WO2009107783A1

WO2009107783A1 - Method and apparatus for producing biodiesel fuel oil and adsorbent-packed columns to be used therein

Info

Publication number: WO2009107783A1
Application number: PCT/JP2009/053692
Authority: WO
Inventors: 茂人早藤
Original assignee: 株式会社シー・ディー・エムコンサルティング
Priority date: 2008-02-27
Filing date: 2009-02-27
Publication date: 2009-09-03
Also published as: JPWO2009107783A1; JP5499302B2

Abstract

A production apparatus for producing a biodiesel fuel oil provided therein with a heater for heating a starting oil, comprising: a heating tank in which an outlet port for the starting oil is formed; an exchangeable first treating column; a reaction tank provided therein with an agitator, a catalyst-pooling tank which is connected to the above-described reaction tank and from which a lower alcohol solution containing an alkali catalyst dissolved therein is supplied to the above-described reaction tank; a three-way valve which is connected to the outlet port for the liquid reaction mixture in the above-described reaction tank; and an exchangeable second treating column in which an inlet port and an outlet port are formed respectively in the upper and lower parts, wherein the first treating column as described above is packed with an acid adsorbent and a moisture absorbent while the second treating column as described above is packed with a base adsorbent and a moisture absorbent.

Description

Biodiesel fuel oil production method, production apparatus, and adsorbent packed column used therefor

The present invention relates to an apparatus for producing biodiesel fuel oil that can be used as a fuel for transportation vehicles, an adsorbent-filled column used therefor, and a method for producing biodiesel fuel oil.

Currently, there is an increasing need for biodiesel fuel worldwide, and it can be used as a fuel for transportation vehicles, and can be manufactured with a small amount of money, and anyone can easily manufacture it. Things are sought.

However, if it is intended to be used as a fuel for transportation vehicles, it will cause trouble unless the purity of the fuel oil is high to some extent. However, various impurities and by-products are produced in the production by the alkali catalyst method, which is a general method for producing biodiesel fuel. The raw material fats and oils vary in content and content depending on the type, but contain free fatty acids, moisture, and solids. Furthermore, there are by-product glycerin obtained in the production process, unreacted lower alcohol, alkali catalyst, triglyceride, reaction intermediate diglyceride, and monoglyceride. In addition, since there is water and free fatty acids, saponified products can be produced. These need to be removed properly and cannot be easily manufactured.

As a method for removing impurities after the transesterification reaction, there are a method of washing with water and a method of removing by adsorption with an adsorbent. The former method has a problem in that the environmental load due to the wastewater is high. Further, the latter method has a problem that it is difficult to judge the replacement time of the column packed with the adsorbent, and that the cost is high if the replacement time is too early, and the quality of the product is deteriorated if the replacement time is too late.

In addition, as a method of removing impurities before the transesterification reaction, conventionally, the raw oil / fat is allowed to stand for a certain period of time to remove moisture, etc., and then the moisture, free fatty acid, etc. contained in the vegetable oil / fat from the beginning Some of the volatile components are removed by decompression (see Patent Document 1). In this method, a certain amount of time and equipment are required to leave it stationary. In addition, the apparatus is allowed to play in that it cannot be transesterified during that time. In addition, when the decompression device is provided, there is a problem that the entire biofuel production device becomes bulky and expensive.
In addition, many biodiesel fuel oil production apparatuses require a large industrial plant. For example, biodiesel fuel oil is produced under a fixed catalyst proposed by the present applicant and by a supercritical method. There is a technology (see Patent Document 2).
Japanese Patent No. 3934630 Japanese Patent Laid-Open No. 2006-193497

The problem to be solved by the present invention is a method for producing biodiesel fuel oil, which can be manufactured as a fuel for transportation vehicles, and can be manufactured even if the apparatus can be reduced in size and with a small amount of funds. To provide parts. More preferably, it is to provide the above-described production method, production apparatus and related accessory parts, which can be used by anyone to easily produce biodiesel fuel oil.

