JP2013107058A - Chemical reaction device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a chemical reaction device capable of grasping the internal state of a reactor.SOLUTION: The chemical reaction device includes: a horizontal flow type reactor 13 that allows a liquid content to flow in a horizontal direction with an unfilled space present upward; a microwave generator 14 that generates microwaves; at least one waveguide 15 that transmits microwaves generated by the microwave generator 14 to the unfilled space of the reactor 13; a microwave invasion blocking tube 51 that is connected with the reactor 13, allows a content to circulate and has such an attribute as to inhibit invasion of microwaves generated by the microwave generator 14; and a detection section 52 that can detect the liquid level position of the content in the reactor through the content in the microwave invasion blocking tube. Thus, the liquid level position in the reactor 13 can be grasped.

Description

  The present invention relates to a chemical reaction apparatus that irradiates microwaves in a reactor.

  Conventionally, a chemical reaction apparatus and a chemical reaction method for performing heat treatment or the like by irradiating a reactant with microwaves (electromagnetic waves) are known (for example, see Patent Document 1).

Special table 2006-516008 gazette

  In addition, in such a chemical reaction apparatus that irradiates microwaves, there has been a desire to know the internal state.

  The present invention has been made to solve the above-described problems, and an object of the present invention is to provide a chemical reaction apparatus that can know the state in the reactor.

In order to achieve the above object, a chemical reaction apparatus according to the present invention includes a horizontal flow reactor in which a liquid content flows in a horizontal direction with an unfilled space above, and a microwave that generates microwaves. A generator, one or more waveguides that transmit the microwave generated by the microwave generator to the unfilled space of the reactor, and a tube that is connected to the reactor and through which the contents can flow. A microwave intrusion prevention tube that has an attribute capable of preventing the generated microwave from entering, and a detection unit capable of detecting the liquid level level of the contents in the reactor through the contents in the microwave intrusion prevention tube And.
With such a configuration, the liquid level level of the contents can be detected via the microwave intrusion prevention tube, so that the liquid level level can be detected without being greatly influenced by the microwave. In addition, since the liquid level level position is not detected in the reactor, the liquid level level position can be prevented from affecting the microwave irradiation in the reactor and the electromagnetic field distribution in the unfilled space. .

Moreover, in the chemical reaction device according to the present invention, the detection unit may be a liquid level gauge that can detect the liquid level level visually.
With such a configuration, it is possible to provide a chemical reaction apparatus that allows the measurer to detect the liquid level level by visual observation.

In the chemical reaction device according to the present invention, the detection unit may measure the liquid level level position.
With such a configuration, it is possible to provide a chemical reaction apparatus in which the detection unit automatically measures the liquid level level position.

In the chemical reaction device according to the present invention, the microwave intrusion prevention tube may be a tube having a cutoff frequency higher than the frequency of the microwave generated by the microwave generator.
With such a configuration, it is possible to make it difficult for the microwave to enter the microwave intrusion prevention tube.

Moreover, in the chemical reaction device according to the present invention, the microwave intrusion prevention tube may be a tube having a length such that the intensity of the invaded microwave is 1/10 or less.
With such a configuration, even if microwaves enter the microwave intrusion prevention tube, the microwaves are attenuated to 1/10 or less when the liquid level level is detected.

Further, in the chemical reaction device according to the present invention, the microwave invasion blocking tube has a length such that the degree of coupling is −10 (dB) or less when the reactor is a main waveguide and the microwave invasion blocking tube is a sub-waveguide. And a tube having a cross-sectional size.
With such a configuration, it is possible to effectively prevent the microwave from entering the microwave intrusion prevention tube.

Moreover, in the chemical reaction device according to the present invention, the microwave intrusion prevention tube may be connected to the reactor at the lowest part of the reactor.
With such a configuration, the microwave intrusion prevention tube is connected to the position farthest from the unfilled space irradiated with the microwave, and it is possible to make it more difficult for the microwave to enter the microwave invasion prevention tube.

The chemical reaction apparatus according to the present invention may further include one or more stirring means for rotating and stirring the contents in the reactor.
With such a configuration, the contents are agitated, so that the contents in the reactor can be more uniformly irradiated with microwaves. As a result, for example, it is possible to avoid a situation in which microwaves are irradiated only to a part of the contents in the reactor.

Further, the chemical reaction apparatus according to the present invention includes two or more microwave generators, the two or more microwave generators generate microwaves having two or more frequencies, and the microwave intrusion prevention tube has two or more microwave invasion tubes. It may have an attribute that can prevent the intrusion of microwaves of a certain frequency.
With such a configuration, even when microwaves having a plurality of frequencies are irradiated, it is possible to make it difficult for the microwaves to enter the microwave intrusion prevention tube.

Moreover, in the chemical reaction device according to the present invention, the reactor has a plurality of partition plates that divide the interior into a plurality of chambers, and each partition plate has a flow path through which contents flow from the upstream side to the downstream side. Also good.
With such a configuration, a plurality of chambers in the reactor can be realized by the partition plate.

  According to the chemical reaction apparatus of the present invention, it is possible to know the internal situation of the reactor, that is, the liquid level level position in the reactor.

The figure which shows the structure of the chemical reaction apparatus by Embodiment 1 of this invention. Explanatory drawing about the detection of the liquid level level position by visual observation in the same embodiment Explanatory drawing about the detection of the liquid level level position by visual observation in the same embodiment Explanatory drawing about the detection of the liquid level level position by the detection part in the embodiment Explanatory drawing about the detection of the liquid level level position by the detection part in the embodiment The figure which shows an example of an internal structure of the reactor by the embodiment The figure which shows the example of the partition plate in the same embodiment The figure which shows the example of the partition plate in the same embodiment The figure which shows the example of the partition plate in the same embodiment The figure which shows the example of the partition plate in the same embodiment The figure which shows the example of the partition plate in the same embodiment The figure which shows the example of the partition plate in the same embodiment The graph which shows the ester conversion rate in the Example of the same embodiment The figure which shows another example of the microwave generation part and waveguide in the same embodiment The figure for demonstrating the irradiation position of the microwave in the embodiment The figure for demonstrating the irradiation position of the microwave in the embodiment The figure for demonstrating the coupling | bonding degree in the same embodiment

  Hereinafter, a chemical reaction apparatus according to the present invention will be described using embodiments. Note that, in the following embodiments, the components given the same reference numerals are the same or equivalent, and repetitive description may be omitted.

(Embodiment 1)
A chemical reaction apparatus according to Embodiment 1 of the present invention will be described with reference to the drawings. The chemical reaction apparatus according to the present embodiment irradiates the contents of the reactor with microwaves, and can detect the liquid level level position in the reactor.

  FIG. 1 is a diagram showing a configuration of a chemical reaction apparatus 1 according to the present embodiment. The chemical reaction apparatus 1 according to the present embodiment includes a mixing unit 12, a reactor 13, a microwave generator 14, a waveguide 15, a microwave control unit 16, a catalyst separation unit 17, and a processing liquid storage tank. 18, a microwave intrusion prevention tube 51, and a detection unit 52.

