烟、无异味,燃烧后残渣少,在高温下(如50℃以上)储存期长,不软化分离等特点,尤其在真空缺氧的条件下,依然能够保持燃烧稳定,火焰旺盛,具有良好的燃烧性能,在海拔6300多米的高原或山地环境中仍然可以燃烧,是其他同类产品无法实现的。本发明固体醇燃料较普通固体燃料有更广的适用范围,在炎热环境以及高原缺氧地区使用具有明显优势,是沙漠地区以及高原地区家居、旅行、运动、或士兵野外训练以及高原山地作战的首选热源。The solid alcohol fuel prepared by the method of the present invention has the characteristics of easy ignition, high combustion calorific value, no black smoke, no peculiar smell, less residue after combustion, long storage period at high temperature (such as above 50 ° C), and no softening and separation. Especially under the condition of vacuum anoxic, it can still maintain stable combustion, strong flame and good combustion performance. It can still burn in the plateau or mountain environment with an altitude of more than 6300 meters, which is impossible for other similar products. The solid alcohol fuel of the present invention has a wider scope of application than ordinary solid fuels, and has obvious advantages in hot environments and plateau anoxic areas. Preferred heat source.
附图说明 Description of drawings
图1为固体醇燃烧实验中平均燃烧速度与燃烧罐直径之间的定量关系曲线。Figure 1 is a quantitative relationship curve between the average burning velocity and the diameter of the combustion tank in the solid alcohol combustion experiment.
具体实施方式 Detailed ways
一种好的固体醇燃料应该具有易点燃、燃烧热值高、无黑烟、无异味,燃烧后残渣少,便于储存,不软化分离等特点。另外还应该具有较好的经济性,原料易得,工艺简单,成本低,适合于工业化生产。A good solid alcohol fuel should have the characteristics of easy ignition, high combustion calorific value, no black smoke, no peculiar smell, less residue after combustion, easy storage, and no softening and separation. In addition, it should have good economy, easy to obtain raw materials, simple process and low cost, and is suitable for industrialized production.
本发明的固体醇燃料由脂肪醇、硬脂酸钠、分散剂为主要原料,是使脂肪醇在凝胶剂硬脂酸钠的作用下凝固成所需要的燃烧块(又称为方便燃料块)。利用硬脂酸受热时软化,冷却后又重新凝固的性质,将脂肪醇牢牢地包裹在硬脂酸钠盐的网状骨架中。由于硬脂酸钠盐的价格昂贵且市场上不易买到。为此本发明采用在一定温度下,将硬脂酸和氢氧化钠混合反应制得硬脂酸钠,从而大大降低了固体醇燃料的成本。在固体燃料中加入一定量的分散剂,可以改变凝胶的微观结构,增加固体燃料的物理强度,提高固体燃料的稳定性,由于所用的分散剂也是一种碳氢化合物,不影响固体燃料的燃烧特性,而且能使燃烧得更为持久并能够释放出很高的热能,在实际应用中更加安全方便。Solid alcohol fuel of the present invention is by fatty alcohol, sodium stearate, dispersant as main raw material, is to make fatty alcohol solidify into required combustion block (also known as convenient fuel block) under the effect of gelling agent sodium stearate ). Utilize the property that stearic acid softens when heated and resolidifies after cooling, the fatty alcohol is firmly wrapped in the network skeleton of sodium stearate. Because the price of sodium stearate is expensive and difficult to buy on the market. For this reason the present invention adopts under certain temperature, stearic acid and sodium hydroxide mixed reaction are made sodium stearate, thereby greatly reduced the cost of solid alcohol fuel. Adding a certain amount of dispersant to the solid fuel can change the microstructure of the gel, increase the physical strength of the solid fuel, and improve the stability of the solid fuel. Since the dispersant used is also a hydrocarbon, it does not affect the stability of the solid fuel. Combustion characteristics, and can make the combustion more durable and can release high heat energy, which is safer and more convenient in practical applications.
本发明所用主要原料有:Main raw material used in the present invention has:
工业乙醇(含乙醇95%):分子式CH3CH2OH,学名乙醇,俗称酒精,无色透明液体有酒香气味、易挥发,易燃,燃烧热值为29.67kJ/g。折射率1.3651,表面张力(20℃)22.8mN/m,粘度(20℃)1.41mPa·s,蒸气压(20℃)5.732kPa,比热容(23℃)2.58J/(g·℃),闪点12.8℃,相对密度0.816,沸点78.15℃,凝固点-114℃,自燃点793℃。在本发明中乙醇为燃料的主要成分,易得价格便宜。Industrial ethanol (contains 95% ethanol): molecular formula CH 3 CH 2 OH, scientific name ethanol, commonly known as alcohol, colorless transparent liquid with wine aroma, volatile, flammable, combustion calorific value 29.67kJ/g. Refractive index 1.3651, surface tension (20°C) 22.8mN/m, viscosity (20°C) 1.41mPa s, vapor pressure (20°C) 5.732kPa, specific heat capacity (23°C) 2.58J/(g°C), flash point 12.8°C, relative density 0.816, boiling point 78.15°C, freezing point -114°C, spontaneous ignition point 793°C. In the present invention, ethanol is the main component of the fuel, which is easy to obtain and cheap.
硬脂酸:分子式CH3(CH2)16COOH,学名十八烷酸。白色带有光泽的叶片状固体。分子量284.48,熔点67~70℃,沸点376.1℃(分解),232℃(2.0kPa),相对密度(20/4℃)0.9408,折射率1.4299(80℃),燃烧热值为42.98kJ/g。在90-100℃下慢慢挥发。几乎不溶于水(20℃时,100毫升水中只溶解0.00029g),溶于酒精,丙酮,易溶于乙醚、氯仿、苯、四氯化碳、二硫化碳、醋酸戊酯和甲苯等。商品硬脂酸实际上是45%硬脂酸和55%软脂酸的混合物,并含有少量油酸,略带脂肪气味。该品具有刺激性,无毒。在本发明中作为凝胶的主要成分,是包藏燃料酒精的重要载体。Stearic acid: molecular formula CH 3 (CH 2 ) 16 COOH, scientific name octadecanoic acid. White glossy leaf-like solid. Molecular weight 284.48, melting point 67-70°C, boiling point 376.1°C (decomposition), 232°C (2.0kPa), relative density (20/4°C) 0.9408, refractive index 1.4299 (80°C), heat of combustion 42.98kJ/g. Slowly volatilize at 90-100°C. Almost insoluble in water (only 0.00029g dissolved in 100ml of water at 20°C), soluble in alcohol, acetone, easily soluble in ether, chloroform, benzene, carbon tetrachloride, carbon disulfide, amyl acetate and toluene, etc. Commercial stearic acid is actually a mixture of 45% stearic acid and 55% palmitic acid, and contains a small amount of oleic acid, which has a slightly fatty smell. The product is irritating and non-toxic. In the present invention, as the main component of the gel, it is an important carrier for enclosing fuel alcohol.