In the past, the inventors have allowed the raw material to stand for a certain period of time to allow the device to play in order to remove impurities such as moisture, by using a specific adsorbent and absorbent. Even if it is not allowed to stand for a long time, it is possible to easily remove impurities in the oil and fat before the transesterification reaction by an appropriate column configuration, and the adsorbent used before the transesterification reaction can also be used after the transesterification reaction. As for the adsorbent to be used, the present inventors have found that a fatty acid alkyl ester of a certain quality or more can be easily obtained by easily exchanging the column at an appropriate time.
That is, the present invention is characterized by the following configurations and structures.

(1) The manufacturing apparatus which manufactures biodiesel fuel oil has a heating tank, a 1st process column, a reaction tank, a three-way valve, a 2nd process column, and a product storage tank if needed from the upper part. The three-way valve is provided with a glycerin recovery tank.
The heating tank is provided with a heating device for heating the raw material fat and oil, and an outlet for the raw material fat is formed. The first processing column has an inlet at the upper part and an outlet at the lower part, and the inlet is the outlet of the heating tank. It is detachably communicated with and can be exchanged.
The reaction tank is detachably connected to the outlet at the bottom of the first processing column, has a sealing property, and has a stirring device inside. A three-way valve is communicated with the reaction solution outlet of the reaction tank, and the three-way valve is detachably communicated with an inlet of a second treatment column having an inlet at the upper portion and an outlet at the lower portion. It can be exchanged.
The storage tank communicating with the reaction tank supplies the lower alcohol solution in which the alkali catalyst is dissolved to the reaction tank. In this case, it is preferable that a heating device is provided in the storage tank, and this heating device is controlled together with the heating device of the heating tank, and the temperature of the heating tank and the catalyst storage tank can be set to be substantially the same. desirable.
The first treatment column is filled with an acid adsorbent and a moisture adsorbent, and the second treatment column is filled with a base adsorbent and a moisture adsorbent.
Here, it is preferable that the first and second processing columns include an indicator for measuring a water absorption function that changes color depending on water content and / or an indicator for measuring an adsorbent function that changes color depending on pH change. In this case, the column container is preferably partially or entirely transparent.

(2) The three-way valve is composed of a solenoid valve, and a sensor for distinguishing between a layer mainly composed of glycerin and a layer mainly composed of fatty acid alkyl ester is disposed between the reaction tank and the three-way valve, The biodiesel fuel oil manufacturing apparatus according to (1), wherein the opening and closing of the three-way solenoid valve is controlled based on the above.
(3) An eye plate having a large number of holes is installed between the outlet of the heating tank and the inlet of the first processing column and / or between the outlet of the reaction tank and the second processing column. The biodiesel fuel oil production apparatus according to (1) or (2) above.

(4) The storage tank of the lower alcohol solution in which the alkali catalyst used in the biodiesel fuel oil production apparatus described in (1) is a detachable column and is attached to the biodiesel fuel oil production apparatus. The former is a moisture-proof container that stores a lower alcohol solution in which an alkali catalyst is dissolved.

(5) The replaceable first processing column or the second processing column used in the biodiesel fuel oil production apparatus according to (1), wherein the color of the column container changes depending on the water content. A replaceable adsorbent-filled column comprising an indicator for measuring a water absorption function and / or an indicator for measuring an adsorbent function that changes color due to pH change, and at least a part of the column container is formed of a transparent wall.
(6) The adsorbent packed column according to (5), wherein the column container is composed of a column container main body and a heat-shrinkable film.
(7) The adsorbent packed column according to (5) or (6), wherein the container body is provided with an easy-open film film that seals the inlet and the outlet.
(8) The adsorbent-filled column according to (7), wherein the easy-open film at the outlet has a folded peel portion.