  The mixing unit 12 mixes the raw material and the solid catalyst. The mixing part 12 may mix a raw material etc. and a reactive agent. The raw material may include a plurality of substances. For example, when esterification is performed in the reactor 13, fats and oils and alcohols may be used as raw materials. The raw material and the solid catalyst may be supplied to the mixing unit 12 by a pump 11 as shown in FIG. 1, or may be supplied to the mixing unit 12 by other methods. For example, the mixing unit 12 may mix two or more substances by rotating a blade-shaped member, a wing-shaped member, or a screw-shaped member. In this embodiment, the case where the catalyst mixed with the raw material is a solid catalyst (heterogeneous catalyst) will be described, but the catalyst may be a liquid catalyst (homogeneous catalyst). Also, the solid catalyst may or may not form a fluidized bed in the reactor 13. The shape of the solid catalyst is not limited. The shape of the solid catalyst may be, for example, an amorphous granular shape, a cylindrical shape (may be hollow or not), a spherical shape, a pellet shape, a ring shape, a shell shape, and the like. Also, the solid catalyst may or may not have, for example, microwave absorption or microwave sensitivity. When the solid catalyst has microwave absorptivity or microwave sensitivity, the solid catalyst is heated by the microwave when the microwave is irradiated inside the reactor 13 described later, and in the vicinity of the solid catalyst. The chemical reaction will be promoted. Note that the microwave absorbability and microwave sensitivity depend on the frequency of the irradiated microwave, the temperature inside the reactor 13, and the like. In other words, the microwave absorption is high in the microwave frequency to be used and the temperature inside the reactor 13 in which the raw material is reacted. Therefore, for example, a solid catalyst containing such a substance having a high microwave absorption property may be used. For example, when 2.45 GHz microwaves are irradiated, carbons other than fullerene (eg, graphite, carbon nanotubes, activated carbon, etc.), iron, nickel, cobalt, There is a ferrite or a metal oxide. Therefore, the solid catalyst may contain a substance having such microwave absorbability. Specifically, the solid catalyst may be a composite in which such a substance having microwave absorbability and microwave sensitivity and a metal or a metal oxide are combined. The composite may be a combination of a substance having wave sensitivity and a catalyst such as an alkali catalyst or an acid catalyst, or a substance having microwave absorption or microwave sensitivity and a catalyst such as an alkali catalyst or an acid catalyst. Further, it may be a composite in which a metal or a metal oxide is combined. The compositing may be performed, for example, by physical adsorption, may be performed by chemical bonding, may be performed by alloying, or may be performed by other methods. In addition, in the mixing unit 12, preliminary heating may or may not be performed in preparation for the reaction in the reactor 13. In the case of performing the preliminary heating, it is preferable that the temperature of the preliminary heating in the mixing unit 12 is controlled so that the raw material or the like has a desired temperature or a desired temperature range when entering the reactor 13. It is. In addition, when preheating in the mixing part 12 is not performed, the heating corresponding to the preheating may be performed in the reactor 13. The raw material and the solid catalyst mixed in the mixing unit 12 are put on the upstream side of the reactor 13.

  The reactor 13 is a horizontal flow type reactor in which liquid contents flow in the horizontal direction with an unfilled space above. Note that the contents flowing in the reactor 13 in the horizontal direction means that the reactor 13 is not a vertical flow type reactor in which the contents flow in the vertical direction, and strictly flows in the horizontal direction. It does not have to be. It is sufficient that the contents flow as a whole in a direction close to horizontal. For example, the reactor 13 may be inclined from the upstream side toward the downstream side. The content is, for example, a mixture of a raw material and a catalyst. The raw material and the catalyst mixed in the mixing unit 12 flow in the reactor 13. In addition, since a product is produced | generated from a raw material by the chemical reaction in the reactor 13, you may consider that the product is contained in the content of the reactor 13. FIG. That is, it can be said that the content is a raw material and / or a product. Moreover, since an unfilled space exists above the contents, the contents are usually other than gas. Further, since the contents have fluidity inside the reactor 13, the contents are other than solids (for example, powder and granular materials). Therefore, the contents are liquid. The liquid content may be high fluidity such as water, oil, aqueous solution, colloidal solution, etc., or low fluidity such as slurry or suspension. There may be. Since the contents of the reactor 13 circulate through the microwave intrusion prevention pipe 51 as will be described later, even if the liquid contents have low fluidity, the liquid contents do not vibrate from the outside for a certain period of time. It is preferable to have fluidity that allows the microwave intrusion prevention pipe 51 to flow as the time passes. In other words, it is preferable that the liquid contents have fluidity that can flow in the pipe without external vibration. The inner wall of the reactor 13 is preferably made of a material that reflects microwaves. An example of a substance that reflects microwaves is metal. The internal configuration of the reactor 13 will be described later.

  The microwave generator 14 generates a microwave. The chemical reaction apparatus 1 according to the present embodiment may include one microwave generator 14 or may include two or more microwave generators 14. The frequency of the microwave is not limited, but may be, for example, 2.45 GHz, 5.8 GHz, 24 GHz, 913 MHz, or other The frequency may be in the range of 300 MHz to 300 GHz.

  The waveguide 15 transmits the microwave generated by the microwave generator 14 to the unfilled space of the reactor 13. As shown in FIG. 1, there are usually as many waveguides 15 as the number of microwave generators 14. In addition, it is preferable to use the waveguide 15 having a standard corresponding to the frequency of the microwave generated by the microwave generator 14.

  The microwave control unit 16 controls the output of the microwave irradiated to the reactor 13 according to the temperature measured by the temperature measurement unit 25 described later. By the control by the microwave control unit 16, the inside of the reactor 13 can be maintained at a desired temperature or a desired temperature range.

  The catalyst separation unit 17 separates the catalyst from the product after the reaction in the reactor 13. When the catalyst mixed with the raw material is a solid catalyst, for example, the solid catalyst may be separated by a filter, or the solid catalyst may be separated by precipitating one of the solid catalyst and the product. When the solid catalyst contains a magnetic material, the solid catalyst may be separated by adsorbing the solid catalyst with a magnet (a permanent magnet or an electromagnet). The separated solid catalyst can be reused as appropriate. When a liquid catalyst is used, the catalyst may be separated by performing distillation, extraction, or neutralization in the catalyst separation unit 17.

  In the treatment liquid storage tank 18, the product from which the catalyst is separated in the catalyst separation unit 17 is placed. And it will be divided into final products and by-products as appropriate. For example, when the raw material is a free fatty acid and esterification is performed in the reactor 13, a product that is a biodiesel fuel and a by-product that is water are obtained. In that case, an acid catalyst is used. For example, when the raw material is triglyceride and transesterification is performed in the reactor 13, a product that is biodiesel fuel and a by-product that is glycerin are obtained. In that case, an alkali catalyst is used.

  It should be noted that a cooler (not shown) for cooling the substance after the reaction in the reactor 13 may be provided in the subsequent stage of the reactor 13, or may not be so. In the former case, for example, the cooler may cool the substance after the reaction in the reactor 13 with water.

  The microwave intrusion prevention pipe 51 is a pipe that is connected to the reactor 13 and through which the contents can flow. The microwave intrusion prevention pipe 51 is a pipe having an attribute capable of preventing the microwave intrusion generated by the microwave generator 14. The phrase “can prevent the microwave from entering” may be that the microwave can be completely blocked, that is, the microwave cannot enter the microwave penetration blocking pipe 51 at all, It may be possible to reduce the intensity of the microwave compared to the location of the reactor 13 to which the wave intrusion prevention pipe 51 is connected. In the latter case, microwaves slightly enter the microwave intrusion prevention pipe 51, but the level of the intrusion does not affect the detection of the liquid level level described later, and in the reactor 13. It is preferable that the range does not affect the microwave irradiation. The cross-sectional shape of the microwave intrusion prevention tube 51 may be, for example, a circle, a rectangle, or other shapes. However, it is preferable that the microwave intrusion prevention pipe 51 has a diameter that allows the contents of the reactor 13 to flow. Further, the position of the reactor 13 to which the microwave intrusion prevention pipe 51 is connected may be anywhere as long as it is below the liquid level position of the contents (that is, below the vertical direction). However, when the liquid level level position fluctuates, it is preferable that the connection is made below the lowest liquid level level position. Further, the microwave intrusion prevention tube 51 may be connected to the reactor 13 at the lowermost part of the reactor 13. By doing so, the microwave intrusion prevention pipe 51 can be connected to the reactor 13 at a position farthest from the unfilled space. As a result, even in the reactor 13, the microwave intrusion prevention tube 51 can be connected to the reactor 13 at a position where the microwave intensity is considered to be particularly weak, and the microwave that enters the microwave invasion prevention tube 51. It is considered that can be further reduced. The attribute of the microwave intrusion prevention pipe 51 that can prevent the microwave intrusion is usually an attribute of the size of the cross section of the microwave invasion prevention pipe 51, for example, an attribute related to a diameter or a radius in the cross section (the cross section is circular). Or the attribute relating to the length and width in the cross section (when the cross section is rectangular). Further, the attribute may include the length of the microwave intrusion prevention tube 51. The length of the microwave intrusion prevention pipe 51 may be, for example, the length from the junction point with the reactor 13 in the microwave penetration prevention pipe 51 to the junction point with the detection unit 52, or with the reactor 13 The microwave intrusion prevention pipe 51 from the junction point may have a length in a straight line range. In general, the microwave intrusion prevention pipe 51 and the wall surface portion of the reactor 13 to which the microwave intrusion prevention pipe 51 is joined are orthogonal to each other. The microwave intrusion prevention tube 51 is preferably made of a material that does not transmit microwaves. The microwave intrusion prevention tube 51 may be made of a material such as iron or stainless steel, for example.