氢氧化钠:分子式NaOH,俗名烧碱、火碱、苛性钠等,分子量40.00,密度:2.130g/cm3,熔点:318℃,沸点:1390℃。相对密度为2.130。纯品的氢氧化钠是无色透明的晶体。不燃烧,但固体易与水或水分接触可能发生足够的热引燃可燃材料。工业品氢氧化钠含有少量氯化钠和碳酸钠,是白色不透明固体。市售产品有块状、片状、粒状和棒状等,统称固碱。溶液状态的产品俗名液碱。液碱中所含氯化钠一类的杂质,要比固碱多。氢氧化钠溶液具有强碱性,对皮肤、织物、纸张等有强烈的腐蚀作用,所以在使用时要特别注意安全。在本发明中作为硬脂酸皂化反应、形成凝胶十分有效的固化剂。Sodium hydroxide: Molecular formula NaOH, commonly known as caustic soda, caustic soda, caustic soda, etc., molecular weight: 40.00, density: 2.130g/cm 3 , melting point: 318°C, boiling point: 1390°C. The relative density is 2.130. Pure sodium hydroxide is a colorless and transparent crystal. Not combustible, but solid Contact with water or moisture may generate sufficient heat to ignite combustible materials. Industrial sodium hydroxide contains a small amount of sodium chloride and sodium carbonate, and is a white opaque solid. Commercially available products are block, sheet, granular and rod, collectively referred to as solid alkali. The common name of the product in the solution state is liquid caustic soda. Liquid caustic soda contains more impurities such as sodium chloride than solid caustic soda. Sodium hydroxide solution is highly alkaline and has a strong corrosive effect on skin, fabrics, paper, etc., so special attention should be paid to safety when using it. In the present invention, it is a very effective curing agent for stearic acid saponification reaction and gel formation.
石蜡:高分子烃类混合物,为无臭、无味的白色固体(含杂质时则为黄色)。密度随熔点上升而增加,通常为0.88~0.915g/cm3,熔点50~70℃,沸点300~550℃,燃烧热值为47.55kJ/g。不溶于水,在醇及酮中溶解度很低,易溶于四氯化碳、三氯甲烷、乙醚、苯、石蜡醚、二硫化碳各种矿物油及大多数植物油中,通常随着熔点升高,溶解度降低。属饱和烃类,化学性质稳定,不易与碱类、无机酸及卤素起反应。遇热熔化,遇高热则燃烧分解。在本发明中用作皂化反应过程的分散剂,可以抑制局部皂化反应形成的结块,提高凝胶的均一分布的特性。Paraffin: a mixture of polymer hydrocarbons, which is an odorless and tasteless white solid (yellow when it contains impurities). The density increases with the melting point, usually 0.88-0.915g/cm3, the melting point is 50-70°C, the boiling point is 300-550°C, and the heat of combustion is 47.55kJ/g. Insoluble in water, very low solubility in alcohols and ketones, easily soluble in carbon tetrachloride, chloroform, ether, benzene, paraffin ether, carbon disulfide, various mineral oils and most vegetable oils, usually with the increase of melting point, Solubility decreased. It is a saturated hydrocarbon with stable chemical properties and is not easy to react with alkalis, inorganic acids and halogens. It melts when exposed to heat, and decomposes when exposed to high heat. Used as a dispersant in the process of saponification reaction in the present invention, it can inhibit the agglomeration formed by local saponification reaction and improve the uniform distribution of the gel.
实验原理:Experimental principle:
硬脂酸与氢氧化钠混合后将发生下列反应:After stearic acid is mixed with sodium hydroxide, the following reactions will occur:
反应生成的硬脂酸钠是一个长碳链的极性分子,室温下在酒精中不易溶。在一定的温度下,硬脂酸钠可以均匀地分散在液体酒精中,而冷却后则形成凝胶体系,能够把酒精分子束缚在相互连接的大分子之间,使酒精呈不流动状态,从而得到了固体状态的酒精。凝胶过程是一个非结晶过程,所以,为了降低凝胶过程的不均匀性,尽可能促进凝胶过程的稳定进行,保证醇类分子稳定地被束缚在凝胶体中,所以在凝胶剂和醇类的混合物中加入适量的分散剂极为重要。分散剂的作用主要是使硬脂酸的亲油基团在分散剂烃类碳氢化合物的亲和力下,使得分散均匀,避免钠盐的局部过量、凝固结块,形成均匀的硬脂酸钠盐和脂肪醇的溶液,然后通过降低温度,使溶液缓慢形成硬脂酸钠盐的凝胶状态,使液态的脂肪醇均一分散在凝胶的网状结构之中,形成具有较高硬度和稳定性好的固体醇类燃料。The sodium stearate produced by the reaction is a polar molecule with a long carbon chain, which is not easily soluble in alcohol at room temperature. At a certain temperature, sodium stearate can be evenly dispersed in liquid alcohol, and after cooling, it will form a gel system, which can bind alcohol molecules between interconnected macromolecules, making alcohol in a non-flowing state, thereby Alcohol in a solid state is obtained. The gel process is a non-crystallization process. Therefore, in order to reduce the inhomogeneity of the gel process, the stability of the gel process should be promoted as much as possible to ensure that the alcohol molecules are stably bound in the gel. Therefore, in the gel It is extremely important to add an appropriate amount of dispersant to the mixture with alcohols. The function of the dispersant is mainly to make the lipophilic group of stearic acid under the affinity of the hydrocarbon hydrocarbon of the dispersant, make the dispersion uniform, avoid local excess of sodium salt, solidification and agglomeration, and form a uniform sodium stearate and a solution of fatty alcohol, and then by lowering the temperature, the solution slowly forms a gel state of sodium stearate, so that the liquid fatty alcohol is uniformly dispersed in the network structure of the gel, forming a gel with high hardness and stability Good solid alcohol fuel.
制备本发明固体醇燃料的工艺条件是:设定好电动搅拌器的搅拌转速,将恒温水槽的水浴升到70℃;再将装有一定量原料的反应釜三口烧瓶置于水浴中加热一定时间;同时,在相同水浴温度下,将装有一定量原料的锥形瓶加热相同时间;然后将锥形瓶中的溶液注入三口烧瓶中,混合反应一定时间;最后将产品趁热倒入容器内,自然冷却后即可得到洁白如玉、硬度很好的固体酒精。The process conditions for preparing the solid alcohol fuel of the present invention are as follows: set the stirring speed of the electric stirrer, raise the water bath of the constant temperature water tank to 70°C; then place the three-neck flask of the reaction kettle with a certain amount of raw materials in the water bath to heat for a certain period of time; At the same time, at the same water bath temperature, heat the conical flask with a certain amount of raw materials for the same time; then inject the solution in the conical flask into the three-necked flask, and mix and react for a certain period of time; finally, pour the product into the container while it is hot, and naturally After cooling, solid alcohol as white as jade and with good hardness can be obtained.
