JP2000061291A - Reaction device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To make performable the uniform kneading or the continuous treatment of a high viscosity reaction object by providing an extruder with reaction object circulating mechanism and a temp. control mechanism. SOLUTION: The reaction device 1 is a biaxial extruder type reaction device having a barrel 2 and 2 screws 3, 3 arranged in parallel in the barrel 2. The screw 3 constituting the reaction object circulating mechanism in the reaction device 1 is formed by engaging a forward screw body 5a, a kneading screw body 5b, a reverse screw body 5c and a forward screw body 5a with a screw shaft center 4 having a hollow structure inside and arranging in order. The temp. control mechanism of the reaction device 1 is constituted of an electric heater provided outside of the barrel 2, a heating device by high temp. steam, a heating medium, electrical heating or the like and a cooling device by water cooling, air cooling, chiller cooling, liquid nitrogen or the like. Particularly the heating device by electrical heating easily performs the control of the temp.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a novel reaction apparatus, and more particularly to a reaction apparatus that can be used for chemical reaction, kneading and the like of highly viscous substances.

[0002]

2. Description of the Related Art A batch reactor is a reactor which is widely used for industrial purposes. This is a device that has a double-jacket structure and reacts while stirring the raw materials charged inside with stirring blades, etc., while mainly heating the reaction target with steam. However, when the viscosity of a reaction target such as a raw material or a reaction product is high, this reaction kettle has problems that uniform temperature cannot be controlled during the reaction, uniform stirring cannot be performed, and it takes time to discharge the product. . In addition, the reaction experimental apparatus has a problem that the reaction container is made of glass and cannot be applied to a pressure change or a reaction in which the amount of a substance changes before and after the reaction. Therefore, it is conceivable to use a twin-screw extruder or a kneader as a device for continuously treating such high-viscosity raw materials and products.

[0003]

However, the extruder and the kneader have the following problems, and a reactor capable of handling a high-viscosity raw material and capable of continuous treatment has not yet existed. 1) The residence time of the reaction target is from 30 seconds to about 6 minutes even when using a special die, and the reaction time cannot be long as a reaction device, so in many cases it cannot be used continuously. 2) In the high temperature range over 120 ° C, the twin-screw extruder also fluctuates by about ± 5 ° C and cannot be used in reactions that require strict temperature control. 3) The pressure of the twin-screw extruder can be operated from atmospheric pressure to about 100 atm, but the pressure is determined by the raw material blending, input amount, operating water, set temperature, die shape, screw combination, screw rotation speed, etc. However, its correlation is unclear and it is not used as a reactor.

Therefore, in order to enable a new chemical synthesis experiment and to effectively produce a new compound in the chemical field, while controlling the reaction time, temperature and pressure,
The advent of a new chemical reaction device capable of uniformly kneading and continuously treating a high-viscosity reaction target is desired.

The present invention has been made in order to solve such a problem, and provides a novel reaction apparatus capable of uniformly kneading and continuously treating a highly viscous reaction target by using an extruder. The purpose is to

[0006]

The reaction apparatus of the present invention is an extruder type reaction apparatus having a barrel and a screw provided in the barrel. It is characterized by comprising a reaction object circulation mechanism for circulation and a temperature control mechanism for controlling the temperature of the reaction object.

The present invention is further characterized by having a pressure control mechanism for applying pressure to the reaction target by changing the screw pattern and the screw rotation speed.

The reaction object circulation mechanism of the reaction apparatus is characterized in that the inside of the screw has a hollow structure and the reaction object is circulated in the hollow structure by the conveying force of the screw.

Another reaction object circulation mechanism is characterized in that the reaction object is circulated by the conveying force of the screw and the external circulation means.

The temperature control mechanism of the reaction apparatus is characterized in that the reaction target itself is heated by energization.

The screw provided in the barrel is characterized in that it is at least one connecting body selected from a screw body and a disc body fitted to the screw shaft core.