Here, the diameter and the vertical and horizontal lengths in the cross section of the microwave intrusion prevention tube 51 will be described. The waveguide has a cut-off frequency that means the lowest frequency of microwaves that can be transmitted. Therefore, usually, a microwave having a frequency equal to or higher than the cutoff frequency is transmitted to the waveguide. The microwave intrusion prevention tube 51 also has contents inside, but can be considered to be the same as the waveguide. Therefore, the microwave intrusion prevention tube 51 which is a tube having a cutoff frequency higher than the frequency of the microwave generated by the microwave generator 14 may be used. By doing so, the microwave generated by the microwave generator 14 can be prevented from propagating through the microwave intrusion prevention tube 51. For example, if the cutoff frequency is f (Hz), the cross section of the microwave intrusion prevention tube 51 is circular, and its radius at the cutoff frequency is r (m),
r = c / (3.41f)
It becomes. Here, c is the speed of light (3.0 × 10 ⁸ m / s). Therefore, when the frequency of the microwave generated by the microwave generator 14 is f, and the radius of the cross section of the microwave intrusion prevention tube 51 is smaller than the above-described r, On the other hand, the frequency of the microwave generated by the microwave generator 14 is lower than the cutoff frequency of the microwave intrusion prevention tube 51. Thus, the radius of the cross section of the microwave intrusion prevention tube 51 may be selected. Note that the relationship between the cutoff frequency and the radius is the relationship in the TE11 mode. If the cut-off frequency is in the TE11 mode, the cut-off frequency is obtained in the other modes, so the TE11 mode is adopted. Here, the case where the cross section of the microwave intrusion prevention pipe 51 is circular has been described. However, when the cross section is a rectangle of a (m) × b (m), a, b and the cutoff frequency Since the similar relationship is known, the a (m in the cross section of the microwave intrusion prevention tube 51 is used so that the cutoff frequency becomes higher than the frequency of the microwave generated by the microwave generator 14. ) Or b (m) may be determined.

As described above, the microwave propagates through the microwave intrusion prevention tube 51 by using the microwave invasion prevention tube 51 which is a tube having a cutoff frequency higher than the frequency of the microwave generated by the microwave generator 14. do not do. That is, the microwave that has entered the microwave intrusion prevention tube 51 is attenuated. However, the method of attenuation differs depending on the frequency of the microwave. For example, it is assumed that the microwave intrusion prevention tube 51 has a rectangular cross section and a width. It is assumed that the direction of the electric field in the microwave penetration blocking tube 51 is perpendicular to the surface having the width a. Then, the electric field strength of the microwave having a frequency equal to or lower than the cutoff frequency is attenuated as follows.
exp (-k'z)
However, k ′ is as follows.
k ′ = ((π / a) ² − (ω / c) ² ) ^1/2
Here, ω is an angular frequency (angular frequency) of the microwave generated by the microwave generator 14. Z is a coordinate in the length direction of the microwave intrusion prevention tube 51 where the junction point with the reactor 13 is 0. Therefore, when the value of z at which the microwave intensity is attenuated to 1/10 is z1, from the above formula,
z1 = 2.3 × ((π / a) ² − (ω / c) ² ) ^−1/2
It becomes. As a result, the microwave intrusion prevention tube 51 only needs to have a length of z1 or more in order for the intensity of the microwave that has entered to be 1/10 or less. Therefore, you may make it use the microwave penetration | invasion prevention pipe | tube 51 of the length more than z1. For the above formula, refer to the following document, for example.
Literature: Feynman, Layton, Sands, "Electromagnetic waves and properties", Iwanami Shoten, 1971

  Although the microwave intrusion prevention tube 51 having a rectangular cross section has been described here, the microwave intensity is similarly reduced to 1/10 for other cross sections, for example, the microwave invasion prevention tube 51 having a circular cross section. Z1 that is the value of z that attenuates to can be calculated. Therefore, also in that case, by setting the length of the microwave intrusion prevention pipe 51 to z1 or more, the microwave at the time of detecting the liquid level level is 1/10 or less of the position of the reactor 13. can do. Although the case where the microwave intrusion prevention tube 51 having a length equal to or longer than 1/10 of the microwave is used has been described here, it is needless to say that the present invention is not limited thereto. For example, a microwave intrusion prevention tube 51 having a length equal to or greater than 1/20 of the microwave may be used, or a microwave invasion prevention tube 51 having a length of 1/50 or more of the microwave may be used. Further, when the microwave intensity is sufficiently small at the junction between the microwave penetration blocking pipe 51 and the reactor 13, the microwave penetration prevention having a length equal to or longer than 1/5 of the microwave at the junction is performed. A tube 51 may be used.

  Moreover, when considering the prevention of the microwave intrusion into the microwave intrusion prevention pipe 51, the attribute of the microwave invasion prevention pipe 51 may be determined in consideration of the degree of coupling. That is, considering the degree of coupling when the reactor 13 is a main waveguide (main line) and the microwave intrusion prevention pipe 51 is a sub-waveguide (sub-line), the length of the coupling degree is less than a desired value and You may determine the attribute of the microwave penetration | invasion prevention pipe | tube 51 so that it may become a pipe | tube of the magnitude | size of a cross section. The desired value may be, for example, -10 (dB), -30 (dB), -50 (dB), or the like. Even in that case, the microwave intrusion prevention tube 51 is usually a tube having a cutoff frequency higher than the frequency of the microwave generated by the microwave generator 14.

ここで、Ｓ＝ａ×ｂは、主導波管の断面積であり、ｔは、導波管結合面の板厚である。また、λは、マイクロ波発生器１４が発生するマイクロ波の自由空間波長であり、λ_０は、管内波長であり、λ_ｃ＝２ａは遮断波長である。なお、主導波管であるリアクター１３に、副導波管であるマイクロ波侵入阻止管５１を接続する場合には、そのマイクロ波侵入阻止管５１の長さがｔであると考えることができる。したがって、マイクロ波侵入阻止管５１の長さｔを用いて上記式を計算すればよい。なお、上記式では、Ｃが正の値となるようになっている。そのため、上述のように、結合度を−１０（ｄＢ）とする場合には、上記Ｃの値が１０（ｄＢ）となるように、マイクロ波侵入阻止管５１の直径（ｄ）や、長さ（ｔ）を決定すればよいことになる。なお、ここでは、主導波管であるリアクター１３の断面が矩形であり、円孔を介して副導波管と接続される場合について説明したが、そうでなくてもよい。例えば、主導波管であるリアクター１３の断面が円形であってもよい。また、例えば、円孔ではなく、矩形の孔を介して副導波管と接続されてもよい。なお、そのような場合には、それに応じた結合度の式を用いてマイクロ波侵入阻止管５１の属性を決定することが好適である。 An example of the above-described method for calculating the coupling degree will be described with reference to FIG. FIG. 9 shows a case where a main waveguide and a sub-waveguide having a rectangular cross section are connected via a circular hole having a diameter d on the long side of the main waveguide. In the cross section of the main waveguide, the length of the long side is a, and the length of the short side is b. Further, x ₀ is the distance from the tube axis circular hole to the center. In such a case, it is known that the degree of coupling C (dB) is as follows.

Here, S = a × b is the cross-sectional area of the main waveguide, and t is the thickness of the waveguide coupling surface. Also, λ is the free space wavelength of the microwave generated by the microwave generator 14, λ ₀ is the guide wavelength, and λ _c = 2a is the cutoff wavelength. In addition, when connecting the microwave penetration | inhibition prevention pipe | tube 51 which is a subwaveguide to the reactor 13 which is a main waveguide, it can be considered that the length of the microwave penetration | invasion prevention pipe | tube 51 is t. Therefore, the above equation may be calculated using the length t of the microwave intrusion prevention tube 51. In the above formula, C is a positive value. Therefore, as described above, when the degree of coupling is −10 (dB), the diameter (d) and the length of the microwave intrusion prevention tube 51 so that the value of C is 10 (dB). It is only necessary to determine (t). Although the case where the reactor 13 serving as the main waveguide has a rectangular cross section and is connected to the sub waveguide via a circular hole has been described here, this need not be the case. For example, the cross section of the reactor 13 that is the main waveguide may be circular. Further, for example, the sub-waveguide may be connected via a rectangular hole instead of a circular hole. In such a case, it is preferable to determine the attribute of the microwave intrusion prevention tube 51 using an expression of the degree of coupling corresponding thereto.