实施例1、固体醇燃料的制备Embodiment 1, the preparation of solid alcohol fuel
原料:石蜡1.3克,硬脂酸4.76克,NaOH的用量0.62克,工业酒精90.73克,蒸馏水2.59克。Raw materials: 1.3 grams of paraffin, 4.76 grams of stearic acid, 0.62 grams of NaOH, 90.73 grams of industrial alcohol, and 2.59 grams of distilled water.
采用两步法制备固体醇燃料,实验步骤为:Adopt two-step method to prepare solid alcohol fuel, experimental procedure is:
第一步,将硬脂酸在酒精中溶解。具体操作如下:In the first step, stearic acid is dissolved in alcohol. The specific operation is as follows:
①固定恒温水槽的水浴温度为70℃,电动搅拌器的搅拌转速为250r/min。①The temperature of the water bath in the fixed constant temperature water tank is 70°C, and the stirring speed of the electric stirrer is 250r/min.
②分别称取硬脂酸、石蜡和50.55克工业酒精,依次加入三口烧瓶中。然后在三口瓶上安装电动搅拌器、温度计和回流冷凝管。② Weigh stearic acid, paraffin and 50.55 grams of industrial alcohol respectively, and add them into a three-necked flask in turn. Then install an electric stirrer, a thermometer and a reflux condenser on the three-neck flask.
③将三口瓶在水浴中加热并搅拌,蒸发的少量酒精经回流冷凝管冷凝后回到三口烧瓶中,直至溶解成均匀透明的无色溶液为止。③Heat and stir the three-necked flask in a water bath. A small amount of evaporated alcohol is condensed by the reflux condenser and returned to the three-necked flask until it dissolves into a uniform and transparent colorless solution.
第二步,将氢氧化钠在酒精中溶解,具体操作如下:In the second step, sodium hydroxide is dissolved in alcohol, and the specific operation is as follows:
①分别称取氢氧化钠和蒸馏水加入到锥形瓶中,使之溶解,然后再加入40.18克① Weigh sodium hydroxide and distilled water into the Erlenmeyer flask to dissolve them, and then add 40.18 grams
工业酒精。industrial alcohol.
②同时也加热搅拌直至成为均匀透明的溶液。②At the same time, heat and stir until it becomes a uniform and transparent solution.
第三步,将锥形瓶中的溶液缓慢注入三口烧瓶中,混合后的溶液继续在70℃加热搅拌,反应时间2分钟,然后趁热将其倒入容器中,让其自然冷却,凝固成型,密封包装,便可得到均匀、半透明的强度很高的凝胶状固体酒精。The third step is to slowly inject the solution in the Erlenmeyer flask into the three-necked flask, and continue to heat and stir the mixed solution at 70°C for 2 minutes, then pour it into the container while it is hot, let it cool naturally, and solidify into shape , sealed packaging, you can get uniform, translucent high-strength gel-like solid alcohol.
实施例2:制备固体醇燃料时各因素的影响Embodiment 2: the influence of each factor when preparing solid alcohol fuel
本实施例详细考察对固体醇燃料产品质量具有影响的因素。本实验中水浴加热时间为10min,混合反应时间为2min,机械搅拌转速250r/min。其中三口烧瓶中酒精(酒精1)用量为50.55g,锥形瓶中酒精(酒精2)用量为40.18g(整个物料基准为100g)。This example examines in detail the factors that have an impact on the quality of solid alcohol fuel products. In this experiment, the heating time in the water bath was 10 minutes, the mixing reaction time was 2 minutes, and the mechanical stirring speed was 250 r/min. Wherein the alcohol (alcohol 1) consumption is 50.55g in the three-necked flask, and the alcohol (alcohol 2) consumption is 40.18g (the whole material benchmark is 100g) in the Erlenmeyer flask.
一、温度的影响1. The influence of temperature
基于硬脂酸的熔点为67~70℃,把实验的温度t=60℃、65℃、70℃、75℃作为四个水平,以考察温度对实验及产品的影响。Based on the melting point of stearic acid being 67-70°C, the experimental temperature t=60°C, 65°C, 70°C, and 75°C were taken as four levels to investigate the influence of temperature on the experiment and the product.
实验所需原料用量如下:The amount of raw materials required for the experiment is as follows:
表1-1 考察温度因素时实验原料的用量Table 1-1 The amount of experimental raw materials when examining the temperature factor
其中,酒精1为三口瓶中的用量,酒精2为锥形瓶中的用量,即所用酒精在原料中共占90.73%。Wherein, alcohol 1 is the amount in the there-necked flask, and
本实验通过改变恒温水浴的温度,考察了温度对产品性能的影响,得出的结论见下表:In this experiment, by changing the temperature of the constant temperature water bath, the influence of temperature on the performance of the product was investigated, and the conclusions drawn are shown in the following table:
表1-2 考察温度因素时的具体实验现象Table 1-2 Specific experimental phenomena when examining temperature factors
从表1-2中可以看出,当温度较低(即60℃、65℃),在反应釜中已有部分固化,这对后面的整体固化影响很大,严重影响了产品的质量;而当温度过高(即75℃),由于接近乙醇的沸点,导致醇回流量过大,也发生了局部超前固化的现象,与温度过低的情况一样也是一种不稳定操作。所以,温度为70℃时的产品在各方面的指标都达到了标准,满足了军需装备的要求。It can be seen from Table 1-2 that when the temperature is low (i.e. 60°C, 65°C), the reaction kettle has been partially cured, which has a great impact on the subsequent overall curing and seriously affects the quality of the product; and When the temperature is too high (that is, 75°C), because it is close to the boiling point of ethanol, the reflux of alcohol is too large, and the phenomenon of local advanced curing also occurs, which is also an unstable operation like the case of too low temperature. Therefore, the products at a temperature of 70°C have reached the standard in all aspects and met the requirements of military equipment.
二、分散剂用量的影响2. The effect of the amount of dispersant
在本实验中,固定其他原料的用量不变,只改变分散剂石蜡的用量,选取五个水平,以考察分散剂用量的变化对产品质量的影响(整个物料基准为100g)。In this experiment, the consumption of other raw materials is fixed, only the consumption of dispersant paraffin is changed, and five levels are selected to investigate the influence of the variation of dispersant consumption on product quality (the whole material benchmark is 100g).
