JP5358351B2 - Biodiesel fuel production equipment - Google Patents

Description

The present invention relates to a production equipment of biodiesel fuel, which is a type of biofuel produced by using biomass.

  Use of fuel to replace fossil fuels for the purpose of countermeasures such as global warming caused by carbon dioxide generated by mass consumption of fossil fuels such as coal and oil, and depletion of fossil fuels Interest in has increased in recent years.

  In particular, interest in biofuel utilization is increasing. Biofuels can be obtained from substances that are photosynthesized from carbon dioxide and water by solar energy, for example, in the life cycle of plants. The carbon dioxide generated by the combustion of the biofuel is the one that was originally present in the atmosphere and is taken into the plant by photosynthesis, so even if it is released into the atmosphere by combustion, It is said to be carbon-neutral fuel without increasing carbon dioxide on the sphere.

  Specifically, as biofuel, biogas (main component is methane) that can be generated by anaerobic decomposition method of biomass, biomass ethanol and oil that can be generated by alcohol fermentation of biomass with microorganisms Examples include biodiesel fuel (BDF) synthesized by reacting a kind.

  Among these, biodiesel fuel (BDF) is a fuel having a fatty acid alkyl ester composition obtained by esterifying triglycerides of biomass such as vegetable oil. Many vegetable oils cannot be used as automobile fuel because they have high kinematic viscosity and flash point. Therefore, triglycerides, which are the main components of fats and oils, are transesterified with an alcohol or the like to obtain a fatty acid alkyl ester, which can be used in which the kinematic viscosity or flash point is lowered.

  In particular, methyl esterified fatty acid methyl ester is common, and is expected as a fuel to replace light oil which is important as a fuel for diesel engines.

  As a technique relating to the production of such biodiesel fuel, a patent application such as the following Patent Document 1 has been filed. As described in claim 1 of Patent Document 1, the invention according to Patent Document 1 is “a step of using an alkali catalyst and transesterifying raw oil with a lower alcohol to produce a fatty acid ester. In the method for producing biodiesel fuel, the reaction mixture obtained by transesterification with the alkali catalyst is neutralized by adding dilute sulfuric acid adjusted with a predetermined amount of water, from the neutralized reaction mixture It includes a step of filtering out sulfate crystals, distilling the filtrate, and separating a glycerin component having a high specific gravity by a specific gravity separation operation.

  However, the biodiesel fuel manufacturing technology using an alkali catalyst as in Patent Document 1 requires a long time for the reaction, and separation of the alkali catalyst used in large quantities (alkali neutralization treatment with dilute sulfuric acid aqueous solution and There are problems such as filtration of precipitates generated at that time and treatment of waste water. Specifically, the reaction took about 1 to 8 hours, and post-treatment such as alkali neutralization and wastewater treatment took about 2 days.

  Therefore, in order to solve such problems, a patent application such as the following Patent Document 2 has been filed. As described in claim 1 of Patent Document 2, the invention according to Patent Document 2 is “by transesterification / esterification reaction of vegetable oil or animal fat and oil with alcohol induced by microwave irradiation. A method for producing biodiesel, wherein the production of fatty acid monoalkyl esters is carried out by transesterification / esterification of vegetable oils, animal fats or free fatty acids with alcohols, and the reaction is carried out with vigorous stirring. Is carried out by microwave heating in the reaction cavity in the presence of a catalyst in / oil / fat / fatty acid and alcohol ".

  The invention according to Patent Document 2 has an effect that the reaction time is remarkably shortened as compared to the biodiesel fuel manufacturing technique using the alkali catalyst as in Patent Document 1 described above.

  However, since the technique described in Patent Document 2 uses a cavity (reaction vessel) in a batch as described in paragraph [0009] of the specification of Patent Document 2, In order to obtain a desired amount of biodiesel fuel, a reaction tank having almost the same volume was required, and the internal volume of the reaction tank tended to increase. Furthermore, as described in [0010], the crude mixture is washed with hot water, and then the pressure of the vacuum pump is completely reduced at 50 ° C. until the water is completely removed, with the help of a vacuum pump. A post-treatment of distillation and drying was necessary. Further, the processing efficiency for the reaction was never good.

JP-A-2005-350630 JP 2007-277374 A

The present invention has been made in order to solve such problems, and in order to obtain a desired amount of biodiesel fuel, the reaction tank can be reduced in size without requiring a reaction tank of almost the same volume. can be of, can achieve an efficient separation of the reactants and the alkaline catalyst, also, an object of the present invention to provide a manufacturing apparatus of a biodiesel fuel processing efficiency can be greatly improved for the reaction .

In order to solve such problems, the present invention provides a reaction tank for reacting oils and fats with alcohol in the presence of a solid alkali catalyst, and a reaction product generated in the reaction tank. A separator for separating the product and unreacted alcohol, reaction in the reaction tank of the fats and alcohols, reaction product generated in the reaction tank and unreacted alcohol The reaction product and unreacted alcohol are separated from each other in order to transfer the reaction product and unreacted alcohol from the reaction vessel to the separator. The present invention provides an apparatus for producing biodiesel fuel, characterized in that a sunphone tube is interposed between the two.