In the above description, the case of considering how much the microwave is attenuated by the microwave intrusion prevention tube 51 has been mainly described. However, the intensity of the microwave at the junction between the microwave intrusion prevention pipe 51 and the reactor 13 depends on the intensity of the microwave generated by the microwave generator 14, the contents, and the like. Therefore, instead of considering the attenuation of the microwave in the microwave intrusion prevention tube 51, the power density of the microwave at the junction between the microwave intrusion prevention tube 51 and the detection unit 52 may be considered. For example, even if the attribute of the microwave intrusion prevention tube 51 is determined so that the microwave power density is 10 (mW / cm ² ) or less at the junction between the microwave intrusion prevention tube 51 and the detection unit 52. Good. The power density of the microwave may be other than 10 (mW / cm ² ). For example, you may determine the attribute of the microwave penetration | invasion prevention pipe | tube 51 so that it may become 5 (mW / cm < ² >) or less, or 1 (mW / cm < ² >) or less. Even in such a case, it goes without saying that it is preferable to use the microwave intrusion prevention tube 51 that is a tube having a cutoff frequency higher than the frequency of the microwave generated by the microwave generator 14.

  The detection unit 52 is a component that can detect the liquid level level of the content in the reactor 13 via the content in the microwave intrusion prevention tube 51. It should be noted that the fact that the liquid level level can be detected via the contents in the microwave intrusion prevention pipe 51 means that at least the contents in the microwave invasion prevention pipe 51 are used to detect the liquid level level position. That's what it means. For example, the liquid level level may be detected by the contents in the microwave intrusion prevention pipe 51 flowing into the detection unit 52, or the microwave invasion prevention pipe 51 may be detected. The liquid level level measurement may be performed using the content itself. The detection of the liquid level level itself may be performed by the detection unit 52 or may be performed by a measurer other than the detection unit 52. That is, the liquid level level position may be detected by (1) the measurer or (2) the detection unit 52. In the case of (1), the detection unit 52 enables the liquid level level position to be detected by the measurer. Hereinafter, each case will be described.

(1) When a measurer detects a liquid level level position In this case, the detection part 52 shows a liquid level level position so that a measurer can detect a liquid level level position. That is, the detection unit 52 may be a liquid level gauge that can detect the liquid level level visually. Specifically, as shown in FIG. 2A, the detection unit 52 may be a tubular member 52 a extending in the vertical direction in which the content 20 in the reactor 13 flows through the microwave intrusion prevention pipe 51. In FIG. 2A, the microwave intrusion prevention tube 51 and the detection unit 52 show their external appearance, and the reactor 13 shows a simplified internal cross section viewed from the length direction. In addition, it is preferable that the tubular member 52a can see the inside at least partially. That is, as shown in FIG. 2A, a window portion 52b through which the inside of the tubular member 52a can be seen may be provided. Alternatively, the tubular member 52a itself may be a transparent member (for example, a tubular level gauge). That is, the tubular member 52a itself may be a glass tube or the like. Note that the window portion 52b may be an inset transparent member, for example. It is preferable that the tubular member 52a and the window part 52b can cover the range from the lowest level of the contents in the reactor 13 to the highest level. In the case of (1), the detection unit 52 may not indirectly indicate the liquid level level position but may indirectly indicate it. That is, a float having a magnet is floated in the tubular member 52a, and the position of the float is magnetically indicated by an indicating mechanism outside the tubular member 52a, so that the measurer can grasp the liquid level level position. May be. Further, the detection unit 52 may be a liquid level gauge that presents the liquid level level position so that the measurer can detect it by other methods. Since various types of liquid level gauges are already known, description thereof will be omitted.

(2) When the detection part 52 detects a liquid level level position In this case, the detection part 52 measures a liquid level level position. Therefore, even if the measurer does not visually detect the liquid level level position, the liquid level level position is automatically measured. Various methods are known, for example, as follows.

(2-1) Method of Detecting Pressure As shown in FIG. 3A, the detection unit 52 measures the pressure of the content 20 in a state where it is communicated with the inside of the reactor 13 through the microwave intrusion prevention pipe 51. Then, the liquid level level position may be measured by converting the pressure into the liquid level level position. In addition, as a method of measuring the pressure, for example, there are a method using a pressure sensor, a method of measuring the pressure of the bubbles when the bubbles are discharged into the contents 20, and the like. The pressure may be measured using other methods.

(2-2) Method Using Float As shown in FIG. 3B, the detection unit 52 includes a tubular member 52e, a float 52c that floats on the liquid level of the content in the tubular member 52e, and the position of the float 52c. And a float detection sensor 52d for detecting. In FIG. 3B, the detection part 52 and the reactor 13 have shown the internal structure simplified. The tubular member 52e is the same as the tubular member 52a described above, and extends in the vertical direction in the same range as the liquid level level position of the reactor 13. Moreover, the float 52c has a magnet, for example, and the float detection sensor 52d may be a sensor capable of detecting the position of the magnet, for example, a reed switch. The position of the float 52c detected by the float detection sensor 52d is the liquid level level measured by the detection unit 52. Note that the liquid level level detection using the float 52c may be performed by a method other than using a magnet. For example, the position of the float 52c corresponding to the liquid level level position may be detected by a change in resistance, or the liquid level level position may be measured by fixing the float 52c and measuring the buoyancy of the float 52c. Well (using the fact that the buoyancy increases as the range of the float 52c below the liquid level increases), the position of the float 52c corresponding to the liquid level level position may be detected using the amount of received light ( For example, the liquid level level measurement using the float 52c may be performed by other methods.

(2-3) Method Using Light In a tubular member 52e similar to FIG. 3B, a plurality of sets of a light emitting unit and a light receiving unit that receives light emitted from the light emitting unit are arranged in the vertical direction, like the sensor 52d. Prepare. The contents are positioned between the light emitting unit and the light receiving unit. Then, since the amount of received light is different between the case where the contents are present and the case where the contents are not present, the liquid level level position of the contents can be detected based on the difference. In addition, as a method using light, there is also a method of continuously measuring the liquid level level position using an optical fiber (for example, see JP-A-2006-47018). Further, the liquid level position using light may be measured by other methods.

(2-4) Method Using Ultrasonic Wave In the tubular member 52e similar to FIG. 3B, the liquid level level position may be measured using ultrasonic waves. As a method for measuring the liquid level level position using the ultrasonic wave, for example, a reflection type measurement method and a transmission type measurement method are known. Either of them may be used. Further, the liquid level position measurement using ultrasonic waves may be performed by other methods.

(2-5) Method Using Thermistor In the tubular member 52e similar to FIG. 3B, a plurality of thermistors are provided in the vertical direction in the same manner as the sensor 52d. Since the contents and air have different thermal conductivities, the heat dissipation efficiency of the thermistor differs depending on whether the thermistor is in contact with the contents or not. Therefore, the electrical resistance when power is supplied to the thermistor differs between the thermistor above the liquid level and the thermistor below the liquid level. Therefore, by using the difference in electric resistance, it is possible to specify the position of the thermistor where the liquid level is, and the liquid level level position can be measured. Further, the liquid level level measurement using a thermistor may be performed by other methods.

(2-6) Method Using Changes in Electrical Conductivity and Impedance In the tubular member 52e similar to FIG. 3B, a plurality of measuring devices for electrical conductivity and impedance are provided in the vertical direction, similar to the sensor 52d. Since the electric conductivity and impedance differ between the contents and air, the electric conductivity measured by the measuring instrument differs depending on whether or not the measuring instrument is in contact with the contents. Therefore, the electrical conductivity and the like are different between the measuring device above the liquid level and the measuring device below the liquid level. Therefore, by using the difference in the electric conductivity or the like, it is possible to specify the position of the measuring device where the liquid level is, and the liquid level level position can be measured. Further, the liquid level level position may be measured using a change in electrical conductivity or impedance by other methods.

  Although several methods for automatically measuring the liquid level level have been described here, it goes without saying that other methods may be used. For example, in each level of the tubular member 52e similar to FIG. 3B, the stirring member is rotated, whether or not there is resistance to the rotation is detected, and whether the position is in the liquid or not is detected. The liquid level level position may be measured or other methods may be used. Moreover, the material which comprises the detection part 52 is not ask | required. It may be microwave transmissive, microwave absorptive, microwave reflective, or any combination of two or more thereof Good.

  Further, when the detection unit 52 automatically measures the liquid level level as described above, the measured liquid level position may be displayed by the output unit 53 as shown in FIG. 3B. Good. Further, the output unit 53 may perform output other than display. Specifically, the output unit 53 may store information indicating the measured liquid level level position in a recording medium (not shown), may be transmitted to another device, or may be printed. Audio output may be performed, or other output may be performed. The output unit 53 may include hardware for performing output (for example, a display device, a transmission device, a printer, or the like), or may be a driver that drives them.

  Moreover, although FIG. 1 shows the case where the microwave intrusion prevention pipe 51 is connected to the upstream position of the reactor 13, this need not be the case. Needless to say, the microwave intrusion prevention pipe 51 may be connected to the midstream position of the reactor 13 or the downstream position.