(9) A method for producing a biodiesel fuel oil comprising the following steps 1) to 5):
1) a step of heating at a temperature not lower than the temperature at which the raw material fats and oils are fluidized and lower than the boiling point of the lower alcohol used in the transesterification reaction;
2) A step of removing moisture and free fatty acids in the raw material fat through the raw material fat passed through the step 1) through the first treatment column filled with the acid adsorbent and the water absorbent.
3) The step of introducing the raw material fats and oils of the above 2) step into the reaction vessel, introducing the lower alcohol solution in which the alkali catalyst is dissolved into the reaction vessel, mixing and stirring the raw material fats and oils and the solution,
4) A step in which the reaction liquid obtained in the step 3) is separated into a layer mainly containing glycerin and a layer mainly containing a fatty acid alkyl ester by self-weight or centrifugal separation, and a layer mainly containing glycerin is taken out,
5) The liquid and the impurities in the layer mainly containing the fatty acid alkyl ester are passed through the second treatment column containing the base adsorbent and the water absorbent through the liquid of the layer mainly containing the fatty acid alkyl ester in the step 4). Removing.

According to the biodiesel fuel oil production method and production apparatus of the present invention, a biodiesel fuel oil that can be easily used as a fuel for transportation vehicles can be obtained. Further, according to the production apparatus for producing the biodiesel fuel oil of the present invention, the first processing column is a replaceable adsorbent column that removes impurities such as moisture and free fatty acid in the raw material, and the second processing column is a fatty acid. An adsorbent column that removes impurities such as catalysts in the alkyl ester, both of which can be exchanged. By installing the first processing column and the second processing column and making them exchangeable, a conventional large-scale apparatus for removing moisture and impurities from the raw material becomes unnecessary, and the apparatus can be downsized. In addition, since the first processing column and the second processing column can be exchanged, the quality of the fuel oil product can be constantly maintained in the process. In particular, if an indicator for measuring the water absorption function and / or an indicator for measuring the adsorbent function is mixed in the column so that the degradation of the functions of the first processing column and the second processing column can be seen, the column can be removed at an appropriate time. Anyone can easily obtain the fatty acid alkyl ester that is a stable quality fuel oil.
Further, when the raw material fat is oxidized, the performance of the fuel oil is deteriorated. In a production apparatus, as soon as raw material fats and oils are obtained, it is required to produce fuel oil promptly and use it quickly. In this respect, this apparatus is small in size, can use a small amount of raw material fats and oils, and can produce a small amount of fuel oil. Furthermore, the alkali catalyst method is used in the manufacturing process of this apparatus. However, the alkali catalyst has a risk of destroying the skin tissue when it touches the skin, and it is dangerous for an amateur to handle it. It is designed to be handled safely.

Embodiments of the present invention will be described below with reference to the accompanying drawings.
FIG. 1 is an example of an embodiment for carrying out the present invention, and is a schematic longitudinal sectional view of a biodiesel fuel production apparatus. FIG. 2 is a longitudinal sectional view when the adsorbent packed column according to the present invention is attached to a production apparatus.
As shown in FIG. 1, the biodiesel fuel production apparatus 1 has a support work 3 assembled on a carriage 2, and a heating tank 4, a first treatment column 5, a reaction tank 6, and a three-way valve in order from the top. 7, a second processing column 8, and a product storage tank 9. Further, a side surface of the support work 3 is provided with a storage tank 10 that is connected to the reaction tank 6 and supplies lower alcohol in which an alkali catalyst is dissolved to the reaction tank 6 and a glycerin recovery tank 11 that is connected to the three-way valve 7.

The heating tank 4 includes a disc-shaped 100-mesh net 12 that can be removed at the top and a cylindrical tank body 13 with a bottom. The raw oil and fat is supplied from above the 100 mesh net 12. Large solids are removed by the 100 mesh net 12. A gas inlet 14 is provided in the cylindrical tank body 13, the gas inlet 14 communicates with a three-way cock 16 through a pipe 15, and pressurized air is supplied into the heating tank 4 from an upper supply port of the three-way cock 16. . The pressurized air passes through the heating tank 4 and pressurizes the first processing column 5 provided in the lower part thereof to quickly move the raw oil and fat in the first processing column 5 downward. A pipe 17 is connected to the three-way cock 16 so that pressurized air can be supplied into the reaction vessel 6.
A heating device 18 is attached to the heating tank 4, a heater 19 of the heating device 18 is disposed in the heating tank 4, and a heater 20 is disposed in the storage tank 10. The temperature of each heater is controlled by a control device (not shown) in the heating device 18, and the temperature in each tank is set to be lower than the boiling point of the alcohol used for the alcohol solution in which the alkali catalyst is dissolved.
An outlet 21 is formed at the center of the bottom wall of the heating tank 4. A filter 22, a lid 24 of the first processing column 5, and an opening 24 a are provided in a flow path communicating with the outlet 21 and the first processing column 5. Is arranged. The filter 22 has a pore size of 10 to 50 μm, and removes solids that could not be removed by the disc-shaped 100-mesh net 12.