It is also possible to further include a return line for returning the separated unreacted alcohols to the reaction tank or its front side. Furthermore, in order to prevent the solid alkali catalyst in the reaction応槽is inadvertently transferred to the separator side, a filter for filtering process, can also be provided between the reaction vessel and the separator.

  Furthermore, it is possible to separate unreacted alcohols from reaction products in the separator by heating by microwave irradiation. Furthermore, it is possible to separate unreacted alcohols from reaction products in the separator by heating by microwave irradiation.

As described above, since the present invention is for subjecting fats and alcohols to microwave irradiation treatment in the presence of a solid alkali catalyst, the reaction time between the fats and alcohols and alcohols is significantly shortened. is there.
In addition, since the solid alkali catalyst used in the reaction is a solid, it is possible to easily separate liquid reaction products and unreacted alcohols from the solid alkali catalyst by filtration using a filter, a filtration membrane or the like. Therefore, it is not necessary to separately perform a neutralization treatment using an acid. As a result, there is an effect that post-treatment such as separation and drainage of the reaction product generated during neutralization becomes unnecessary.

  Furthermore, since the reaction product produced in the reaction vessel and the unreacted alcohols are continuously separated in the separator, the reaction product in the reaction vessel and the unreacted product are not reacted according to the transfer rate. It becomes possible to control the residence amount of alcohols, and the effect that the volume of the reaction tank can be reduced is produced.

  In addition, after reacting oils and alcohols in the presence of a solid alkali catalyst, they are separated into a mixture of fatty acid alkyl ester (biodiesel fuel) and glycerin and unreacted alcohols in the separator. Since the unreacted alcohols are effectively separated from the mixture of biodiesel fuel, which is the main reaction product of alcohols and alcohols, and glycerin, which is a reaction byproduct, it is necessary to refine biodiesel fuel in the subsequent stage. There is an effect that it is possible to perform more suitably.

  Furthermore, when the separated unreacted alcohols are returned to the reaction tank or the preceding stage for reuse, the alcohols can be used repeatedly. Therefore, there is an effect that continuous supply and reuse of fats and alcohols to the reaction tank are performed more efficiently.

The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as one Embodiment. The schematic front view which shows the part of the reaction tank and separator in the manufacturing apparatus. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment.

  Hereinafter, embodiments of the present invention will be described.

  The biodiesel fuel production apparatus of the present invention, as described above, produces a reaction tank for reacting oils and fats and alcohol by irradiation with microwaves in the presence of a solid alkali catalyst, and the reaction tank. A separator for separating unreacted alcohols from the reaction product, reaction in the reaction tank of the fats and alcohols, reaction product generated in the reaction tank and unreacted The alcohol is separated continuously from each other.

  Here, the reaction product produced in the reaction vessel includes a reaction main product of biodiesel fuel as a target product and a reaction by-product such as glycerin.

  The biodiesel fuel production method of the present invention, as described above, reacts oils and fats and alcohols in the reaction vessel by irradiation with microwaves in the presence of a solid alkali catalyst, and then the reaction vessel. The reaction product and unreacted alcohol produced in the above are separated by a separator, the reaction between the fats and alcohols in the reaction tank, the reaction product produced in the reaction tank and the unreacted alcohol Separation is performed continuously.

  Examples of the fats and oils include safflower oil, tung oil (can be collected from paulownia plant seeds such as cinnamon brasil, arabragi), sunflower oil, cottonseed oil, corn oil, rapeseed oil, soybean oil, sesame oil, olive oil, peanut oil, castor oil, Plant oils such as palm oil, cacao oil, palm oil, oilseed oil (Yatropha), moringa, or animal oils such as fish oil, beef tallow, pig oil, whale oil can be used.

  Among oils and fats, safflower oil, tung oil, sunflower oil, cottonseed oil, corn oil, rapeseed oil, soybean oil, sesame oil, olive oil, peanut oil, castor oil and other vegetable oils or fish oils are liquid at room temperature, while palm oil Vegetable oils and fats such as oil, cacao oil and coconut oil, or animal fats and oils such as beef tallow, pig oil and whale oil are solid at room temperature. In the production of biodiesel fuel, it has the advantage that it can be easily handled at room temperature.

  Furthermore, sunflower oil, rapeseed oil, soybean oil, palm oil, etc. are easy to obtain in large quantities both in the world and in Japan. Furthermore, from the viewpoint of not limiting the use as food, it is possible to use paulownia oil, sunflower oil, cottonseed oil, castor oil, moringa oil and the like that have not been used as food.