  FIG. 4 is a diagram showing an example of the internal structure of the reactor 13 according to the present embodiment. In FIG. 4, the reactor 13 is partitioned into a plurality of chambers 31, 32, 33, and 34 by a partition plate 21. The plurality of chambers 31 to 34 are chambers continuous in series. As described above, the unfilled space 22 exists above the reactor 13. The unfilled space 22 is irradiated with the microwave generated by the microwave generator 14 through the waveguide 15. FIG. 4 shows a case where a single unfilled space 22 exists inside the reactor 13, that is, a case where the unfilled space 22 is shared by all the chambers 31 to 34, but this is not the case. May be. That is, the unfilled space 22 may be shared in at least some of the two or more chambers among all the chambers, or may not be shared in all the chambers (in this case, each The unfilled space 22 is divided by the partition plate 21). The position of the reactor 13 to which each waveguide 15 is connected does not matter. For example, the waveguide 15 may be provided at a position near the center of each chamber, may be provided at the position of the partition plate 21, or may be at another position. In addition, since the microwave propagates through the unfilled space 22, for example, the microwave transmitted by the waveguide 15 at the position of the chamber 31 irradiates the contents of the chamber 32 and the chamber 33 through the unfilled space 22. Will be. In addition, by providing the waveguide 15 at the position of the partition plate 21, that is, at a position above the partition plate 21, the microwave transmitted to the unfilled space 22 by the one waveguide 15 is transmitted to the waveguide. The two chambers separated by the partition plate 21 at the position corresponding to 15 are mainly irradiated. In addition, when the unfilled space 22 is shared by a plurality of chambers, the microwaves transmitted to the shared unfilled space 22 are transmitted from the plurality of chambers sharing the unfilled space 22. The contents 20 are irradiated. The partition plate 21 may be microwave transmissive, microwave absorptive, or may reflect microwaves. Examples of the material that transmits microwaves include Teflon (registered trademark), quartz glass, ceramic, and silicon nitride alumina. Therefore, the microwave-permeable partition plate 21 may be made of such a material that transmits microwaves. Examples of materials that absorb microwaves include carbons other than fullerene. Accordingly, the microwave-absorbing partition plate 21 may be made of a material that absorbs such microwaves. Moreover, as a material which reflects a microwave, there exists a metal, for example. Therefore, the partition plate 21 that does not transmit microwaves may be made of a material that reflects such microwaves. Moreover, the partition plate 21 may be comprised by the combination of arbitrary 2 or more materials among a microwave transparent material, a microwave absorptive material, and a microwave reflective material.

  The content 20 such as the raw material that has entered the reactor 13 flows between the chambers 31 to 34 and is finally output from the downstream (the right end of the reactor 13 in FIG. 4). The partition plate 21 has a flow path through which the contents flow. The flow path is a flow path in which the contents mainly flow from the upstream side (left side in FIG. 4) to the downstream side (right side in FIG. 4) of the reactor 13, but as indicated by the arrows in FIG. In addition, a part may flow from the downstream side to the upstream side. The flow path of the partition plate 21 may be, for example, a flow path in which the content overflows above the partition plate 21, or may be a flow path in which the content flows in a gap between the partition plates 21. 5A to 5F are views of the partition plate 21 provided in the cylindrical reactor 13 as seen from the length direction of the reactor 13. In the case of the former overflow channel, for example, as shown in FIGS. 5A and 5B, the partition plate 21 does not exist at the position of the unfilled space 22, and the position (that is, above the partition plate 21) is the content. Things may flow. In that case, as shown in FIG. 5B, a recess 41 through which the contents flow may be provided on the upper side of the partition plate 21. In that case, for example, even if the liquid level of the content 20 is at the same level as the upper side of the partition plate 21, the content circulates through the notch (notch) of the recess 41. In addition, the shape of the recessed part 41 is not ask | required. FIG. 5B shows a case where the concave portion 41 is semicircular, but the cut shape of the concave portion 41 may be, for example, a triangle, a rectangle, a trapezoid, or Other shapes may be used. Further, the number of the concave portions 41 is not limited. For example, the number may be one as shown in FIG. 5B or may be plural. In the case of the latter gap flow path, for example, as shown in FIG. 5C, a gap 27 may exist between the partition plate 21 and the inner wall of the reactor 13, and as shown in FIG. There may be a gap 27 in 21 itself. The size of the gap 27 is preferably larger than the content can be circulated. The shape and number of the gaps 27 are not limited. Although FIG. 5C shows a case where the gap 27 has an annular shape, the shape of the gap 27 may be, for example, a C shape in which a part of the annular ring is closed. 5D illustrates the case where the gap 27 is circular, the shape of the gap 27 may be, for example, a triangle, a rectangle, or other shapes. Further, the number of the gaps 27 may be larger or smaller than that in FIG. 5D, for example (one or more). Further, as shown in FIG. 5E and FIG. 5F, the overflow channel and the channel of the gap 27 of the partition plate 21 may be combined. The reactor 13 may or may not have a slope that decreases from the upstream side toward the downstream side. 5A, FIG. 5B, FIG. 5E, and FIG. 5F show the partition plate when the unfilled space 22 is shared by the two chambers partitioned by the partition plate 21, the unfilled space 22 is shown in FIG. When not shared, the partition plate 21 may also exist at the position of the unfilled space 22. In addition, when the reactor 13 has a shape other than the cylindrical shape, it goes without saying that the shape of the partition plate 21 according to the shape is obtained. Further, when there are a plurality of partition plates 21 in the reactor 13, the partition plates 21 may or may not have the same shape.

  Further, as shown in FIG. 4, the chemical reaction apparatus 1 may further include a stirring unit 23. That is, the chemical reaction apparatus 1 according to the present embodiment may also have one or more stirring means 23 for rotating and stirring the contents 20 in the reactor 13. Although FIG. 4 shows a case where the stirring means 23 is present in each of the chambers 31 to 34, this need not be the case. The stirring means 23 may not be present in one or more chambers. In addition, FIG. 4 shows a case where the stirring means 23 has a blade-like shape, but this schematically shows the stirring means 23, and the stirring is performed, for example, in a blade-like shape, a wing-like shape, or The rod-shaped rotating member may be rotated. The rotating member may be a microwave transmissive member, a microwave absorbing member, a microwave reflecting member, or a microwave transmitting material, It may be constituted by a combination of any two or more materials among a microwave absorbing material and a microwave reflecting material. The rotation may be performed, for example, by rotating a rotating member attached to the shaft according to the rotation of the shaft, or even if the rotating member is rotated using magnetism, such as a magnetic stirrer. Good. In the former case where a shaft is used, the shaft may be independent for each chamber, or may be commonly used in a plurality of chambers. In the latter case using magnetism, a rotating member (magnetic stirrer) such as a rod shape, a blade shape, or a wing shape is rotated by a magnet. It should be noted that the stirring of the contents by the stirring means 23 may or may not be used to flow the contents in the upstream to downstream direction or the reverse direction. In addition, about rotation stirring, it is already well-known and those detailed description is abbreviate | omitted. In addition, when the chemical reaction apparatus 1 includes the stirring unit 23, it is preferable that the microwave intrusion prevention pipe 51 is connected to a location that is not at a position where the contents can be flowed by the stirring unit 23. This is because if the contents flow into the microwave intrusion prevention pipe 51 by the stirring, the liquid level level position may not be detected accurately.

  Here, the reason why the stirring means 23 rotates and stirs the contents of the reactor 13 will be briefly described. The first reason that the stirring means 23 stirs the contents is to heat the contents uniformly by the microwave. Although it depends on the type of contents and the temperature of the contents, the depth of penetration of a certain microwave is fixed, so that the entire contents are uniformly irradiated with microwaves and stirred so that they are heated uniformly. Will do. Moreover, if the surface area of the content in the unfilled space 22 becomes large, it becomes possible to irradiate the content more efficiently. Therefore, the second reason for stirring the contents is to increase the microwave irradiation area. Therefore, it is preferable that the stirring of the contents by the stirring means 23 is so intense that a wave is generated on the surface of the contents in the unfilled space 22, but this need not be the case (for the first reason). This is because if the corresponding stirring is performed, the entire contents are heated as a result, which may be sufficient). In addition, since the raw material is stirred using the stirring means 23 as described above, even when two or more substances having different densities are contained in the raw material, both are appropriately mixed and reacted. Will be able to. For example, in a vertical flow type reactor, even if alcohols and waste oils having different densities are reacted, they are easily separated. If the stirring means 23 is present, both can be appropriately mixed and reacted.