The reaction means a process in which another substance or substance group having a different composition / structure is produced from a certain substance or substance group. In the process, the reaction amount, reaction time, reaction temperature, reaction pressure are , Is an important parameter that defines the reaction. Particularly when the reaction target is a high-viscosity substance, it is difficult to sufficiently mix and disperse the substances, and it is also difficult to control the reaction temperature for a high-viscosity substance having a low thermal conductivity. The present inventor has found that by using an extruder, the reaction amount, reaction time, reaction temperature, reaction pressure can be controlled even with a highly viscous substance, and it can be used as a reactor. The present invention has been made based on such knowledge, and even if the reaction target is a high-viscosity substance, by providing the reaction target circulation system and the temperature control mechanism in the extruder, the reaction of the reaction target A reactor in which the time and temperature control can be adjusted arbitrarily is obtained. Further, by controlling the screw pattern and the screw rotation speed, the pressure on the reaction target can also be controlled. For this reason, the extruder, which has been conventionally used for only a maximum residence time of about 6 minutes even with a special die, can be used as a reaction apparatus capable of arbitrarily controlling the reaction temperature, time and pressure.

[0013]

BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the reaction apparatus of the present invention will be described with reference to FIG. FIG. 1 shows a cross-sectional view when the reaction object circulation mechanism is an internal circulation system. The reactor 1 and the barrel 2 are arranged in parallel in the barrel 2 in parallel.
It is a twin-screw extruder type reactor having three screws 3, 3. The barrel 2 has a cocoon shape as seen in a sectional view perpendicular to the screw axis, and two screws 3 and 3 are provided inside the cocoon shape. The two screws 3 and 3 may each rotate in the same direction or in different directions.

The structure of the screws 3 and 3 is shown in FIG. FIG. 2 is a perspective view of a screw, FIG. 2 (a) shows a screw shaft core and a connecting body fitted to the shaft core, and FIG. 2 (b) shows a screw. The screw 3 is composed of a connected body with at least one selected from a screw body 5 and a disc body 6 which are fitted to the screw shaft core 4. Further, a stop ring body (not shown) can be combined. The screw body 5 includes a forward screw body for advancing the reaction target in the barrel from the supply section 8 or a reverse screw body for retreating the reaction object. The disc body 6 is a kneading disc body for kneading / shearing the reaction target in the barrel by combining a plurality of disc pieces having the same or different thickness, a forward disc body for advancing, or a reverse disc for retreating. I have a body.

The screw body 5 and the disc body 6 will be described with reference to FIG. FIG. 3 is a perspective view of the screw body 5 and the disc body 6. The screw body 5 is a cylindrical body having a spiral concave-convex portion on the outer peripheral surface and a fitting groove with the screw shaft core 4 on the inner peripheral surface, and the conveyance amount of the reaction target can be controlled by the spiral pitch. (FIG. 3 (a)). The disc body 6 is formed by connecting a disc piece 6a having a convex portion 6b and a concave portion 6c to the circumferential surface.
That is, in the case where a plurality of disc pieces 6a are prepared and fitted and connected on the screw shaft core 4, the loci of every other convex portion 6b or concave portion 6c to which the screws are connected in a plan view are the axes. By sequentially disposing the disc pieces 6a so as to be parallel to the core, a kneading disc body having a kneading / shearing function can be obtained (FIG. 3).
(B)). In addition, the convex portion 6b or the concave portion 6 to be connected
By sequentially disposing the disc pieces 6a so that the locus of c has a predetermined angle with respect to the axis, a forward disc body or a reverse disc body can be obtained (FIG. 3C). Incidentally, even a kneading disk body can be made into a forward disk body or a reverse disk body by providing a taper on the circumferential surface of the disk piece 6a. In addition, the stop ring body,
Any shape may be used as long as it can suppress the transport amount of the reaction target.