  As these fats and oils, unused ones (virgin oil) can be used, and used waste oil recovered after use can also be used. Moreover, about vegetable fats and oils, it is also possible to use the oil collect | recovered as waste utilization from the various seeds which are the raw material of extraction of each oil, and the fruit extractor.

  An alcohol for transesterification is mixed with these fats and oils. The type of alcohol is not particularly limited. For example, methanol, ethanol, propanol or the like can be used. However, from the viewpoint of having an advantage of easily absorbing microwaves, lower alcohols such as methanol and ethanol are used. It is preferable to use methanol.

  The point is that the alcohol for transesterification can be arbitrarily selected as long as the obtained fatty acid alkyl ester satisfies the standards for diesel fuel such as kinematic viscosity, flash point, and cetane number.

  The mixing ratio of such fats and oils and alcohols is also not particularly limited, but the alcohols are preferably about 6 to 24 moles per mole of the fats and oils.

  Furthermore, although fats and oils are reacted in the presence of a solid alkali catalyst in a reaction vessel, the type of the solid alkali catalyst is not particularly limited, and for example, calcium oxide or hydroxide Something like that can be used. Moreover, the property, such as a granular form and a powder form, does not ask | require, the point is that the solid alkali catalyst should just be used.

  The solid alkali catalyst is added to the reaction vessel as it is. For example, a porous support is placed above and below the reaction vessel, and a large number of granular solid alkali catalysts are filled between the upper and lower supports. By doing so, it can be accommodated in the reaction vessel. In that case, as a reaction tank, a cylindrical thing can be used, for example, and it is comprised like a fixed bed type column as a whole. When the reaction vessel is thus formed into a cylindrical shape, the shape of the reaction vessel can be designed more compactly by processing with a plug flow.

  The microwave irradiation time is not particularly limited, but is preferably 5 minutes or less. This is because when the microwave irradiation is performed for a long time, the product may be decomposed or deteriorated. Moreover, although the intensity | strength of the microwave to irradiate can be controlled by the output of an apparatus, an output is not specifically limited, either. For example, a microwave with an output of about 100 to 1500 W can be used, and a microwave with an output of about 100 to 300 W can be used more preferably.

  The frequency of microwaves that can be used practically is determined by the Radio Law (IMS frequency: 933.92 MHz, 2.45 GHz, 5.8 GHz, 24.125 GHz). In the present invention, microwaves of any of these frequencies can be used. More preferably, a frequency of 2.45 GHz can be used from the viewpoint of cost and versatility of the microwave generator.

Further, fats and oils and alcohols are supplied to the reaction vessel and reacted to form a mixture of the reaction main product fatty acid alkyl ester (biodiesel fuel) and the reaction byproduct glycerin, and then the mixture is separated into a separator. It is also possible to separate the unreacted alcohols from the mixture and return them to the reaction tank or the previous stage for reuse.
As a means for separating unreacted alcohols from the reaction product in the separator, distillation means for separating the alcohols having the lowest boiling point using the difference in boiling points of the respective components is mainly employed. As a means for separating such reaction product and unreacted alcohol, means other than distillation can be employed.
Furthermore, it is also possible to perform microwave heating irradiation treatment for performing the distillation.

In this case, the reaction tank and the separator Ki de be arranged vertically, the reaction vessel and the separator are connected via a sub Ifon tube. By connecting via such a siphon tube, the oils and alcohols supplied to the reaction tank are irradiated with microwaves until they reach a position higher than the height of the top of the siphon tube. Fats and oils react with each other to produce biodiesel fuel as a main reaction product and glycerin as a reaction by-product. Next, when a mixture of oils and fats and alcohols is further supplied and the total volume of the liquid in the reaction vessel exceeds the top of the Sanphon tube, the mixture in the reaction vessel is separated through the siphon tube. Will be transferred to.

  Hereinafter, more specific embodiments of the present invention will be described with reference to the drawings.

(Embodiment 1)
FIG. 1: shows the schematic block diagram of the manufacturing apparatus of the biodiesel fuel as one Embodiment. The biodiesel fuel production apparatus of the present embodiment includes an oil and fat storage tank 1 as an undiluted solution, an alcohol storage tank 2, a mixer 3, a reaction tank 4, a separator 5, and a recovery tank 6. Configured.

  The fats and oils storage tank 1 is a tank for storing fats and oils that are stock solutions that are raw materials for producing biodiesel fuel. As the fats and oils, for example, waste oil such as rapeseed oil (salad oil) that has been used in homes and facilities is used.

  The alcohol storage tank 2 is a tank for storing alcohol for reacting with the fats and oils. As the alcohol, for example, methanol is used.

  The mixer 3 is for mixing the fats and oils supplied from the fats and oils storage tank 1 and the alcohols supplied from the alcohols storage tank 2. As the mixer 3, for example, a simple mixer such as a line mixer is used.