本实验通过改变分散剂的用量,在上述实验水平下分别进行实验,可得出以下结论:In this experiment, by changing the amount of dispersant, experiments were carried out at the above-mentioned experimental level, and the following conclusions can be drawn:
表2 考察分散剂用量时的具体实验现象Table 2 Specific experimental phenomena when investigating the amount of dispersant
从表2中可以看出,适量分散剂的加入对产品硬度的影响很大。不加分散剂,产品质地较软,凝胶颗粒大,硬度低,稳定性差;如果加入适量的分散剂,则产品的硬度得到提高,可以任意切割,制作各种形状,洁白如玉,有较高的透明度,这是由于适量的分散剂对硬脂酸的烃类基团具有亲和性,能够避免局部因酸碱浓度过高而凝固的现象,起到了极其有效的分散作用。但当分散剂过多时,由于溶解性的差异,易出现分层现象,而且,固化剂加入后易出现混浊现象。当分散剂的加入量为1.30g时,所得产品在各方面的性能指标最符合要求。It can be seen from Table 2 that the addition of an appropriate amount of dispersant has a great influence on the hardness of the product. Without dispersant, the product has soft texture, large gel particles, low hardness, and poor stability; if an appropriate amount of dispersant is added, the hardness of the product will be improved, and it can be cut arbitrarily and made into various shapes. High transparency, this is because a proper amount of dispersant has affinity to the hydrocarbon group of stearic acid, which can avoid local solidification due to excessive acid-base concentration, and has played an extremely effective dispersion effect. However, when the dispersant is too much, due to the difference in solubility, stratification is easy to occur, and turbidity is easy to occur after the curing agent is added. When the added amount of the dispersant was 1.30g, the performance index of the obtained product most met the requirements in all aspects.
三、固化剂用量的影响3. The effect of curing agent dosage
根据硬脂酸与氢氧化钠的酸碱反应可知,固化剂氢氧化钠的用量直接影响硬脂酸与氢氧化钠的反应摩尔比,本实验在保持酒精和硬脂酸的量不变的情况下,进行不同实验。先改变氢氧化钠的量,将其调整到一个合适的摩尔比。在固化剂的最佳用量已经确定下来后,保持固化剂的量不变,然后再调整酒精的量,通过这样一系列的探索和实验研究,确定最佳的固化剂和酒精的量。According to the acid-base reaction of stearic acid and sodium hydroxide, it can be known that the amount of curing agent sodium hydroxide directly affects the reaction molar ratio of stearic acid and sodium hydroxide. In this experiment, the amount of alcohol and stearic acid is kept constant. Next, different experiments were carried out. First change the amount of sodium hydroxide to adjust it to a suitable molar ratio. After the optimum amount of curing agent has been determined, keep the amount of curing agent unchanged, and then adjust the amount of alcohol. Through such a series of exploration and experimental research, determine the optimal amount of curing agent and alcohol.
在本实验中,固定其他原料的用量不变,把NaOH与硬脂酸的摩尔比0.73∶1、0.83∶1、0.92∶1、1.02∶1、1.12∶1作为五个水平,以考察固化剂用量的变化对产品质量的影响(整个物料基准为100g)。In this experiment, the amount of fixed other raw materials remains unchanged, and the molar ratio of NaOH to stearic acid is 0.73:1, 0.83:1, 0.92:1, 1.02:1, 1.12:1 as five levels to investigate the curing agent The impact of dosage changes on product quality (the whole material benchmark is 100g).
表3 考察固化剂用量时的具体实验现象Table 3 Specific experimental phenomena when investigating the amount of curing agent
从表3中可以看出,适量固化剂的加入对产品质量的影响也很大。固化剂为NaOH和少量水,其中少量水主要作用是使NaOH处于离子状态,使之与硬脂酸的反应更为充分完全,从而得到所需的凝胶剂硬脂酸钠盐。NaOH的用量加得过多或过少,都达不到预期的效果。所以,当固化剂的加入量为0.62g时,所得产品在各方面的性能指标最符合要求。It can be seen from Table 3 that the addition of an appropriate amount of curing agent also has a great impact on product quality. The curing agent is NaOH and a small amount of water, wherein the main function of a small amount of water is to make NaOH in an ion state, so that the reaction with stearic acid is more fully and completely, thereby obtaining the required gelling agent sodium stearate. If the amount of NaOH added is too much or too little, the desired effect cannot be achieved. Therefore, when the addition amount of curing agent is 0.62g, the performance index of the obtained product meets the requirements most in all aspects.
四、酒精中含水量的影响4. The influence of water content in alcohol
一般来说,工业用酒精的纯度≥95%(质量百分数)。如果酒精中含水量过多,由于水对钠盐的溶解特性,会破坏凝胶的强度,对产品的质量将会产生很大影响,并且还会降低产品的燃烧热值,影响固体酒精燃料的使用性能。Generally speaking, the purity of industrial alcohol is more than or equal to 95% (mass percentage). If there is too much water in the alcohol, due to the solubility of water to sodium salt, it will destroy the strength of the gel, which will have a great impact on the quality of the product, and will also reduce the combustion calorific value of the product, affecting the performance of solid alcohol fuel. Use performance.
在本实验中,将酒精的纯度作为一个考察指标,即将原料酒精中水所占的质量分率1%、3%、5%、7%、9%作为五个水平,以考察酒精的含水量对产品质量的影响(整个物料基准为100g)。In this experiment, the purity of alcohol is used as an investigation index, that is, the mass fraction of water in raw alcohol is 1%, 3%, 5%, 7%, and 9% as five levels to investigate the water content of alcohol Impact on product quality (the whole material benchmark is 100g).
实验所需原料各组分用量如表2-4所示:The amount of each component of the raw materials required for the experiment is shown in Table 2-4:
本实验将酒精的纯度(即酒精中的含水率)作为变量,进行实验,得到实验结果如下:In this experiment, the purity of the alcohol (i.e. the water content in the alcohol) is used as a variable, and the experiment is carried out, and the experimental results are as follows:
表4-1 考察酒精中含水率时实验原料的用量Table 4-1 The amount of experimental raw materials when examining the water content in alcohol
其中,酒精1为三口瓶中的用量,酒精2为锥形瓶中的用量,即所用酒精在原料中共占90.73%。Wherein, alcohol 1 is the amount in the there-necked flask, and
表4-2 考察酒精纯度因素时的具体实验现象Table 4-2 Specific experimental phenomena when examining alcohol purity factors
从表4-2中可以看出,酒精中含水量对产品质量影响很大。当酒精的含水量过少时,在反应釜中已有局部固化现象;当酒精的含水量过高时,由于水对钠盐的溶解特性,凝胶的强度将破坏,产品的质量受到很大影响,产品的燃烧热值会降低。所以,当酒精的含水量为5%,所制得的产品效果最佳。It can be seen from Table 4-2 that the water content in alcohol has a great influence on product quality. When the water content of the alcohol is too small, there is a partial solidification phenomenon in the reaction kettle; when the water content of the alcohol is too high, the strength of the gel will be destroyed due to the solubility of the sodium salt by water, and the quality of the product will be greatly affected. , the combustion calorific value of the product will decrease. Therefore, when the water content of the alcohol is 5%, the resulting product works best.