  As shown in FIG. 4, the reactor 13 may also include a temperature measurement unit 25. That is, the chemical reaction device 1 according to the present embodiment may include a temperature measurement unit 25 that measures the temperature inside the reactor 13. The temperature inside the reactor 13 is preferably the temperature of the contents of the reactor 13. Although FIG. 4 shows a case where the temperature measuring unit 25 is present in each of the chambers 31 to 34, this need not be the case. The temperature measuring unit 25 may not be present in one or more chambers. 4 schematically shows the temperature measurement unit 25, the temperature measurement unit 25 may measure the temperature with a thermocouple, the temperature with an infrared sensor, or the optical fiber, for example. The temperature may be measured by, or the temperature may be measured by other methods. The temperature measured by the temperature measuring unit 25 (strictly speaking, it is data indicating temperature) is passed to the microwave control unit 16 and used for controlling the microwave output by the microwave generator 14. The control is for maintaining the temperature of each of the chambers 31 to 34 at a desired temperature or a desired temperature range as described above. For example, as shown in FIG. 4, when microwaves are irradiated to the position of the partition plate 21, the control of the output of the microwaves irradiated to that position is performed, for example, at the position where the microwaves are irradiated. Of the temperatures of the two chambers separated by the partition plate 21, the temperature may be determined using one or both. In the former case, for example, control may be performed using a lower temperature, control may be performed using a higher temperature, or control may be performed using a predetermined room temperature. You may go. In the latter case, for example, the control may be performed using the average of both.

  In the reactor 13 of the present embodiment, the level position of the liquid level of the content 20 is not limited. 5C to 5F, when the gap 27 exists, the height of the liquid level is determined by the position of the outflow hole through which the product etc. flows out from the reactor 13. . Therefore, the position of the outflow hole may be provided at a position corresponding to the desired liquid level. That is, the position of the outflow hole of the reactor 13 may be set so that a desired unfilled space 22 can be secured. On the other hand, when the raw material or the like overflows as in the partition plate 21 in FIGS. 5A and 5B, the liquid level in the chambers 31 to 33 other than the most downstream chamber 34 depends on the height of the partition plate 21. (In this case also, the height of the liquid level in the most downstream chamber 34 is determined by the position of the outflow hole). Therefore, the partition plate 21 having a height corresponding to the desired liquid level may be provided inside the reactor 13. That is, the height (position) of the overflow channel in the partition plate 21 may be set so that a desired unfilled space 22 can be secured. Needless to say, the height of the liquid level of the content 20 and the height of the unfilled space 22 are not limited to those described above as long as the content 20 can be appropriately irradiated with microwaves.

Moreover, the shape of the reactor 13 is not ask | required. For example, as shown in FIGS. 2A, 3A, and 3B, the reactor 13 may have a cylindrical shape whose length direction is the left-right direction in FIG. 4, or a rectangular parallelepiped shape. Alternatively, other shapes may be used. When the reactor 13 is a rectangular parallelepiped, the microwave intrusion prevention tube 51 may be connected to the reactor 13 as shown in FIG. 2B, for example. In the present embodiment, the case where the reactor 13 is cylindrical will be mainly described. 5A to 5F also show the partition plate 21 when the reactor 13 is cylindrical as described above.
The wall surface of the reactor 13 may be covered with a heat insulating material. By doing so, it is possible to prevent the heat inside the reactor 13 from being released to the outside.

  Next, operation | movement of the chemical reaction apparatus 1 by this Embodiment is demonstrated easily. The raw material and the catalyst are supplied to the mixing unit 12 by the pump 11. And it mixes in the mixing part 12, and is thrown into the reactor 13. FIG. The supply speed of the raw material or the like to the reactor 13 may be determined in advance.

  The raw material or the like supplied to the reactor 13 flows from the upstream side to the downstream side while being stirred by the stirring means 23. At that time, the microwave generated by the microwave generator 14 is transmitted to the unfilled space 22 of the reactor 13 through the waveguide 15 and irradiated to the raw material or the like. As a result, the raw material and the like are heated, and the reaction of the raw material and the like is promoted. In addition, the temperature of each chamber 31-34 is measured by the temperature measurement part 25, and is passed to the microwave control part 16 by the path | route which is not shown in figure. And the microwave control part 16 controls the output of the microwave generator 14 so that the temperature of each chamber 31-34 may become desired temperature or a desired temperature range. Further, the liquid level level position in the reactor 13 can be detected by the detection unit 52. Therefore, for example, when some inconvenience occurs and the liquid level level is lowered or raised, the microwave irradiation may be stopped to eliminate the inconvenience. By doing so, stable microwave irradiation can be realized.

  The product output from the reactor 13 is input to the catalyst separation unit 17 to separate the catalyst. Then, the product from which the catalyst is separated is introduced into the treatment liquid storage tank 18 by the pump 11, and is divided into a target product and a by-product in the treatment liquid storage tank 18. In this way, the final product is obtained. In addition, by repeatedly executing such processing, target products are sequentially generated.

  The catalyst separation process in the catalyst separation unit 17 and the product and by-product separation process in the treatment liquid storage tank 18 may be performed sequentially each time the product is added, or It may be carried out in a lump after the charged product has accumulated a certain amount. That is, the processing in the reactor 13 is processed by a flow method (flow type), but the processing in the subsequent catalyst separation unit 17 and the processing liquid storage tank 18 may be processed by a flow method or by a batch method. May be processed.

  In addition, the chemical reaction performed in the chemical reaction apparatus 1 according to the present embodiment is anything as long as it is a microwave reaction itself or a chemical reaction caused by heating according to the microwave irradiation. Also good. For example, biodiesel fuel may be generated by esterification or transesterification, ink raw material that is an ester, or other chemical reaction may be used.

  Next, the process which produces | generates biodiesel fuel (fatty acid methyl ester) from waste oil using the chemical reaction apparatus 1 by this Embodiment is demonstrated using an Example. Needless to say, the present invention is not limited to the examples.

(Example of reaction system construction)
In this example, as a raw material, a mixture of fats and oils and free fatty acids and alcohol were used. Alcohol is a reactant. The raw material and the catalyst are respectively sent to the mixing unit 12 by the pump 11 and mixed uniformly. The mixed solution is supplied to the reactor 13. The mixed liquid in the reactor 13 is irradiated with microwaves generated from the microwave generator 14 to promote the esterification reaction. Further, the mixed liquid in the reactor 13 is filled in the chambers 31 to 34 partitioned by the partition plate 21 in the reactor 13. The reaction proceeds by microwave irradiation while the mixed solution is stirred by the stirring means 23 together with the catalyst. The microwave is applied to the unfilled space 22 existing inside the reactor 13 and diffuses into the reactor 13. The reaction solution in each chamber moves to the next chamber through a flow path provided in the partition plate 21. The reaction liquid is discharged out of the reactor 13 after maintaining a certain residence time in the reactor 13. The mixed liquid after the reaction discharged from the reactor 13 is supplied to the catalyst separation unit 17, where the catalyst is separated and filled into the treatment liquid storage tank 18. The reaction liquid after the catalyst separation is separated from the by-product water and glycerin in the treatment liquid storage tank 18, and the target crude methyl ester is taken out.

(Esterification reaction of industrial waste oil)
The typical example of esterification reaction of free fatty acid using industrial waste oil is shown. Industrial waste oil containing 34 wt% of free fatty acid (containing other triglycerides, pitch components, etc.) and 2.8 molar equivalents of methanol as a reactant (moles when converting free fatty acids of industrial waste oil to oleic acid And 3 wt% of the solid acid catalyst (which is the weight% with respect to industrial waste oil) was mixed in the mixing unit 12 and then supplied to the reactor 13. The feed rate to the reactor 13 was about 1.2 / h at the space velocity shown below. Here, the reactor capacity is a capacity obtained by subtracting the capacity of the unfilled space 22 from the total capacity in the reactor 13 in this embodiment.
(Space velocity) = (Volume flow rate of waste oil) / (Reactor capacity)

The microwave output of the reactor 13 was feedback-controlled by the internal temperature of each chamber 31 to 34, and the temperature of each chamber 31 to 34 was kept constant. In this experiment, the reaction temperature was set to 70 ° C. FIG. 6 shows the conversion rate of fatty acid methyl ester by the esterification reaction of fatty acid and methanol in this example. The formula for calculating the methyl ester conversion is as follows.
Methyl ester conversion (%) = [methyl ester concentration] / [fatty acid initial concentration] × 100

  As is apparent from FIG. 6, the esterification reaction proceeded rapidly after the start of the reaction, and the conversion reached 87% in 30 minutes. Thereafter, the conversion gradually increased, and the reaction almost reached equilibrium in 1.5 hours. In addition, the other components in the waste oil were not particularly changed. From this result, it is possible for the esterification reaction by the flow reactor according to the present embodiment to efficiently carry out the esterification reaction on the free fatty acids in the waste oil and continuously carry out a stable reaction. I understand that.