  The reaction tank 4 is a tank for performing a transesterification reaction between fats and oils and alcohols. The reaction tank 4 is supplied with a mixture of fats and oils mixed with the mixer 3 and alcohols. Since the liquid mixture previously mixed in the mixer 3 is supplied to the reaction tank 4, it is not necessary to provide a stirring means such as a stirrer in the reaction tank 4. Although not shown in FIG. 1, the reaction tank 4 contains a solid alkali catalyst. As the solid alkali catalyst, for example, granular or powdery calcium hydroxide is used.

  Such a granular or powdery solid alkali catalyst is added and accommodated in the reaction vessel as it is, but is not limited thereto, and for example, a porous support is arranged above and below the reaction vessel, It is also possible to accommodate a large number of granular solid alkali catalysts between the supports in the reaction vessel.

  The separator 5 is obtained from a mixture of fatty acid alkyl ester (biodiesel fuel), which is a main reaction product produced by the reaction between fats and oils supplied to the reaction tank 4, and glycerin, a reaction byproduct. It is for distilling and separating the alcohol of reaction. In FIG. 1, the reaction tank 4 and the separator 5 are illustrated as being disposed at the front stage and the rear stage, but in actuality, they are disposed in a vertical positional relationship as illustrated in FIG. 2. That is, the reaction tank 4 is arranged on the upper side and the separator 5 is arranged on the lower side.

  The reaction vessel 4 and the separator 5 are housed in a casing 7 as shown in FIG. 1, and a microwave oscillator 8 is provided in the casing 7, so that the microwave is fed into the reaction vessel 4 and the separator 5. It is comprised so that it may irradiate in. The casing 7 is preferably made of a metal having a high microwave reflectivity, as indicated by an arrow line in FIG. 1. The reaction tank 4 and the separator 5 are the reaction tank 4 and the separator 5. In order to make the microwave reach the liquid mixture passing through the inside, it is preferably made of glass which is a material having a high microwave transmittance. Each material of the casing 7, the reaction tank 4, the separator 5 and the like is required to satisfy the microwave absorption characteristics, and the material and shape are not limited.

  The unreacted alcohols separated by the separator 5 are returned from the separator 5 to the mixer 3 disposed on the upstream side of the reaction tank 4 through the return line 9. In the middle portion of the return line 9, a condenser 10 is provided, and the alcohol to be returned is returned to the mixer 3 in a state of being condensed and liquefied by the condenser 10.

The reaction tank 4 and the separator 5 are connected via the cylinder part 11 as shown in FIG. In addition, a siphon tube 12 as a connecting portion is connected to the bottom 4 a of the reaction vessel 4. More specifically, the inlet portion 12a of the siphon tube 12 is connected to the bottom portion 4a of the reaction vessel 4, and the outlet portion 12b of the siphon tube 12 protrudes into the separator 5 through the cylindrical portion 11. Is provided. A filter 16 is provided at the boundary between the bottom 4 a of the reaction tank 4 and the inlet 12 a of the siphon tube 12.
The height of the top portion 12c of the siphon tube 12 is set so as to be within the range of the height of the reaction vessel 4, and the mixed liquid of oils and fats supplied to the reaction vessel 4 is added to the siphon tube. When the liquid is stored in the reaction tank 4 at a depth that is higher than the height of the top portion 12c of the twelve, the mixed liquid in the reaction tank 4 passes through the filter 16 to the inlet of the siphon tube 12. It is configured to be supplied to the separator 5 from the outlet portion 12b via the portion 12a and the top portion 12c.

  Furthermore, the reaction tank 4 is provided with a connecting pipe 13 that serves as an inlet portion for the mixed liquid of the oils and fats. In addition, the separator 5 is provided with a connecting pipe 14 serving as an outlet part to the return line 9 and a connecting pipe 15 serving as an outlet part to the recovery tank 6.

  The recovery tank 6 is a tank for recovering a mixture of the produced biodiesel fuel, which is the main reaction product, and glycerin, which is a reaction byproduct. Although not shown in FIG. 1, the biodiesel fuel can be purified by easily separating the biodiesel fuel and glycerin by a general technique such as precipitation separation.

  Next, an embodiment of a method for producing biodiesel fuel using the apparatus as described above will be described.

  First, the fats and oils, which are stock solutions for producing biodiesel fuel, are supplied from the fats and oils storage tank 1 to the mixer 3, and the alcohols are supplied from the alcohols storage tank 2 to the mixer 3. Although these oils and fats and alcohols are not shown in FIG. 1, they are continuously supplied by, for example, a pump.

  Then, fats and oils and alcohols are mixed by the mixer 3. The mixed liquid of the mixed fats and alcohols is supplied to the reaction tank 4 and stored in the reaction tank 4. Thus, in the process in which the liquid mixture is stored in the reaction vessel 4, the microwave oscillator 8 provided in the casing 7 is operated to perform the irradiation process with microwaves. By operating the microwave oscillator 8 in this manner, the mixed solution is irradiated with microwaves within the time that the mixed solution exists in contact with the solid alkali catalyst in the reaction vessel 4.