As shown in FIG. 2, a protrusion 26 is formed in advance on the outer wall of the column container 23, and the column container 23 is detachably provided via the protrusion 26 and a fastener 25 provided on the lid 24. The wide opening surface of the opening 24a of the lid 24 is fitted with the upper inlet 29 of the column container 23, and the eye plate 27 is formed in the flow path above the wide opening surface of the opening 24a. When the liquid from the upper part enters the column, the eye plate 27 having a large number of holes once flows into the column and drops onto the adsorbent layer. A mounting portion 63 of an elastic ring (polyurethane) 28 is formed on the lower peripheral edge of the lid 24, and the elastic ring 28 presses the peripheral edge of the inlet 29 of the column container 23 when fitting with the column container 23. As a result, the inlet 29 of the first processing column 5 is sealed.

As shown in FIG. 2, the column container 23 has a large-diameter inlet 29 at the top and an outlet 30 at the bottom. The inlet 29 of the container main body 23 is separated or displaced relative to the lid 24 during column replacement.
At least a part of the side wall of the column container 23 is a transparent wall, and a filter 31 for holding the adsorbent is provided at the bottom of the column container 23 to prevent the adsorbent from leaking downstream. Yes.
Before installation, the inlet 29 and the outlet 30 of the column container 23 are sealed with a moisture-proof film (easy-opening film) 64 that can be easily peeled (in FIG. 1, the inlet and outlet films are already installed, The film is not shown.), Can be easily peeled off and opened at the time of mounting. In particular, as the moisture-proof film 64 covering the lower end of the column in order to prevent ejection of its contents, use a film having a folded peel portion so that it can be easily peeled off when the container is attached. Is preferred.

Since the first processing column 5 is in the form of a replaceable cartridge, the column container is also an adsorbent storage container. For this reason, moisture-proof materials such as olefin-based plastics and glass are used so that the adsorption performance does not deteriorate due to moisture absorption during the storage period. A sealed structure having moisture resistance, such as being sealed with a moisture-proof film until use, is preferred. Particularly preferred is a combination of a column container body made of a hard plastic and a heat-shrinkable moisture-proof film accommodated in the column container. The adsorbent is sealed in a heat-shrinkable film, and the parts corresponding to the inlet and outlet of the raw material oil and fat have a structure that can be easily peeled. In such a structure, when the column is mounted on the apparatus of the present invention, the portions corresponding to the inlet and outlet of the raw oil and fat are released by the easy peel, but along the inner wall of the column container main body. Since the film remains attached to the inner wall and the liquid flows between the inner wall and the adsorbent, it is possible to avoid as much as possible the film that does not receive the adsorbing action by the adsorbent. Before use, the heat-shrinkable moisture-proof film may be shrunk by heat after sealing the adsorbent, or may be shrunk at the temperature during the transesterification reaction. The heating temperature for shrinking is higher than the stretching temperature when the film is formed and lower than the melting point of the film. When the film has a laminated structure of a plurality of resins, it is in the constituent resin and The temperature is lower than the melting point of the resin having the lowest melting point among the stretched resins. Furthermore, in the latter case, in addition to the above conditions, the stretching temperature is made lower than the temperature during the transesterification reaction. When such a heat-shrinkable moisture-proof film is heat-shrinked, the vicinity of the inlet 29 of the column container 23 is not heat-shrinked. As a result, the heat-shrinkable film can be attached to the container 23 while being folded at the inlet 29 and covering the protrusion 26.