The screw 3 transfers the reaction target in the barrel by connecting the screw body 5, the disc body 6 and the like and fitting them to the screw shaft core 4.
Any reaction state such as filling and pressurizing, kneading and the like can be used. In addition, these states can be arbitrarily combined. For example, in the case of the reaction apparatus 1 shown in FIG. 1, the screw 3 is fitted with a forward screw body 5a, a kneading screw body 5b, a reverse screw body 5c and a forward screw body 5a on a screw shaft core 4 having a hollow structure inside. They are arranged in order. The hollow structure inside the screw shaft core may be cylindrical or may be provided with a spiral groove on the inner surface of the cylinder to assist the circulation transfer of the reaction target.

As the material of the screw body 5 and the disk body 6, metal, plastics, ceramics or the like can be used according to the application. For example, by using a plastics material having a larger coefficient of thermal expansion such as metal, it is possible to design the screw 3 that has the minimum clearance with the barrel 2 at the set reaction temperature, and to improve the transportability of the reaction target. A reactor having is obtained. Further, in the case of a heating device by electric heating described later, insulating materials such as plastics and ceramics are preferable.

The reaction object circulation mechanism in the reaction apparatus 1 shown in FIG. 1 is constituted by a screw 3 having a hollow structure inside. Interlocking with the rotation of the screw 3, the reaction target 7 supplied from the supply unit 8 indicates an arrow A between the space between the screw 3 and the barrel 2 and the inside of the screw 3.
Cycle as shown in. As a result, the reaction target 7 is filled, pressurized, and kneaded, and even a high-viscosity substance can be chemically reacted.

Table 1 shows the results of confirming the internal circulation in the reactor 1 using a screw composed of only a forward screw body. Wheat flour and water were prepared as test samples, and these were mixed in the proportions shown in Table 1 and charged into the reactor 1. Table 1 shows the input amount, screw rotation speed, load and the like. The internal circulation was confirmed by checking whether the dye was dispersed inside the hollow structure of the screw shaft core 4 by disassembling the reaction device after charging the dye from the sample supply section. When completely dispersed, it was evaluated as ◯, and when not dispersed, was evaluated as ×.

[0020]

[Table 1]

As shown in Table 1, the water content is 65 to 100% by weight.
Internal circulation was performed in the range of. Moisture content 60% by weight
In the case of 1, the circulation was not sufficient, but it can be circulated by changing the screw pattern and / or the screw rotation speed.

Specifically, Table 2 shows the results obtained by measuring the change in the circulation amount due to the change in the screw pattern by the residence time and the progress of the reaction by viscosity measurement. The screw pattern used is shown in FIG. In Fig. 4, all forward means that all are forward screws, and kneading 10 × n F means that kneading discs with a length of 10 mm are assembled into a 45-degree feed phase. The kneading 10 × n 90 means n pieces of kneading disc with a length of 10 mm, and the kneading disc is assembled into a 90 ° phase. The kneading 10 × n R shows n pieces of a kneading disc with 10 mm length, It means that they are assembled in the reverse feed phase of 45 degrees. The rest of the kneading disk is the forward screw. In Table 2, the extrusion rate is 8 kg / hr
The screw rotation speed was fixed at 40 rpm. Moreover, flour represents wheat flour. Table 2 shows that the reaction of starch below the gelatinization temperature is based on the formation of a gluten network, and therefore the screw pattern and
It is the result of examining the residence time and the change in viscosity in the reactor.

[0023]

[Table 2]

As shown in Table 2, it is possible to secure a stable circulation amount even with a highly viscous substance. For example, the residence time can exceed 6 minutes, and a sufficient reaction time can be secured even if an extruder is used. Further, the circulation amount can be changed by changing the screw pattern. Therefore, the formation reaction of the gluten network can be tested with the reactor of the present invention. In Table 2, the fact that the viscosity cannot be measured means a viscosity above the measurement limit of the viscometer used for the measurement. This circulation amount is
Regardless of the internal circulation method or the external circulation method described later,
It is an important factor contributing to the reaction time and can be controlled not only by the circulation time but also by changing the screw pattern.