  Thus, the fats and alcohols and alcohol which were supplied to the reaction tank 4 in the state by which the irradiation process by the microwave was performed react in this reaction tank 4, and the alcohol ester of fats and oils is obtained. In this embodiment, rapeseed oil, which is vegetable oil, is used as the fat and oil, and methanol is used as the alcohol. Therefore, rapeseed oil fatty acid methyl ester is produced.

  In this case, since the irradiation treatment with microwaves is performed, the rapeseed oil and methanol in the reaction tank 4 react in a very short time, and the methyl ester of triglyceride (fatty acid), which is the main component of the rapeseed oil, is immediately generated. The Rukoto.

  When the mixed liquid is stored up to a predetermined depth in the reaction tank 4, that is, the mixed liquid is stored in the reaction tank 4 to a depth that is higher than the height of the top portion 12 c of the siphon tube 12. Then, the mixed liquid in the reaction tank 4 is supplied to the separator 5 from the outlet portion 12b through the filter 16 through the inlet portion 12a and the top portion 12c of the siphon tube 12. In this case, since a filter 16 is provided at the boundary between the bottom 4a of the reaction tank 4 and the inlet 12a of the siphon tube 12, the solid alkaline catalyst present in the reaction tank 4 is accompanied by the mixed liquid. There is no inadvertent transition to siphon tubes. In addition, the transferred liquid mixture is obtained by reacting methyl ester of triglyceride (fatty acid) which is a main reaction product obtained by the reaction of rapeseed oil and methanol as described above, unreacted methanol, and glycerin as a reaction byproduct. Consists of.

  In this way, the mixed solution is supplied to the separator 5 as described above, and unreacted methanol is distilled and separated from the fatty acid methyl ester. In this case, the separator 5 is irradiated with microwaves. By performing this treatment, methanol absorbs microwaves and generates heat rapidly, and methanol distillation and separation of methanol and fatty acid methyl ester are performed in a very short time.

  In this case, since both the separator 5 and the reaction tank 4 are accommodated in the casing 7, and the microwave oscillator 8 is provided in the casing 7, the liquid mixture of fats and oils and alcohols as described above. Is stored in the reaction tank 4, the microwave energy irradiated by the operation of the microwave oscillator 8 is used to promote the reaction between the oils and fats in the reaction tank 4, As described above, the mixed liquid is stored in the reaction tank 4 to a predetermined depth, and the mixed liquid in the reaction tank 4 is supplied from the outlet part 12b to the separator 5 via the inlet part 12a and the top part 12c of the siphon tube 12. After that, the microwave energy is used for distillation of alcohols in the separator 5.

  That is, the energy of the microwave irradiated by the operation of the microwave oscillator 8 provided in the casing 7 causes the reaction between the fats and oils and the alcohols in the reaction tank 4 and the distillation of the alcohols in the separator 5. Therefore, the microwave processing is effectively used.

  The methanol separated by distillation is returned from the separator 5 to the mixer 3 on the upstream side of the reaction tank 4 through the return line 9. In this case, since the condenser 10 is provided in the middle portion of the return line 9, the alcohol to be returned is efficiently returned to the mixer 3 while being condensed in the condenser 10. It will be. Thereby, the returned methanol is mixed with the vegetable oil as the raw material supplied from the oil and fat storage tank 1 and reused.

  On the other hand, the fatty acid methyl ester which is a product separated from methanol by the separator 5 is supplied to the recovery tank 6 and used as biodiesel fuel.

  In the present embodiment, as described above, vegetable oil and methanol, which are stock solutions that are raw materials for producing biodiesel fuel, are continuously supplied from the stock solution tank 1 to the reaction tank 4 by a pump. By activating the oscillator 8 and performing irradiation treatment with microwaves, the fatty acid in the vegetable oil reacts with methanol in a very short time to produce a fatty acid methyl ester, which reacts with the fatty acid methyl ester as the main reaction product. A mixture of glycerin, which is a by-product, and unreacted methanol are supplied to the separator 5, and distillation is performed in the separator 5 to separate unreacted methanol. Subsequently, the separated unreacted methanol is removed. After returning to the upstream side of the reaction tank 4 and reusing it, the fatty acid methyl ester and glycerin separated by the separator 5 are supplied to the recovery tank 6 for purification, Since subjected to diesel fuel, along with allowing continuous regeneration of methanol enables continuous production of biodiesel fuels.

  In addition, since continuous production of biodiesel fuel as described above is possible, the reaction tank does not increase in size as in a conventional biodiesel fuel production apparatus equipped with a batch-type reaction tank. Therefore, it is possible to provide a small device.

(Embodiment 2)
FIG. 3: shows the schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. The biodiesel fuel production apparatus of the present embodiment is different from the first embodiment in which the mixer 3 is not provided and the mixer 3 is provided in this respect.