In the 1st processing column 5, since water | moisture content and a free fatty acid are contained in raw material fats and oils, these are removed. Therefore, the adsorbent filled in the first processing column 5 is composed of a basic adsorbent and a moisture absorbent.
The basic adsorbent adsorbs free fatty acids, and basic alumina, alkali-treated activated carbon, basic silica gel and the like are exemplified, but basic alumina is preferable from the viewpoint of adsorption efficiency.
Examples of moisture absorbents include molecular sieves and silica. For example, silica contains cobalt chloride whose color changes with a change in moisture content as an indicator for measuring a function change (moisture adsorption ability). It is preferable to fill with silica. As is well known in the case of silica containing an indicator for measurement, it can be clearly recognized by changing from a blue color to a light pink color when the moisture adsorption ability decreases. Silica may be mixed with a basic adsorbent in the column or may be layered.

The content ratio between the basic adsorbent and the color changing agent that changes color due to the change in water content and silica is appropriately used depending on the type and characteristics of the raw oil. One reason is that free fatty acids and moisture differ greatly depending on the types and characteristics of the raw oils and fats. Another reason is whether or not the adsorption capacity of the first treatment column 5 has reached its limit, because it uses a color-changing agent due to a change in water content, so it does not directly indicate whether or not there is free fatty acid adsorption capacity. Because there is no.

At least a part of the column container in contact with the color changing agent is made transparent so that it can be seen that the color changing agent as the measurement indicator has changed color from the outside. The transparent portion is preferably in the vicinity of the raw material oil and fat outlet of the column container. The adsorbent in the adsorption column is generally white, but there is also black as in the case of alkali-treated activated carbon, so the discoloration may not be clearly recognized. In such a case, it is particularly necessary, but even if it is not the case, the color change agent alone or the white adsorption A structure in which a layer dispersed in a high concentration in the agent is separately provided and at least a part of the column container in contact with the layer is made of a transparent material is preferable.
Therefore, the extent to which free fatty acids are removed should be determined from the values obtained from empirical values that the free fatty acids have been removed to the extent that moisture has been removed to this extent regarding the type and identity of the raw fats and oils. Based on this, it is best to select the content ratio of the color changing agent that changes color due to the change in water content, silica, and basic adsorbent.

In the apparatus of the present invention, the outlet 30 of the first processing column 5 is communicated with the reaction tank 6 via a detachable handle 33 and a connecting pipe 34. The reaction tank 6 has airtightness and has a stirrer 35 inside. As described above, the reaction tank 6 is connected to the pipe 36 capable of taking in pressurized air and the intake pipe 37 from the lower alcohol storage tank 10 in which the alkali catalyst is dissolved. As described above, the raw fats and oils from which free fatty acids and moisture have been removed are supplied to the reaction tank 6 in a heated or heated state, and the alcohol reaction solution in which the alkali catalyst is dissolved is also stored in the heated or heated state. The reaction vessel 6 is charged from the tank 10 through the inlet 37.

Examples of the alkali catalyst include potassium catalysts such as potassium hydroxide, potassium hydrogen carbonate, potassium carbonate and potassium alcoholate; sodium catalysts such as sodium hydroxide, sodium oxide, sodium carbonate and sodium alcoholate; magnesium hydroxide, magnesium carbonate and magnesium oxide Magnesium catalysts; calcium catalysts such as calcium hydroxide and calcium carbonate; barium hydroxide, lithium carbonate and the like are exemplified, but a potassium catalyst is preferably used. The lower alcohol is an alcohol having 1 to 10 carbon atoms, preferably 1 to 4 carbon atoms such as n-butanol and isobutyl alcohol.

The amount of the alkali catalyst is 0.3 to 3.0% by mass, preferably 0.6 to 2.0% by mass, based on the raw material fat. The amount of the lower alcohol added is 0.15 to 0.75 mol, preferably 0.25 to 0.35 mol, per 100 g of the raw oil and fat. Alkali catalysts can destroy skin tissue when touched. The alkaline catalyst storage tank 10 is prepared in advance so that a lower alcohol solution in which an alkali catalyst is dissolved is prepared, and a container for storing the alkali catalyst is detachably connected to the manufacturing apparatus of the present invention as a storage tank for the lower alcohol solution in which the alkali catalyst is dissolved. It is preferable that the container is made of such a material, and this makes it easy to handle. What is used for the storage container and storage tank 10 is preferably moisture-proof, and for example, plastic having moisture-proof properties such as polyethylene is suitable.