通过以上实验确定本发明最佳工艺条件以及原料配比为:操作温度70℃,固体醇燃料的化学组分分别为按重量比,分散剂1.30%,硬脂酸4.76%,NaOH的用量0.62%,质量浓度为95%工业酒精90.73%,蒸馏水2.59%。采用该工艺生产的固体醇燃料外观光滑平整,洁白如玉,凝胶颗粒均匀细致,硬度大,稳定性高,耐热性能良好,质地均匀,易成型包装,特别适合中小企业和家庭生产,具有广阔的市场前景。Determine optimum process condition of the present invention and raw material proportioning by above experiment: operating temperature 70 ℃, the chemical composition of solid alcohol fuel is respectively by weight ratio, dispersant 1.30%, stearic acid 4.76%, the consumption of NaOH 0.62% , the mass concentration is 90.73% of 95% denatured alcohol and 2.59% of distilled water. The solid alcohol fuel produced by this process is smooth and flat, white as jade, uniform and fine gel particles, high hardness, high stability, good heat resistance, uniform texture, easy to form and package, especially suitable for small and medium-sized enterprises and household production, with Broad market prospects.
实施例3、固体醇燃料的性能测试Embodiment 3, the performance test of solid alcohol fuel
该实施例中所用本发明固体醇燃料均采用实施例2优化工艺条件与原料配比制备得到。对照的类似产品(对照品1),原料用工业酒精500ml、氢氧化钠2.5g、硬脂酸14.5g、石蜡4.0g、水10g为主要原料用与实施例2同样工艺加工而成。对照样乌洛托品(对照品2)军用固体燃料购自北京东新国际保健品有限公司。The solid alcohol fuels of the present invention used in this example are prepared by optimizing the process conditions and raw material ratios in Example 2. The similar product (reference substance 1) of contrast, raw material industrial alcohol 500ml, sodium hydroxide 2.5g, stearic acid 14.5g, paraffin 4.0g, water 10g are that main raw material is processed with the same process as
1、固体醇燃料的熔点实验:1. Melting point experiment of solid alcohol fuel:
实验方法:在一个稳定的超级恒温水浴进行,具体的操作步骤如下:Experiment method: carried out in a stable super constant temperature water bath, the specific operation steps are as follows:
测定前,先将水浴温度降至40℃,将已放入样品的小锥形瓶固定于水浴槽中,慢慢加热。一开始每隔20min,进行一次升温,每次升温幅度为4℃,然后保持20min,仔细观察锥形瓶,无异常现象发生。继续升高温度,当水浴温度达到48℃时,每隔30min,进行一次升温,每次升温幅度为1℃,然后保持30min,仔细观察锥形瓶中现象。当锥形瓶中样品开始出现塌落和湿润现象,而且还出现下滴液体,这表明样品已开始熔化,记下此时温度即为熔点。Before the measurement, lower the temperature of the water bath to 40°C, fix the small Erlenmeyer flask with the sample in the water bath, and heat it slowly. At the beginning, the temperature was raised every 20 minutes, each time the temperature was raised to 4°C, and then kept for 20 minutes, and the Erlenmeyer flask was carefully observed, no abnormal phenomenon occurred. Continue to raise the temperature. When the temperature of the water bath reaches 48°C, raise the temperature every 30 minutes with a temperature increase of 1°C each time, and then keep it for 30 minutes. Carefully observe the phenomenon in the Erlenmeyer flask. When the sample in the Erlenmeyer flask begins to slump and wet, and there is also dripping liquid, this indicates that the sample has begun to melt, and the temperature at this time is recorded as the melting point.
熔点测定,至少有两次重复的数据,每一次测定都必须更换新的锥形瓶。For the determination of melting point, there are at least two repeated data, and a new Erlenmeyer flask must be replaced for each determination.
在重复两次实验之后,可以确定在水浴槽的设定温度51℃下,水浴槽的实际温度为52℃,所以确认为固体醇燃料的熔点为52℃。After repeating the experiment twice, it can be determined that the actual temperature of the water bath is 52 °C when the set temperature of the water bath is 51 °C, so it is confirmed that the melting point of the solid alcohol fuel is 52 °C.
为此由实验结果可知,在本发明最佳工艺条件下制得的固体醇燃料熔点为52℃,具有良好的物理性能,可长时间储存,便于携带或运输。同样方法测定的对照品1的熔点为50℃。For this reason, it can be seen from the experimental results that the solid alcohol fuel produced under the optimum process conditions of the present invention has a melting point of 52° C., has good physical properties, can be stored for a long time, and is easy to carry or transport. The melting point of reference substance 1 measured by the same method was 50°C.
2、固体醇燃料的燃烧实验2. Combustion experiment of solid alcohol fuel
燃烧实验方法如下,在电子天平上放上隔热装置,然后在上面放上所要加热的小容器,放入固体燃料,点火燃烧,定时记下燃烧时间与固体燃料减少的量,通过这些数据能计算出燃烧的速度以及燃烧过程的平均燃烧速度,还可以计算出燃烧过程的残渣率。The combustion experiment method is as follows. Put a thermal insulation device on the electronic balance, then put a small container to be heated on it, put in solid fuel, ignite and burn, and record the burning time and the amount of solid fuel reduction at regular intervals. Through these data, you can Calculate the burning speed and the average burning speed of the burning process, and also calculate the residue rate of the burning process.
残渣率的计算公式如下:The formula for calculating the residue rate is as follows:
实验结果参见表5。See Table 5 for the experimental results.
由上述结果分析可知,不同直径的燃烧容器,固体醇燃料在其中的燃烧速度是不同的。在相同的燃烧用量的条件下,容器的面积,即直径越大,燃烧的火焰越旺,燃烧时放出的热量越高,因而燃烧速度就越快,固体醇燃料的平均燃烧速度是随着直径的减少而降低的。而且,当燃烧盘直径小时,残渣量相对较高,这是因为燃烧时挥发出的脂肪醇与空气中的氧气接触不够充分,燃烧时不够完全,得到的残渣自然稍多。From the analysis of the above results, it can be seen that the burning speed of solid alcohol fuel is different in combustion vessels with different diameters. Under the condition of the same amount of combustion, the larger the area of the container, that is, the larger the diameter, the more vigorous the burning flame, the higher the heat released during combustion, and the faster the burning speed. The average burning speed of solid alcohol fuel increases with the diameter. reduced by the reduction. Moreover, when the diameter of the combustion disc is small, the amount of residue is relatively high. This is because the fatty alcohol volatilized during combustion does not contact sufficiently with the oxygen in the air, and the combustion is not complete enough, so naturally a little more residue is obtained.
结合以上六组实验所得出的平均燃烧速度,利用非线性回归可以得到燃烧速度与直径之间的定量关系曲线,如图1所示。曲线方程为Y=0.013X1.833,相关系数为0.9932。说明相关性很好,其中Y表示燃烧速度,单位为g/s,X表示为容器的直径,单位为cm。Combined with the average burning velocity obtained from the above six groups of experiments, the quantitative relationship curve between burning velocity and diameter can be obtained by using nonlinear regression, as shown in Figure 1. The curve equation is Y=0.013X 1.833 and the correlation coefficient is 0.9932. It shows that the correlation is very good, where Y represents the burning speed in g/s, and X represents the diameter of the container in cm.