  In this embodiment, since the mixer 3 is not provided, the fats and oils are directly supplied from the fats and oils storage tank 1 to the reaction tank 4, and the alcohols are directly supplied from the alcohols storage tank 2 to the reaction tank 4. It will be.

  Moreover, since the mixer 3 is not provided in this embodiment, fats and oils and alcohol are mixed in the reaction tank 4 while stirring. As the stirring means, for example, any stirring means such as a magnetic stirrer or a stirrer can be employed.

  Furthermore, since the mixer 3 is not provided, the unreacted methanol distilled from the separator 5 and separated from the product fatty acid methyl ester is returned to the reaction tank 4 and reused. .

  Also in this embodiment, the casing 7 is made of metal as in the first embodiment, and the reaction tank 4 and the separator 5 are made of glass. Since the oil and fat storage tank 1, the alcohol storage tank 2, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the first embodiment, the description thereof is omitted. .

  Also in this embodiment, vegetable oil and methanol, which are raw materials for biodiesel fuel, are continuously supplied to the reaction tank 4, and irradiation with microwaves is performed in the reaction tank 4 to produce fatty acid methyl esters in a very short time. The unreacted methanol separated from the fatty acid methyl ester is returned and reused, and the fatty acid methyl ester separated by the separator 5 is supplied to the recovery tank 6 and biodiesel. Since the fuel is used as a fuel, the methanol can be continuously regenerated and the biodiesel fuel can be continuously produced. In addition, since a continuous biodiesel fuel can be manufactured, a small device can be provided.

(Embodiment 3)
FIG. 4: shows the schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. In the biodiesel fuel production apparatus of the present embodiment, the casings 7a and 7b for accommodating the reaction tank 4 and the separator 5 are separately provided, and accordingly, the microwave oscillators 8a and 8b are respectively connected to the casings 7a and 7b. Is provided. This is different from the first and second embodiments in which the reaction tank 4 and the separator 5 are accommodated in one casing 7.

  Therefore, in this embodiment, microwave irradiation for promoting the reaction between fats and oils and alcohols in the reaction tank 4 and microwave irradiation for promoting distillation of alcohols in the separator 5 are performed. Are separately performed in the respective casings 7a and 7b by the respective microwave oscillators 8a and 8b.

  In this embodiment, since the microwave irradiation is performed on the reaction tank 4 and the separator 5 in the separate casings 7a and 7b by the separate microwave oscillators 8a and 8b as described above, the fats and oils and alcohol in the reaction tank 4 are used. Irradiation with microwaves can be appropriately performed according to the conditions necessary for the reaction with the alcohol and the conditions necessary for the distillation of the alcohols in the separator 5.

  Since the oil and fat storage tank 1, the alcohol storage tank 2, the mixer 3, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the first embodiment, the description thereof is omitted. Is omitted.

  Also in the present embodiment, vegetable oil and methanol, which are raw materials for biodiesel fuel, are continuously supplied to the reaction tank 4, and irradiation with microwaves is performed in the reaction tank 4 to produce fatty acid methyl esters in a very short time. Distillation is performed in the separator 5, unreacted methanol separated from the fatty acid methyl ester is returned and reused, and the fatty acid methyl ester separated in the separator 5 is supplied to the recovery tank 6 to be biodiesel fuel. Therefore, the methanol can be continuously regenerated and the biodiesel fuel can be continuously produced. In addition, since a continuous biodiesel fuel can be manufactured, a small device can be provided.

(Embodiment 4)
FIG. 5: shows the schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. Also in the biodiesel fuel production apparatus of the present embodiment, as in the third embodiment, casings 7a and 7b for accommodating the reaction tank 4 and the separator 5 are separately provided, and the microwave oscillator 8a, 8b is provided in each casing 7a, 7b.

  Moreover, in this embodiment, the mixer 3 is not comprised like the said Embodiment 2, and fats and oils are directly supplied to the reaction tank 4 from the fats and oils storage tank 1, and alcohol is directly sent from the alcohols storage tank 2. It will be supplied to the reaction tank 4.

  Since the oil and fat storage tank 1, the alcohol storage tank 2, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the second embodiment, the description thereof is omitted. .

  Also in the present embodiment, vegetable oil and methanol, which are raw materials for biodiesel fuel, are continuously supplied to the reaction tank 4, and irradiation with microwaves is performed in the reaction tank 4 to produce fatty acid methyl esters in a very short time. Distillation is performed in the separator 5, unreacted methanol separated from the fatty acid methyl ester is returned and reused, and the fatty acid methyl ester separated in the separator 5 is supplied to the recovery tank 6 to be biodiesel fuel. Therefore, the methanol can be continuously regenerated and the biodiesel fuel can be continuously produced. In addition, since a continuous biodiesel fuel can be manufactured, a small device can be provided.

(Embodiment 5)
FIG. 6 shows a schematic block diagram of an apparatus for producing biodiesel fuel as another embodiment. In the biodiesel fuel production apparatus of this embodiment, only the reaction tank 4 is accommodated in the casing 7, and the separator 5 is not accommodated in the casing 7. This is different from the first embodiment in which both the reaction tank 4 and the separator 5 are accommodated in the casing 7.