In the reaction tank 6, the lower alcohol solution in which the raw oil and fat and the alkali catalyst are dissolved is transferred to the reaction tank and then stirred by the stirrer 35 to perform the transesterification reaction. After the reaction, stirring is stopped, and the layer is separated into a layer mainly composed of glycerin (multilayer) and a layer mainly composed of fatty acid alkyl ester (light layer). Layer separation is gravity separation. Centrifugation may be used instead of gravity separation.
As for the reaction tank 6, the outflow port 38 of the bottom wall is connected to the three-way valve 7, and the three-way valve 7 is formed of an electromagnetic valve in this embodiment. Therefore, the three-way solenoid valve 7 is controlled in conjunction with the layer discriminating sensor 39. The layer mainly composed of glycerin is fed to the glycerin recovery tank 11 via the connecting pipe 40 and the drive pump 41, and the layer mainly composed of fatty acid alkyl ester is ester. It is made to flow into the 2nd process column 8 which is an adsorption column after exchange reaction. The three-way valve 7 may be a normal manual valve, and the above operation may be performed by visual confirmation. The collection tank 11 is a detachable tank.

The ester of the fatty acid alkyl ester layer containing impurities from the reaction vessel 6 is a color changer that is an indicator for measurement that measures the functional change of the adsorbent and / or moisture absorbent that changes color due to pH change and / or water content change. It is passed through a second processing column 8 filled with an adsorbent containing activated clay. The container main body and the like of the second processing column 8 have the same structure or configuration as the first processing column 5 described above. A pipe 17 is connected to the three-way cock 16 so that pressurized air flows from a gas inlet 36 provided in the reaction vessel 6. The pressurized air passes through the reaction tank 6 and pressurizes the second processing column 8 provided in the lower part thereof to quickly move the ester of the fatty acid alkyl ester layer containing impurities downward.
The adsorbent packed inside the second processing column 8 is mainly activated clay, but besides this, acid clay, activated carbon, silica, florisil, alumina, activated alumina, zeolite, molecular sieves, sodium sulfate, magnesium sulfate, Examples include calcium chloride, alcohol adsorption resin, water absorption resin and the like.
Of these, activated clay is acidic and the entire adsorbent is also acidic. However, the activated clay gradually changes to alkaline due to the influence of the alkali catalyst contained in the layer mainly composed of fatty acid alkyl ester. When the activated clay shifts from acidic to alkaline, other impurities are generally adsorbed.

As the measurement indicator, the column replacement time may be determined by a color changing agent that changes color due to the change in the moisture content. Alternatively, the column replacement time may be determined by a color changing agent that changes color due to pH change.
In addition, as an indicator for measuring the change in pH, an indicator that is hardly soluble in water or lower alcohol and discolors when the pH is around 7 is suitably used. For example, PH such as phenol red (phenol sulfophthalein) is used. An indicator is exemplified. As a color changing agent that changes color due to a change in water content, silica gel containing cobalt chloride is preferable because of its excellent sensitivity, as in the case of the adsorption column before the transesterification reaction.
The indicator may be mixed with the adsorbent as in the first processing column 5 or may be layered.

In the apparatus of the present invention, the outlet 42 of the second processing column 8 is communicated with the product storage tank 9 via a detachable handle 43 and a connecting pipe 44. In the product storage tank 9, product biodiesel fuel oil is sent out through a pumping pump 45 and a delivery valve 46.

Next, the manufacturing method of the fuel oil is demonstrated using the biodiesel fuel oil manufacturing apparatus comprised in this way.
The raw oil / fat used in the production method of the present invention is preferably a virgin oil / fat derived from plants or its edible oil, but animal fat / oil can also be used. Examples of those derived from plants include palm oil, palm oil, palm kernel oil, rapeseed oil, soybean oil, sunflower oil, corn oil and the like.