  As described above, according to the chemical reaction device 1 according to the present embodiment, the contents can be efficiently irradiated to the contents in the reactor 13. As a result, the chemical reaction inside the reactor 13 can be promoted. In particular, by rotating and stirring the contents inside the reactor 13 using the stirring means 23, even when the penetration depth of the microwave is not so deep, the contents are evenly irradiated with microwaves. Can become possible. Further, since the reactor 13 is divided into a plurality of chambers, the contents react while staying in the respective chambers, so that the contents can be effectively irradiated with microwaves in each chamber. It becomes like this. As a result, it can be avoided that unreacted raw material is output from the reactor 13 (that is, the raw material is short-circuited from the inflow hole of the reactor 13 to the outflow hole). In addition, when the solid catalyst has microwave absorptivity and microwave sensitivity, the solid catalyst is efficiently heated by the microwave irradiation, which may promote a chemical reaction in the vicinity of the solid catalyst. it can. As described above, the chemical reaction inside the reactor 13 is promoted, so that the product can be obtained more efficiently.

  Further, by using the microwave intrusion prevention tube 51 and the detection unit 52, the liquid level level position of the contents of the reactor 13 can be easily known. As a result, if the liquid level level deviates from the expected range, microwave irradiation is stopped, the cause is investigated, and the cause is removed, thereby continuing a stable chemical reaction. Will be able to. In addition, since the reactor 13 is irradiated with microwaves, there is a demand that it is desirable not to provide unnecessary objects inside the reactor 13 as much as possible. Therefore, by detecting the liquid level level via the microwave intrusion prevention pipe 51, the liquid level level can be detected without affecting the microwave irradiation inside the reactor 13. become. Further, by detecting the liquid level level of the contents through the microwave intrusion prevention pipe 51, it is possible to reduce the influence of the microwave on the detection of the liquid level level. .

  In addition, although FIG. 4 demonstrated the case where the stirring means 23 existed for every chamber, it may not be so. In a plurality of chambers, a single or a plurality of stirring means 23 may be present. When the chemical reaction apparatus 1 has the single stirring means 23, as mentioned above, the stirring means 23 may have a shaft (rotating shaft) that is commonly used in a plurality of chambers. . In that case, the stirring means 23 may include a rotating shaft, a plurality of rotating members, and a rotating means. The rotation axis is an axis extending in the flow direction of the reactor 13. For example, in FIG. 4, the rotation axis may extend from the left end surface of the reactor 13 to the right end surface. The rotation axis may be provided in parallel to the bottom surface of the reactor 13. This rotating shaft may be made of, for example, a microwave permeable material, may be made of a microwave absorbing material, or may be made of a microwave reflective material. Or a combination of any two or more of these materials. As described above, the rotating member may be, for example, a blade-shaped member, or may be a wing-shaped member, a rod-shaped member, or the like. Further, the rotating member may or may not be present in each chamber. There may be a chamber in which no rotating member exists. Two or more rotating members may exist in one chamber. The stirring means 23 only needs to have at least one rotating member. Further, the rotating means rotates each rotating member. When the rotating member is fixed to the rotating shaft, the rotating means may rotate the rotating shaft. In that case, the rotating means may be, for example, a motor or an engine. Further, the rotation shaft may rotatably support the rotation member, and the rotation shaft itself may not rotate. In that case, for example, the rotating means may rotate a rotating member having a magnet by a magnetic force. Specifically, in the same manner as a motor of a type that rotates a rotor (rotor), which is a permanent magnet, with an electromagnet stator (stator) provided around the rotor, a rotating member (rotor) You may rotate by a rotation means (stator). In this case, it is preferable that the rotating means that is a stator exists outside the reactor 13, but this need not be the case. This is because, depending on the material of the reactor 13, the rotating means that is a stator may not be provided outside the reactor 13. In addition, when the stirring means 23 has a rotation shaft extending over a plurality of chambers, the partition plate 21 may have a hole through which the rotation shaft passes, or a concave position or a gap 27 that is a flow path. The rotating shaft may pass through the position.

  In the present embodiment, the liquid level level of the contents may be detected using the microwave intrusion prevention tube 51 and the detection unit 52 for two or more chambers of the reactor 13. . At that time, the liquid level level may be detected for all the chambers, or the liquid level level may be detected for some of the chambers. In the latter case, for example, the liquid level level detection may be performed for the most upstream chamber and the most downstream chamber, or for other combinations of two or more chambers. The detection of the liquid level level position may be performed.

  Moreover, in this Embodiment, the number of the rotating shafts and rotating means which the stirring means 23 has is not ask | required. For example, one or more rotating members may be rotated by a single rotating shaft or rotating means, or two or more rotating members may be rotated by using two or more rotating shafts or two or more rotating means.

  Moreover, although the case where the mixing unit 12 that mixes the raw material and the catalyst is described in the present embodiment, this need not be the case. For example, when a raw material and a catalyst mixed in advance are used, when mixing is also performed in the reactor 13, a solid catalyst flowing in the reactor 13 remains in the reactor 13, or a solid catalyst flowing in the reactor 13 In the case where a fixed bed solid catalyst is used instead, the chemical reaction apparatus 1 may not include the mixing unit 12. When a fixed bed solid catalyst is used, the fixed bed solid catalyst usually exists inside the reactor 13. For example, the solid catalyst of the fixed bed may be affixed to the inner wall of the reactor 13 or may be fixed by being packed in a catalyst packed bed or a column inside the reactor 13. There may be. The shape of the solid catalyst is, for example, amorphous granular, cylindrical (which may or may not be hollow), spherical, pellet, ring, shell, honeycomb, foam, It may be a fiber, cloth, plate, or other shape.

  Moreover, although this Embodiment demonstrated the case where the some chambers 31-34 were comprised by the inside of the reactor 13 being partitioned off with a partition plate, it may not be so. That is, the reactor 13 may have a single chamber. Further, when the reactor 13 has a plurality of chambers continuous in series, the number of the chambers is not limited. Usually, the larger the number of chambers, the more effectively the raw material can be prevented from flowing short-circuiting from the inflow hole of the reactor 13 to the outflow hole.

  Moreover, although this Embodiment demonstrated the case where the some microwave generator 14 was provided, it may not be so. For example, as shown in FIG. 7, the microwave generated by the microwave generator 14 may be transmitted to a plurality of locations by a waveguide 15 having a branch. The plurality of locations may be, for example, a plurality of chambers. FIG. 7 shows the case where the chemical reaction apparatus 1 includes only one microwave generator 14, but when the chemical reaction apparatus 1 includes two or more microwave generators 14, Microwaves generated by any of the plurality of microwave generators 14 may be transmitted to a plurality of locations by the waveguide 15 having branches. For example, when the microwaves generated by the microwave generator 14 are transmitted to a plurality of chambers, the microwave control unit 16 causes each chamber to which the microwaves generated by the microwave generator 14 are transmitted. Any or all of these temperatures may be used to control the output of the microwave generator 14. For example, the microwave control unit 16 may perform control using an average of all temperatures in each room, or may perform control using the maximum value or the minimum value of the temperature in each room.

  Moreover, although the case where the chemical reaction apparatus 1 includes the temperature measurement unit 25 and the microwave control unit 16 has been described in the present embodiment, this need not be the case. For example, when the temperature of the reactor 13 can be maintained at a desired temperature or temperature range by setting the microwave output to a predetermined value, the microwave output control using the temperature is performed. It is not necessary to perform.

  In the present embodiment, the case where the catalyst separation unit 17 is provided in the subsequent stage of the reactor 13 has been described, but this need not be the case. When the catalyst is separated by another device, or when the solid catalyst flowing in the reactor 13 remains in the reactor 13, when a solid catalyst in a fixed bed is used instead of the solid catalyst flowing in the reactor 13, In the case where it is not necessary to separate the catalyst in the chemical reaction apparatus 1 according to the present embodiment as in the case where no catalyst is used for the chemical reaction, the catalyst separation unit 17 may not be provided.