  Since only the reaction tank 4 is accommodated in the casing 7, microwave irradiation by the operation of the microwave oscillator 8 is performed only on the reaction tank 4, and not on the separator 5.

  Since the oil and fat storage tank 1, the alcohol storage tank 2, the mixer 3, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the first embodiment, the description thereof is omitted. Is omitted.

(Embodiment 6)
FIG. 7: shows the schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. In the biodiesel fuel production apparatus of the present embodiment, only the reaction tank 4 is stored in the casing 7 as in the fifth embodiment, and the separator 5 is not stored in the casing 7. Moreover, the mixer 3 is not comprised similarly to the said Embodiment 2, and fats and oils are directly supplied to the reaction tank 4 from the fats and oils storage tank 1, and alcohol from the alcohol storage tank 2 to the reaction tank 4 directly. Will be supplied.

  Since the oil and fat storage tank 1, the alcohol storage tank 2, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the second embodiment, the description thereof is omitted. .

(Embodiment 7)
FIG. 8: shows the schematic block diagram of the manufacturing apparatus of the biodiesel fuel as other embodiment. In the biodiesel fuel production apparatus of the present embodiment, the mixer 3, the reaction tank 4, and the separator 5 are housed in the casing 7, and the microwave irradiation by the operation of the microwave oscillator 8 is performed by the mixer 3, It is comprised so that it may be made with respect to the reaction tank 4 and the separator 5. FIG.

  Since the oil and fat storage tank 1, the alcohol storage tank 2, the mixer 3, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the first embodiment, the description thereof is omitted. Is omitted.

(Embodiment 8)
FIG. 9 shows a schematic block diagram of an apparatus for producing biodiesel fuel as another embodiment. In the biodiesel fuel production apparatus of this embodiment, the mixer 3 and the reaction tank 4 are housed in one casing 7a, and the separator 5 is housed in another casing 7b.

  Therefore, in this embodiment, the microwave irradiation by the operation of the microwave oscillator 8a provided in one casing 7a is performed on the mixer 3 and the reaction tank 4, and the microwave oscillator provided in the other casing 7b. The microwave irradiation by the operation of 8b is configured to be performed on the separator 5.

  Since the oil and fat storage tank 1, the alcohol storage tank 2, the mixer 3, the reaction tank 4, the separator 5, and the recovery tank 6 are provided in common with those of the first embodiment, the description thereof is omitted. Is omitted.

(Other embodiments)
In addition, in each said embodiment, although the fats and oils storage tank 1 which stores the fats and oils as stock solution, and the alcohol storage tank 2 which stores alcohols were comprised, such fats and oils storage tank 1 and alcohols were comprised. Providing the storage tank 2 is not an essential condition for the present invention. For example, fats and oils such as waste oil discharged from a factory can be directly supplied to the mixer 3 or the reaction tank 4.

  In each of the above embodiments, after supplying the fats and alcohols to the reaction tank, the alcohols are distilled in a distiller and returned to the reaction tank or the previous stage for reuse. It is not an essential condition for the present invention to return a class for reuse. In short, it is only necessary to effectively separate unreacted alcohols from a mixture of biodiesel fuel, glycerin and unreacted alcohols.

Furthermore, the shape of the reaction tank 4 in FIG. 2 of the above embodiment is not limited to that shown in FIG. It is sufficient that the solid alkali catalyst can be provided inside, and it is possible to use a spherical shape, a column shape, and other various shapes. Further, the shape and material of the filter 16 installed in the reaction tank 4 are not limited. In short, it is sufficient that the solid alkali catalyst has an opening that does not pass through.
Further, in each of the above embodiments, the reaction tank 4 and the separator 5 are accommodated in the casings 7, 7a, 7b, and by the operation of the microwave oscillators 8, 8a, 8b provided in the casings 7, 7a, 7b. Microwaves pass through the reaction tank 4 and the separator 5 from outside the reaction tank 4 and the separator 5, and the microwaves are irradiated to the fats and oils and alcohols in the reaction tank 4, or the alcohols in the separator 5. However, the present invention is not limited to this. For example, the outer wall of the reaction vessel 4 or the separator 5 may be used as a casing, and the microwave oscillators 8, 8a, 8b may be provided on the outer wall (casing). is there.
When the reaction tank 4 and the separator 5 are accommodated in the casings 7, 7 a, and 7 b as in the above embodiments, the microwave passes through the reaction tank 4 and the separator 5 from the outside. 4 and the separator 5 need to be made of a material having a high microwave transmittance. However, when the outer wall of the reaction vessel 4 or the separator 5 is also used as a casing, the material is not necessarily a material having a high microwave transmittance. It is not necessary to configure the reaction tank 4 or the separator 5.