The temperature control mechanism of the reactor shown in FIG. 1 comprises an electric heater provided outside the barrel, high temperature steam, a heat medium,
It is composed of a heating device such as electric heating and a cooling device such as water cooling, air cooling, chiller cooling or liquid nitrogen. In particular, the heating device using electric heating is a system in which the reaction target object itself is energized to heat by utilizing its Joule heat, and the product temperature can be controlled more easily. In addition, in food chemistry and the like, the reaction may be promoted by a catalytic action due to electrolysis accompanying electric heating.

An electric heating was tested using wheat flour as a test sample. Stainless steel electrode (size 90mm x 90mm, between electrodes 1
In a cylindrical plastic container (diameter 170 mmφ) equipped with 00 mm, 2 kg of wheat flour with adjusted water content was placed, and a precision power amplifier (manufactured by NF Circuit, model 4510, maximum 16 A) and function synthesizer (manufactured by NF Circuit, model 191)
According to 5), the water content, frequency, and waveform were changed at a voltage of 185V, and the product temperature was measured. The results are shown in FIGS. FIG. 5 shows the results of examining the relationship between the product temperature and the heating time by using the water content, FIG. 6 as the frequency, and FIG. 7 as the waveform as parameters. As shown in FIG. 5, the water content is 30.4% by weight (curve: a), 42.0% by weight (curve: b), 50.3% by weight (curve: c), 56.5% by weight (curve: d) and 71.0% by weight.
Wheat flour adjusted to (curve: e), the temperature rise time is 5
6.5 wt% (curve: d) is the fastest from 25 ℃ 10
The temperature was raised to 0 ° C in 90 seconds. Next, when the frequency was changed with the wheat flour whose water content was adjusted to 56.5% by weight, as shown in Fig. 6, 60Hz (curve: f), 2kHz (curve: g), 10kHz.
(Curve: h) and 20 kHz (curve: i), no large difference in temperature rising rate was observed, and the temperature could be adjusted around 100 ° C. As for the change in the waveform, as shown in FIG. 7, no significant difference was observed in the sine wave (curve: j), square wave (curve: k), and triangular wave (curve: l) with the same water content adjusting raw material, and the temperature adjustment was performed. I knew I could do it. As a result of the above, temperature control can be performed within a range of ± 2 ° C by electric heating.

When a heating device using electric heating is used, the electrodes 9 can be installed between screws and screws, between screws and barrels, and between barrels and barrels where electricity is applied from both ends of the barrels. Also, the members in contact with these electrodes need to be insulated from each other. Therefore, in FIG. 1, it is preferable that the forward screw bodies 5a and 5a in contact with the kneading screw body 5b and the reverse screw body 5c are made of an insulator. Precision power amplifier for reactor 1 (manufactured by NF Circuit, model 451
0, maximum 16 A) and a function synthesizer (manufactured by NF Circuit, type 1915) are attached, liquid egg and flour are selected as reaction targets, and between screw and barrel,
A uniform heat generation was observed when the electrodes were installed so that electricity could be applied between the barrels and the current was continuously applied while the reaction target was continuously charged. Also, ± 2
The temperature could be controlled in the range of ° C.

The pressure control mechanism according to the present invention is a mechanism controlled by a screw pattern and a screw rotation speed in which a screw body, a disk body and the like are combined. That is, the transfer / circulation amount of the reaction target can be controlled by the combination pattern of the screw body, the disc body, etc. and the screw rotation speed, so that the internal pressure can be controlled to be generated. Table 3 shows the measurement results of the internal pressure in the barrel in the reaction between the flour and water when specifically changing the screw pattern and the screw rotation speed.
Shown in. The display of the screw pattern shown in Table 3 is the same as that in FIG. 4, and the extrusion rate is 10 kg / hr.