First, in the heating tank 4, the raw material oil and fat is heated at a temperature not lower than the temperature at which the raw material oil and fat are fluidized and lower than the boiling point of the lower alcohol used in the transesterification reaction.
The transesterification described below is performed at a temperature lower than the boiling point of the lower alcohol and at which the raw material fats and oils are fluidized. Therefore, heating is unnecessary when the raw material oil and fat already has fluidity, but it is effective to raise it to near the reaction temperature. Here, the lower alcohol refers to an alcohol having 1 to 10 carbon atoms, preferably 1 to 4 carbon atoms, such as methanol, ethanol, propanol, butanol, and isobutyl alcohol. For example, in the case of methanol, the transesterification reaction is preferably performed at 55 to 60 ° C., so it is preferable that the heating tank 4 is preheated to 55 to 60 ° C.

Next, the raw material oil is passed through the filter 22 to remove solids in the heated raw material fat.
Even if the raw material fats and oils are subjected to the above-described temperature, solid content may be mixed in, so that they are removed. It is preferably removed before the reaction and immediately before the end of the production. If necessary, a mesh filter 22 having a size of about 10 to 50 μm is used before the reaction, and a mesh filter having a size of about 1 to 5 μm is used as necessary immediately before the end of production. It is not necessary to heat the raw oil and fat. If it is originally liquid, the solid content may be removed before heating.

Next, the water and free fatty acids in the raw oil and fat are removed by passing through the first treatment column 5 filled with the acid adsorbent and the water absorbent. It is best to use the first treatment column 5 having an adsorbent configuration according to the amount of water and the amount of free fatty acids contained in the raw oil and fat. In this case, the color change in the first processing column 5 can be confirmed visually. That is, the removal function of the adsorbent and moisture absorbent packed in the first processing column 5 can be easily determined and can be easily replaced.

Raw material fats and oils are introduced into the reaction tank 6, and an alcohol solution in which the alkali catalyst is dissolved is introduced into the reaction tank 6 from the catalyst storage tank 10 in which the solution of the lower alcohol in which the alkali catalyst is dissolved is stored. The raw oil and fat and the solution are mixed and stirred for a transesterification reaction. At this time, it is preferable to heat the raw oil and fat so that the temperatures of the alcohol solution in which the alkali catalyst is dissolved substantially coincide with each other.

Next, the reaction solution obtained in the reaction vessel 6 is separated into its own weight or a layer by centrifugal separation into a layer mainly containing glycerin and a layer mainly containing a fatty acid alkyl ester. The three-way solenoid valve 7 includes a layer discrimination sensor 39, and a layer mainly composed of glycerin is collected into the glycerin collection tank 11 through the connection pipe 40 and the drive pump 41 by interlocking control opening and closing. The layer mainly composed of fatty acid alkyl ester is caused to flow into the second treatment column 8 which is an adsorption column after the transesterification reaction.
In this case, the three-way valve 7 may be a normal manual valve, and the above operation may be performed by visual confirmation.

The second processing column 8 filled with the base adsorbent and the water absorbent is passed through the liquid of the layer mainly containing the fatty acid alkyl ester to remove water and impurities in the fatty acid alkyl ester. In this case as well, the replacement timing of the second processing column 8 can be determined visually as in the first processing column 5.
The product biodiesel fuel oil from the second processing column 8 is stored in the product storage tank 9 after passing through a filter for removing solids, if necessary, and sent through a feed valve 46 according to the supply request. Is done.
In such a configuration, impurities and by-products can be removed accurately and easily in the first and second processing columns 8. For this reason, the apparatus can be miniaturized, biodiesel fuel oil can be manufactured even with a small amount of funds, and high quality products can be manufactured.

The production apparatus for producing the biodiesel fuel oil of the present invention can be manufactured even if the apparatus can be miniaturized and the funds are small, and anyone can use the adsorbent column including the indicator according to the present invention. However, there is a high industrial applicability that can easily produce biodiesel fuel oil that can be used as a fuel for transportation.