  Furthermore, although each said embodiment demonstrated the case where the distiller which performs distillation which is a means to isolate | separate alcohol with the lowest boiling point using the difference in the boiling point of each component was used as the separator 5, It is also possible to use a separator 5 having a separating means.

Examples of the present invention will be described below.
(Examples 1 to 6)
The present embodiment is an embodiment of a manufacturing method for manufacturing biodiesel fuel using the apparatus as shown in FIG. In this example, distillation by a separator was performed, and the separated methanol was returned to the previous stage of the reaction tank to perform continuous production.

  Rapeseed oil was used as the fat and oil, and methanol was used as the alcohol. Slaked lime (commercially available 60% purity) was used as the solid alkali catalyst. The reaction temperature in the reaction vessel was 60 ° C., and the microwave frequency was 2.45 GHz.

  Table 1 shows the experimental operation conditions in Examples 1 to 6. That is, each condition of the mixing ratio of rapeseed oil and methanol, the amount of slaked lime added, the microwave output, the supply speed of the mixed liquid of rapeseed oil and methanol, and the residence time of the mixed fluid (mixed liquid) in the reaction tank are shown.

  The test results are shown in Table 2. Table 2 shows the yield (% by weight) of the biodiesel fuel (methyl ester in the oil phase) obtained by the reaction and the composition (% by weight) of the components in the fuel. As components, methyl esters of linolenic acid, linolenic acid, oleic acid, stearic acid, and palmitic acid were recovered, and the most methyl ester of oleic acid was recovered. Furthermore, when the results of the examples were compared, it was found that the yield varied with each treatment condition, but the composition of the components hardly changed.

  In addition, when the other conditions are the same and only the mixing ratio of rapeseed oil and methanol is changed (Examples 1, 4 and 5), the yield of methyl ester and the composition of the components are independent of the mixing ratio. It turned out to be similar. Furthermore, when the microwave output was changed (Examples 1, 4 and 6), it was also found that the yield of methyl ester and the composition of the components were the same regardless of the output. Furthermore, when the difference due to the residence time was examined (Examples 1, 2 and 3), the longer the residence time, the higher the yield of methyl ester, but the composition of the components may be the same. I understood.

(Examples 7 to 9)
This embodiment is an embodiment of a production method for producing biodiesel fuel using the apparatus as shown in FIG. However, in this example, the reaction vessel is not used as a reaction vessel having the shape as shown in FIG. 2, but a continuous production is performed using a round bottom flask type reaction vessel with improved fluid mixing in the vessel. It was.

  Rapeseed oil was used as the fat and oil, and methanol was used as the alcohol. Slaked lime (commercially available 60% purity) was used as the solid alkali catalyst. The reaction temperature in the reaction vessel was 60 ° C., and the microwave frequency was 2.45 GHz.

  Table 3 shows the experimental operation conditions in Examples 7 to 9. That is, each condition of the mixing ratio of rapeseed oil and methanol, the amount of slaked lime added, the microwave output, the supply speed of the mixed liquid of rapeseed oil and methanol, and the residence time of the mixed fluid (mixed liquid) in the reaction tank are shown.

  The test results are shown in Table 4. Table 4 shows the yield (% by weight) of the biodiesel fuel (methyl ester in the oil phase) obtained by the reaction and the composition (% by weight) of the components in the fuel. As components, methyl esters of linolenic acid, linolenic acid, oleic acid, stearic acid, and palmitic acid were recovered, and the most methyl ester of oleic acid was recovered. Furthermore, when the results of the examples were compared, it was found that the longer the residence time, the higher the yield, but the composition of the components hardly changed. This tendency was the same as in Examples 1 to 6.

4 Reaction tank 5 Separator

Claims (4)

A reaction tank (4) for reacting oils and fats with alcohol in the presence of a solid alkali catalyst, and reacting unreacted alcohols from the reaction product produced in the reaction tank (4). A separator (5) for separating, the reaction of the oils and fats in the reaction tank (4), and the reaction product produced in the reaction tank (4) and unreacted Separation of alcohols in the separator (5) is performed continuously, and the reaction product and unreacted alcohols are transferred from the reaction tank (4) to the separator (5). Accordingly, a biodiesel fuel production apparatus is characterized in that a Sanphon tube (12) is interposed between the reaction vessel (4) and the separator (5) .   The biodiesel fuel production apparatus according to claim 1, further comprising a return line (9) for returning the separated unreacted alcohols to the reaction tank (4) or its front side. In order to prevent the solid alkali catalyst in the reaction vessel (4) from being inadvertently transferred to the separator (5) side, a filter (16) for performing a filtration treatment includes the reaction vessel (4) and the separator. (5) The biodiesel fuel production apparatus according to claim 1 or 2, which is provided between the two . The biodiesel fuel production according to any one of claims 1 to 3 , wherein separation of unreacted alcohols from reaction products in the separator (5) is performed by heating by microwave irradiation. apparatus.

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