该方程说明,燃烧速度与燃烧容器的面积不呈线性关系。在相同实验条件下,固体醇燃料在不同的燃烧容器中的燃烧速度是不一样的。从能量传递角度来看,燃烧面积过大,能量损失就越大,所以要根据被加热的容器底面积来合理地确定燃烧容器的尺寸。这种燃烧速度与直径之间的定量关系揭示了燃烧的特性。由回归曲线还可知道,固体醇燃料在各个不同面积的燃烧容器中燃烧时的平均燃烧速度,同时还可以计算出,不同时间下固体醇燃料的消耗量。This equation shows that the burning rate is not linearly related to the area of the burning vessel. Under the same experimental conditions, the burning speed of solid alcohol fuel in different combustion containers is different. From the perspective of energy transfer, the larger the combustion area, the greater the energy loss, so the size of the combustion container should be reasonably determined according to the bottom area of the heated container. This quantitative relationship between burning velocity and diameter reveals the nature of the combustion. It can also be known from the regression curve that the average burning speed of the solid alcohol fuel when it burns in combustion containers with different areas can also be calculated at the same time, the consumption of the solid alcohol fuel at different times.
3、固体醇燃料的水加热实验3. Water heating experiment of solid alcohol fuel
实验方法与燃烧实验类似,把400g冷水架在装有13.8克固体醇燃料的燃烧盘之上,点燃后,定时记下燃烧时间与水的温度,通过这些数据即可得出固体醇燃料加热水实验时水温升高与燃烧时间的关系。其中400g水正是野外作业时煮一袋方便面所需要的水量。The experimental method is similar to that of the combustion experiment. Put 400g of cold water on a burning plate containing 13.8 grams of solid alcohol fuel. After igniting it, record the burning time and temperature of the water regularly. From these data, you can get that the solid alcohol fuel heats water. The relationship between water temperature rise and burning time during the experiment. Among them, 400g of water is exactly the amount of water needed to cook a bag of instant noodles when working in the field.
在达到沸腾以后,能持续燃烧至少3分钟,满足了野外作业的使用要求。After boiling, it can continue to burn for at least 3 minutes, which meets the requirements for field operations.
类似方法用乌洛托品军用固体燃料进行烧水试验。结果显示,有燃烧容器时,燃烧速度明显下降,火力较小,在环境温度较冷的情况下,很难将水烧开;无燃烧容器的乌洛托品在达到沸腾以后,还能持续燃烧3分钟以上,满足了野外作业的使用要求。实验过程观察到乌洛托品军用固体燃料从点火到整个燃烧需要40秒,不易点燃,容易熄灭。In a similar way, the water heating test was carried out with urotropine military solid fuel. The results show that when there is a burning container, the burning speed drops obviously, the firepower is small, and it is difficult to boil water when the ambient temperature is relatively cold; the urotropine without a burning container can continue to burn after reaching boiling More than 3 minutes, which meets the use requirements of field operations. During the experiment, it was observed that the military solid fuel of urotropine took 40 seconds from ignition to complete combustion, and it was not easy to ignite, but easy to extinguish.
该实验说明燃烧条件下,环境的中氧气的浓度以及氧气的传递速度十分重要,而固体醇燃料在相同条件下燃烧性能就更好,即使在稍加缺氧的条件下,也能充分燃烧,与乌洛托品军用固体燃料相比,更能适应高原地区。This experiment shows that under the combustion conditions, the concentration of oxygen in the environment and the transfer rate of oxygen are very important, and the combustion performance of solid alcohol fuel is better under the same conditions, even under the condition of a little oxygen deficiency, it can fully burn, Compared with urotropine military solid fuel, it is more adaptable to plateau areas.
另外,从燃烧的实验还可以看到乌洛托品固体燃料燃烧时,因氮氧化合物等有毒、刺鼻气味气体的排放,严重污染了环境,特别在室内或帐篷中燃烧时,对人体的危害很大。在这两种条件下燃烧,最终结果都可以看到,被加热容器的加热面上残留大量的煤烟黑灰,很难清除,给重复使用带来不便,因而降低了固体燃料便捷性的特点。In addition, it can also be seen from the combustion experiment that when the solid fuel of urotropine is burned, the environment is seriously polluted due to the emission of toxic and pungent odor gases such as nitrogen oxides, especially when it is burned indoors or in a tent, it is harmful to the human body. The danger is great. Burning under these two conditions, the final result can be seen that a large amount of soot and black ash remains on the heating surface of the heated container, which is difficult to remove and brings inconvenience to repeated use, thus reducing the convenience of solid fuels. .
4、固体醇燃料的贮存实验4. Storage experiment of solid alcohol fuel
为了考察固体醇燃料的贮存条件,在高温下对固体醇燃料进行反复的水浴加热实验,通过对现象的仔细观察,从而得到贮存固体醇燃料的温度极限。In order to investigate the storage conditions of solid alcohol fuel, repeated water bath heating experiments were carried out on solid alcohol fuel at high temperature. Through careful observation of the phenomenon, the temperature limit of solid alcohol fuel storage was obtained.
贮存实验的实验方法与熔点测定类似,具体操作步骤如下:The experimental method of the storage experiment is similar to that of the melting point determination, and the specific operation steps are as follows:
①将现做的固体醇燃料直接在三口瓶中固化,待固化完全后,设定恒温水浴的温度为44℃,将三口瓶固定于水浴中加热。① Solidify the ready-made solid alcohol fuel directly in the three-necked bottle. After the solidification is complete, set the temperature of the constant temperature water bath to 44°C, and fix the three-necked bottle in the water bath to heat.
②一开始每隔1h,进行一次升温,每次升温幅度为2℃,然后保持1h,仔细观察三口瓶,样品表面干燥无水分,也无异常现象发生。②At the beginning, the temperature was raised every 1 hour, each time the temperature was increased by 2°C, and then kept for 1 hour, and the three-necked bottle was carefully observed. The surface of the sample was dry and free of moisture, and no abnormal phenomenon occurred.
③继续升高温度,当水浴温度达到48℃时,每隔2h,进行一次升温,每次升温幅度为1℃,保持2h,仔细观察三口瓶中现象。当温度为51℃时,三口瓶中现象如表6所示,在此温度下仍然保持着相对稳定的状态。③Continue to increase the temperature. When the temperature of the water bath reaches 48°C, raise the temperature every 2 hours, each time the temperature rises by 1°C, keep for 2 hours, and carefully observe the phenomenon in the three-necked bottle. When the temperature is 51°C, the phenomenon in the three-neck flask is shown in Table 6, and it still maintains a relatively stable state at this temperature.