It is a schematic longitudinal cross-sectional view of the manufacturing apparatus of the biodiesel fuel oil which concerns on this invention. It is a longitudinal cross-sectional view which shows the state which attached the adsorption agent filling column which concerns on this invention to the manufacturing apparatus.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Biodiesel fuel oil manufacturing apparatus 4 ... Heating tank 5 ... 1st processing column 6 ... Reaction tank 7 ... Three-way valve 8 ... 2nd processing column 9 ... Product Storage tank 10 .... Alkali catalyst storage tank 11 .... Glycerin recovery tank 23 ... Column container 27 ... Eye plate 28 ... Elastic ring

Claims

A production apparatus for producing biodiesel fuel oil,
The manufacturing apparatus includes a heating device that heats at least the raw material fat and oil therein, and a heating tank in which the outlet of the raw material fat and oil is formed;
An inlet at the top and an outlet at the bottom, the inlet detachably communicated with the outlet of the heating tank, and a replaceable first processing column;
A reaction tank detachably connected to the outlet of the first processing column and having a stirring device therein;
A storage tank that communicates with the inside of the reaction tank and supplies a lower alcohol solution in which an alkali catalyst is dissolved in the reaction tank;
A three-way valve communicating with the reaction solution outlet of the reaction vessel;
An inlet is formed in the upper part and an outlet is formed in the lower part, and the inlet comprises a second processing column that is detachably communicated with the three-way valve and is replaceable.
The biodiesel characterized in that the first treatment column is filled with an acid adsorbent and a water absorbent, and the second treatment column is filled with a base adsorbent and a water absorbent. Fuel oil production equipment.
The three-way valve is composed of a solenoid valve, and a sensor for distinguishing between a layer mainly composed of glycerin and a layer mainly composed of fatty acid alkyl ester is disposed between the reaction tank and the three-way valve, and is based on the sensor. The biodiesel fuel oil manufacturing apparatus according to claim 1 which controls opening and closing of a three-way solenoid valve.
An eye plate having a number of holes is installed between an outlet of the heating tank and an inlet of the first processing column and / or between an outlet of the reaction tank and the second processing column. The biodiesel fuel oil production apparatus according to 1 or 2.
A storage tank of a lower alcohol solution in which an alkali catalyst used in the biodiesel fuel oil production apparatus according to claim 1 is dissolved, and is a column detachable from the biodiesel fuel oil production apparatus, A moisture-proof container capable of storing a lower alcohol solution in which an alkali catalyst is dissolved.
The replaceable first processing column or the second processing column used in the biodiesel fuel oil production apparatus according to claim 1, wherein the water absorption function measurement changes in color depending on the water content in the column container. An exchangeable adsorbent-filled column comprising an indicator for use and / or an indicator for measuring an adsorbent function that changes color due to pH change, wherein at least a part of the column container is formed of a transparent wall.
6. The adsorbent packed column according to claim 5, wherein the column container comprises a column container main body and a heat shrinkable film.
The adsorbent packed column according to claim 5 or 6, wherein the container is provided with an easy-open film that seals the inlet and the outlet.
The adsorbent-filled column according to claim 7, wherein the easily openable film at the outlet has a folded peel portion.
A process for producing a biodiesel fuel oil comprising the following steps (1) to (5):
(1) A step of heating at a temperature not lower than the temperature at which the raw oil and fat is fluidized and lower than the boiling point of the lower alcohol used for the transesterification reaction,
(2) A step of removing moisture and free fatty acids in the raw material fats and oils through the raw material fats and oils subjected to the step (1) through the first treatment column filled with the acid adsorbent and the water absorbent.
(3) The step of introducing the raw material fats and oils of the above step (2) into the reaction vessel, introducing the lower alcohol solution in which the alkali catalyst is dissolved into the reaction vessel, mixing and stirring the raw material fats and oils and the solution,
(4) The reaction liquid obtained in the step (3) is separated into a layer mainly composed of glycerin and a layer mainly composed of fatty acid alkyl ester by its own weight or by centrifugation, and a layer mainly composed of glycerin is taken out. Process,
(5) The water and impurities in the fatty acid alkyl ester are removed by passing the liquid of the layer mainly containing the fatty acid alkyl ester in the step (4) through the second treatment column containing the base adsorbent and the water absorbent. Process.