  In the present embodiment, the case where the raw material and the catalyst are mixed and put into the reactor 13 has been described, but this need not be the case. For example, only the raw material may be charged into the reactor 13. In addition, when the raw material and the catalyst are not mixed, only the raw material may flow through the reactor 13. That is, the content of the reactor 13 may be, for example, a mixture of a plurality of raw materials. Even when the raw material and the catalyst are not mixed, for example, when the solid catalyst flowing in the reactor 13 remains in the reactor 13, the raw material and the catalyst may flow through the reactor 13. Good. Moreover, when mixing of a raw material and a catalyst is not performed, the mixing part 12 may mix a raw material, for example, or may mix a raw material (substrate) and a reactive agent. Moreover, when mixing of the raw material etc. is unnecessary, the chemical reaction apparatus 1 does not need to be provided with the mixing part 12 as mentioned above.

  Moreover, although this Embodiment demonstrated the case where the 1 or more stirring means 23 which stirs the raw material in the reactor 13 was provided, it may not be so. For example, when the reactor 13 is configured to easily irradiate the entire raw material with microwaves (for example, when the inner diameter of the reactor 13 is small), the stirring means 23 may not be provided.

  Moreover, although the case where the chemical reaction apparatus 1 includes the treatment liquid storage tank 18 has been described in the present embodiment, this need not be the case. For example, with respect to a mixture of products and by-products output from the chemical reaction device 1, the product may be extracted in another device.

  In the present embodiment, the chemical reaction apparatus 1 includes two or more microwave generators 14, and the two or more microwave generators 14 may generate microwaves having two or more frequencies, respectively. Good. That is, the contents of the reactor 13 may be irradiated with microwaves having two or more frequencies. In that case, microwaves of two or more frequencies may be irradiated at the same position, and microwaves of two or more frequencies may be irradiated at different positions. For example, as shown in FIG. 8A, microwaves having the frequencies X and Y generated by the microwave generators 14 a and 14 d may be irradiated at the same position of the reactor 13, that is, in the midstream region of the reactor 13. Note that the microwaves of the frequencies X and Y are transmitted to the reactor 13 via the waveguides 15a and 15d, respectively. Further, for example, as shown in FIG. 8B, the microwave of the frequency X generated by the microwave generators 14 a, 14 b and 14 c is irradiated from the upstream side of the reactor 13 to the midstream region, and on the downstream side of the reactor 13, You may irradiate the microwave of the frequency Y which 14d of microwave generators generate | occur | produced. Note that the microwaves having the frequency X are transmitted to the reactor 13 via the waveguides 15a, 15b, and 15c, respectively. Further, the microwave of frequency Y is transmitted to the reactor 13 via the waveguide 15d. Here, FIGS. 8A and 8B are views of the reactor 13 as viewed from above, and the arrows in the drawings indicate the flow of contents in the reactor 13. When microwaves with two or more frequencies are irradiated, the number of frequencies may be two, or three or more. The two or more frequencies may be any combination as long as they are two or more frequencies selected from the range of 300 MHz to 300 GHz. For example, when microwaves of two frequencies are irradiated, the combination of the frequencies may be 2.45 GHz and 5.8 GHz, may be 2.45 GHz and 24 GHz, and may be 2.45 GHz. It may be 913 MHz, 5.8 GHz and 24 GHz, 5.8 GHz and 913 MHz, or 24 GHz and 913 MHz. Moreover, when irradiating the microwave of 2 or more frequencies, the timing which irradiates them does not ask | require. For example, microwaves having two or more frequencies may be irradiated at the same time, or microwaves may be irradiated so that the period of irradiation differs for each frequency. For example, in the latter case, the microwave of the frequency X may be irradiated in a certain period, and the microwave of the frequency Y may be irradiated in the next period. When microwaves with two or more frequencies are irradiated, microwaves are also applied to substances that are not subjected to microwave action (for example, heating) by microwave irradiation with one frequency. Therefore, microwaves can be applied to a wider material. In addition, when irradiating the contents with microwaves having two or more frequencies, it is preferable that the microwave intrusion prevention tube 51 has an attribute capable of preventing the penetration of the microwaves having two or more frequencies. . For example, a microwave intrusion prevention tube 51 that is a tube having a cutoff frequency larger than the highest frequency among the plurality of frequencies may be used. Further, for example, the length of the microwave intrusion prevention tube 51 considering the attenuation in the microwave invasion prevention tube 51 may be determined using the largest frequency among the plurality of frequencies. Further, the degree of coupling is calculated using the plurality of frequencies, and the cross-section of the microwave intrusion prevention tube 51 is set so that the largest degree of coupling is not more than a desired value (for example, −10 (dB)). You may make it determine a magnitude | size and length.

  Further, in the above embodiment, information such as threshold values, mathematical formulas, addresses, etc. used by each component in the processing is temporarily stored in a recording medium (not shown) even if it is not specified in the above description. Alternatively, it may be held for a long time. Further, the storage of information in the recording medium (not shown) may be performed by each component or a storage unit (not shown). Further, reading of information from the recording medium (not shown) may be performed by each component or a reading unit (not shown).

  In the above embodiment, when information used by each component, for example, information such as a threshold value, an address, and various setting values used by each component may be changed by the user Even if it is not specified in the above description, the user may be able to change the information as appropriate, or it may not be. If the information can be changed by the user, the change is realized by, for example, a not-shown receiving unit that receives a change instruction from the user and a changing unit (not shown) that changes the information in accordance with the change instruction. May be. The change instruction received by the receiving unit (not shown) may be received from an input device, information received via a communication line, or information read from a predetermined recording medium, for example. .

  In the above embodiment, each component may be configured by dedicated hardware, or a component that can be realized by software may be realized by executing a program. For example, each component can be realized by a program execution unit such as a CPU reading and executing a software program recorded on a recording medium such as a hard disk or a semiconductor memory.

  Further, the present invention is not limited to the above-described embodiment, and various modifications are possible, and it goes without saying that these are also included in the scope of the present invention.

  As described above, according to the chemical reaction device of the present invention, the effect of being able to know the liquid level level position in the reactor is obtained, and it is useful as a chemical reaction device that performs a chemical reaction by irradiating microwaves.

DESCRIPTION OF SYMBOLS 1 Chemical reactor 12 Mixing part 13 Reactor 14, 14a-14d Microwave generator 15, 15a-15d Waveguide 16 Microwave control part 17 Catalyst separation part 18 Process liquid storage tank 20 Contents 21 Partition plate 23 Stirring means 25 Temperature measurement unit 51 Microwave intrusion prevention tube 52 Detection unit

Claims (10)

A horizontal flow reactor in which the liquid content flows horizontally with an unfilled space above;
A microwave generator for generating microwaves;
One or more waveguides for transmitting the microwave generated by the microwave generator to an unfilled space of the reactor;
A microwave intrusion prevention pipe which is connected to the reactor and is a pipe through which the contents can circulate, and which has an attribute capable of preventing the microwave intrusion generated by the microwave generator;
A chemical reaction device comprising: a detection unit capable of detecting a liquid level level of the content in the reactor through the content in the microwave intrusion prevention tube. The chemical reaction device according to claim 1, wherein the detection unit is a liquid level gauge that can detect the liquid level level visually. The chemical reaction apparatus according to claim 1, wherein the detection unit measures the liquid level level position. The chemical reaction device according to any one of claims 1 to 3, wherein the microwave intrusion prevention tube is a tube having a cutoff frequency higher than a frequency of a microwave generated by the microwave generator. The chemical reaction apparatus according to claim 4, wherein the microwave intrusion prevention tube is a tube having a length such that the intensity of the invaded microwave becomes 1/10 or less. The microwave penetration blocking tube is a tube having a length and a cross-sectional size in which the degree of coupling is −10 (dB) or less when the reactor is a main waveguide and the microwave penetration blocking tube is a sub-waveguide. The chemical reaction device according to claim 4 or 5, wherein The chemical reaction apparatus according to any one of claims 1 to 6, wherein the microwave intrusion prevention pipe is connected to the reactor at a lowermost part of the reactor. The chemical reaction device according to any one of claims 1 to 7, further comprising one or more stirring means for rotating and stirring the contents in the reactor. Two or more microwave generators,
The two or more microwave generators generate microwaves of two or more frequencies,
The chemical reaction device according to any one of claims 1 to 8, wherein the microwave intrusion prevention tube has an attribute capable of preventing intrusion of microwaves having the two or more frequencies. The reactor has a plurality of partition plates that divide the interior into a plurality of chambers,
The chemical reaction device according to any one of claims 1 to 9, wherein each partition plate includes a flow path through which contents flow from an upstream side to a downstream side.

Images