④当温度升至52℃时,保持1h后,三口瓶中样品表面已渗出少许液体,瓶壁也出现液滴,此时将三口瓶取出,在室温冷却后仍有液体存在。④ When the temperature rises to 52°C, after keeping for 1 hour, a little liquid has seeped out from the surface of the sample in the three-necked bottle, and droplets also appear on the wall of the bottle. At this time, the three-necked bottle is taken out, and there is still liquid after cooling at room temperature.
⑤由此可知,本实验研制的固体醇燃料贮存条件的温度极限值为51℃,若环境温度高于51℃,固体醇燃料将可能受高温影响而使被包裹在高分子凝胶中的液体醇渗出,从而导致固体醇燃料质量下降。⑤It can be seen that the temperature limit of the storage conditions of the solid alcohol fuel developed in this experiment is 51°C. If the ambient temperature is higher than 51°C, the solid alcohol fuel may be affected by the high temperature and the liquid wrapped in the polymer gel may Alcohol bleeds, resulting in poor solid alcohol fuel quality.
表6 温度为51℃时贮存实验现象Table 6 Storage experiment phenomenon when the temperature is 51°C
由表6可知,加热半小时后,固体醇燃料在与玻璃壁面接触的部位上渗出极少量的液膜,这是由于产品原料中含有一定量的水分,而水不是亲油基团,经高温加热,壁面处的水分易从固体醇燃料中渗出。经具体试验可知,重新冷却后固体醇燃料仍然可以恢复到原来的状态,因此对产品的质量影响很少。在加热一小时后,固体醇燃料表面干燥,无液滴;再经过一小时,固体醇燃料表面依然保持干燥。这表明固体醇燃料在该温度下贮存状况良好,经一定包装后便可在该温度下长期贮存,这是因为凝胶状态的固体燃料中的凝胶成分是通过酸碱的皂化反应形成的硬脂酸盐,成份极为稳定,不会随时间而变化,只要在适当的贮存温度下,可以保存三年。As can be seen from Table 6, after heating for half an hour, the solid alcohol fuel oozes a very small amount of liquid film on the part in contact with the glass wall. When heated at high temperature, the moisture on the wall is easy to seep out from the solid alcohol fuel. It can be seen from specific tests that the solid alcohol fuel can still return to its original state after recooling, so it has little impact on the quality of the product. After heating for one hour, the surface of the solid alcohol fuel was dry without droplets; after another hour, the surface of the solid alcohol fuel remained dry. This shows that the solid alcohol fuel is in a good storage condition at this temperature, and can be stored at this temperature for a long time after a certain package. This is because the gel component in the solid fuel in the gel state is formed by the saponification reaction of acid and alkali. Fatty acid salt, the composition is extremely stable and will not change with time, as long as it is stored at an appropriate storage temperature, it can be stored for three years.
继续调节温度,通过多次反复实验可知固体醇燃料的贮存温度应在极限温度51℃以下。而相对对照品1贮存温度极限为49℃,超过该极限,则不能保持良好的物理特性。通常固体醇燃料在常温下储藏即可,但在特殊情况如沙漠环境、炎热环境下,本发明固体醇燃料仍然具有良好的性能指标,因此,本发明产品保质时间长,便于长期储备和长途运输,不仅适合于酒店餐饮行业,而且还适合于旅游、野外作业及部队野营训练。Continue to adjust the temperature. Through repeated experiments, it can be known that the storage temperature of solid alcohol fuel should be below the limit temperature of 51°C. However, the storage temperature limit of the reference product 1 is 49° C., and if it exceeds this limit, good physical properties cannot be maintained. Generally, the solid alcohol fuel can be stored at normal temperature, but in special circumstances such as desert environment and hot environment, the solid alcohol fuel of the present invention still has good performance indicators. Therefore, the product of the present invention has a long shelf life and is convenient for long-term storage and long-distance transportation. , not only suitable for the hotel and catering industry, but also suitable for tourism, field work and army camping training.
5、固体醇燃料的真空燃烧实验5. Vacuum combustion experiment of solid alcohol fuel
该实验用于验证本发明产品在缺氧的环境下燃烧状态。This experiment is used to verify the combustion state of the product of the present invention in an oxygen-deficient environment.
本实验是在真空干燥箱中进行,通过充气阀和真空泵来调节真空干燥箱中的空气绝对量,以模拟固体燃料在高原气候下燃烧时的真实自然环境。This experiment is carried out in a vacuum drying oven, and the absolute amount of air in the vacuum drying oven is adjusted by an air valve and a vacuum pump to simulate the real natural environment of solid fuel burning in a plateau climate.
①称取1.57g的固体醇燃料,在直径为2.024cm的燃烧盘(直径最小的燃烧盘)中点燃,待燃烧稳定后放入真空干燥箱中,关紧干燥箱,使整个干燥箱内空气含量一定,不随外界环境变化;① Weigh 1.57g of solid alcohol fuel, ignite it in a combustion disc (the smallest diameter combustion disc) with a diameter of 2.024cm, put it into a vacuum drying oven after the combustion is stable, and close the drying oven tightly so that the air content in the entire drying oven Definitely, not changing with the external environment;
②将真空泵的电源接通,此时真空干燥箱中空气的绝对量发生变化,从而真空表的读数也发生变化,当空气绝对量逐渐减少时,真空表的读数不断增大,调节充气阀,使真空度以稳定的速度增加,样品的燃烧过程稳定,便于观察现象和记录数据;② Turn on the power of the vacuum pump. At this time, the absolute amount of air in the vacuum drying box changes, so the reading of the vacuum gauge also changes. When the absolute amount of air gradually decreases, the reading of the vacuum gauge continues to increase. Adjust the inflation valve. Make the vacuum degree increase at a stable speed, the combustion process of the sample is stable, and it is convenient to observe the phenomenon and record the data;
③仔细观察样品的燃烧现象,同时注意真空表读数的变化,当样品在某一真空度下熄灭时,记下此时的真空度,即为所得实验数据;③ Carefully observe the burning phenomenon of the sample, and pay attention to the change of the reading of the vacuum gauge at the same time. When the sample is extinguished under a certain vacuum degree, record the vacuum degree at this time, which is the obtained experimental data;
④为保证实验数据的可靠性,重复实验3次,取其平均值;④ In order to ensure the reliability of the experimental data, the experiment was repeated 3 times and the average value was taken;
同样,分别称取1.57g的对照品1,1.60g的对照品2乌洛托品固体燃料在相同条件下进行平行实验。由于乌洛托品在燃烧盘中燃烧极不充分,故对乌洛托品不采用燃烧盘,直接在玻璃皿中点燃,待燃烧稳定后,放入干燥箱中。Similarly, 1.57g of the reference substance 1 and 1.60g of the
固体醇燃料与对照品的真空燃烧对比实验具体现象如表7所示:The concrete phenomenon of the vacuum combustion contrast experiment of solid alcohol fuel and reference substance is as shown in table 7:
表7 真空燃烧实验记录表Table 7 Vacuum combustion experiment record table
通过观察可知,固体醇燃料一点即燃,放入真空干燥箱,接通真空泵电源,起初火焰很弱,待真空干燥箱的空气含量稳定后,燃烧稳定,火焰旺盛,实验进行到后期时,火焰又逐渐减弱,直至熄灭;对照品1的主要燃料也是酒精,燃烧时与本发明的固体醇燃料燃烧现象基本相同;对照品2乌洛托品极不易点燃,需要先点燃,待火焰稳定后再放入真空干燥箱,然后接通真空泵电源,从而初时火焰就很大,待真空干燥箱的空气含量稳定后,燃烧也趋于稳定,火焰旺盛,实验进行到后期时,火焰开始逐渐减弱,直至熄灭,It can be seen from observation that the solid alcohol fuel burns immediately at one point, put it into the vacuum drying box, and turn on the power of the vacuum pump. At first, the flame is very weak. After the air content in the vacuum drying box is stable, the combustion is stable and the flame is strong. Gradually weaken again until it goes out; the main fuel of reference substance 1 is also alcohol, and it is basically the same as the combustion phenomenon of solid alcohol fuel of the present invention during combustion; Put it into the vacuum drying box, and then turn on the power of the vacuum pump, so that the flame is very large at the beginning. After the air content in the vacuum drying box is stable, the combustion also tends to be stable, and the flame is strong. When the experiment progresses to the later stage, the flame gradually weakens until off,
由真空燃烧实验可得出固体醇燃料和对照品在缺氧时的不同燃烧性状,根据实验结果所得的真空度数值,再结合真空度与海拔高度的换算关系,即每升高12米,大气压减少1mmHg,因此通过简单计算,就可得出在高原缺氧条件下燃料可燃时的海拔高度的最大值。From the vacuum combustion experiment, the different combustion properties of the solid alcohol fuel and the reference substance in the absence of oxygen can be obtained. According to the vacuum degree value obtained from the experimental results, combined with the conversion relationship between the vacuum degree and the altitude, that is, every 12 meters rises, the atmospheric pressure Reduce 1mmHg, so by simple calculation, you can get the maximum altitude when the fuel is combustible under the condition of plateau anoxic.
(一)固体醇燃料(1) Solid alcohol fuel
对于固体醇燃料,火焰熄灭时真空度为0.07Mpa。For solid alcohol fuel, the vacuum degree is 0.07Mpa when the flame is extinguished.
由于1mmHg=133Pa=0·000133MPa,Since 1mmHg=133Pa=0·000133MPa,
可换算为缺氧环境下的压力值P1=0.07/0.000133=526.32mmHgIt can be converted into the pressure value under hypoxic environment P 1 =0.07/0.000133=526.32mmHg
则在该压力下的海拔高度值为H1=526·32×12=6315.84mThen the altitude value under this pressure is H 1 =526·32×12=6315.84m
从而得出结论:在高原缺氧环境下,固体醇燃料可以燃烧的海拔高度的最大值约为6300m。It is thus concluded that the maximum altitude at which solid alcohol fuel can be burned is about 6300m in the plateau anoxic environment.
(二)对照品(2) Reference substance
对于两种对照品,火焰熄灭时真空度均为0.06Mpa。For the two reference substances, the vacuum degree is 0.06Mpa when the flame is extinguished.
由于1mmHg=133Pa=0.000133MPa,Since 1mmHg=133Pa=0.000133MPa,
可换算为缺氧环境下的压力值P2=0.06/0.000133=451.13mmHgIt can be converted into the pressure value under hypoxic environment P 2 =0.06/0.000133=451.13mmHg
则该压力下的海拔高度值为H2=451.13×12=5413.56mThen the altitude value under this pressure is H 2 =451.13×12=5413.56m
从而得出结论:在高原缺氧环境下,对照品燃料可以燃烧的海拔高度的最大值约为5400m。It is thus concluded that the maximum altitude at which the reference fuel can be burned is about 5400m in the plateau anoxic environment.
通过以上对比实验可以得知,在真空缺氧的条件下,本发明的固体醇燃料具有明显优势,在高原缺氧如此苛刻的环境下,依然能够保持燃烧稳定,火焰旺盛,具有良好的燃烧性能。而对照品则稍有不足,在同样的环境条件下,燃烧火焰不旺,燃烧过程不稳定,燃烧的真空度极限值也较低,其各方面的燃烧性能都不如固体醇燃料。通过计算数据可知,固体醇燃料在海拔6300多米的高原或山地环境中仍然可以燃烧,而对照品则只能在海拔5400米以下的高原或山地环境中使用。显然,本发明固体醇燃料更适合用于高原缺氧地区,具有明显优势,是高原士兵野外训练以及高原山地作战的首选热源,可广泛应用于现代化军需装备。From the above comparative experiments, it can be known that under the condition of vacuum anoxic, the solid alcohol fuel of the present invention has obvious advantages, and it can still maintain stable combustion, strong flame and good combustion performance in such a harsh environment of plateau anoxic . However, the reference substance is slightly insufficient. Under the same environmental conditions, the combustion flame is not strong, the combustion process is unstable, and the vacuum limit value of combustion is also low, and its combustion performance in all aspects is not as good as that of solid alcohol fuel. According to the calculated data, the solid alcohol fuel can still burn in the plateau or mountain environment with an altitude of more than 6300 meters, while the reference product can only be used in the plateau or mountain environment with an altitude of less than 5400 meters. Apparently, the solid alcohol fuel of the present invention is more suitable for use in plateau anoxic regions and has obvious advantages. It is the preferred heat source for plateau soldiers' field training and plateau mountain operations, and can be widely used in modern military equipment.
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| CN104212533A (en) * | 2013-06-05 | 2014-12-17 | 傅苏华 | Making method of sky lantern lift-off fuel |
| CN104593113A (en) * | 2013-10-31 | 2015-05-06 | 孙立 | Method for producing solid fuel from swill-cooked dirty oil |
| CN103555384A (en) * | 2013-11-11 | 2014-02-05 | 夏祖菊 | Solid fuel |
| CN105982814A (en) * | 2015-02-10 | 2016-10-05 | 韩小东 | Moxa-moxibustion smoke discharge system realizing stepless air volume regulation |
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| CN107502025B (en) * | 2016-11-29 | 2019-11-22 | 北京交通大学 | A kind of microcapsule thermosensitive material and its preparation method and application |
| CN108018105A (en) * | 2017-12-13 | 2018-05-11 | 柳州市金升汽车配件有限公司 | A kind of solid fuel and preparation method thereof |
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| CN109536236A (en) * | 2018-11-30 | 2019-03-29 | 乐山师范学院 | Application, solid alcohol and preparation method of the biodiesel in solid alcohol preparation |
| CN110240967A (en) * | 2019-07-03 | 2019-09-17 | 华中农业大学 | A kind of biochar-alcohol solid fuel and preparation method thereof |
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