[0029]

[Table 3]

As shown in Table 3, by changing the screw pattern and the screw rotation speed, 0 to 2.5 kg / c
The generation of an internal pressure of m ² is recognized and the internal pressure can be controlled.

The reaction object circulation mechanism according to the present invention can be constituted by a screw conveying force and an external circulation means. An embodiment of the reaction device having the external circulation means will be described with reference to FIG. FIG. 8 is a flow sheet diagram of an extruder type reaction device having an external circulation means. Reactor 1
Is a twin-screw extruder type reactor 10 and a heat exchanger 1
This is a structure in which 1 and the circulation pump 12 are connected via a circulation path 14. The reaction target 7 circulates in the twin-screw extruder type reactor 10 and the heat exchanger 11 by the conveying force of the screw in the extruder and the discharge force of the circulation pump 12. The screw is rotated by a drive device 15 mounted on the base. Also, the product take-out section 1
6 and a sample collecting unit 17 are provided.

The twin-screw extruder type reactor 10 is the same as the twin-screw extruder type reactor shown in FIG.
The biaxial extruder shown in FIG. 1 can be used except that the screw shaft core is not hollow. A twin-screw extruder having a hollow screw shaft core can also be used. The temperature of the twin-screw extruder type reactor 10 is controlled by an electric heater provided outside the barrel 2, high temperature steam,
A heating device 18 such as a heating medium or electric heating, and a cooling device 19 such as water cooling, air cooling, chiller cooling or liquid nitrogen 19
Can be done by.

The heat exchanger 11 is provided to maintain the circulating reaction object 7 at a predetermined temperature, and its temperature control is provided outside the jacket 13 as in the twin-screw extruder type reactor 10. Electric heater, high temperature steam,
A heating device 18 such as a heating medium or electric heating, and a cooling device 19 such as water cooling, air cooling, chiller cooling or liquid nitrogen 19
Can be done by. When heating by electric heating, the electrodes should be between the top and bottom of the piping using an insulator, and /
Alternatively, it is preferable to install them on the left and right of the pipe using the insulator. Further, it is preferable that the heating / cooling device is also provided around the pipe connecting the twin-screw extruder type reactor 10 and the heat exchanger 11.

The temperature of the reaction object in the heat exchanger 11 may be the same as or different from the temperature in the twin-screw extruder type reactor 10. When they are the same, the reaction device can hold the reaction time as a constant temperature reaction for an arbitrary time, for example, 30 minutes or more. on the other hand,
When they are different, the reaction device can be used for reactions in which constant temperature and high temperature are repeated. Further, the temperature control mechanism may be the same as or different from that of the twin-screw extruder type reactor 10.

As the circulation pump 12, any circulation pump having a discharge capacity larger than that of at least the twin-screw extruder type reactor 10 can be used.

Table 4 shows the results of gluten network formation reaction using flour and water using an external circulation type twin-screw extruder type reactor. The total amount of wheat flour and water was 500 g, and the water content was adjusted to the value shown in Table 4. Specifically, when the water content is 71.3% by weight, 167 g of wheat flour and 333 g of water are added,
For 78.5% by weight, add 125 g of flour and 375 g of water,
In the case of weight%, 100 g of flour and 400 g of water were mixed. The circulation time is 30 minutes, and the heat exchanger 1
The temperature of 1 was also set to be the same as the barrel temperature.

[0037]

[Table 4]

As shown in Table 4, the reactor of the present invention is
The reaction temperature can be changed to perform the gluten network formation reaction.

The reaction apparatus of the present invention is equipped with a measuring instrument for measuring PH, viscosity, circulation flow rate, temperature, pressure, etc. in the apparatus of the circulating reaction object even when the internal circulation or the external circulation means is used. It is preferable to install them, and as these measuring instruments, known PH meters, viscometers, etc. can be used. Further, it is preferable to install a double valve type reaction object charging / discharging port for additionally charging the raw materials or for sampling during the reaction.

In the present invention, the pressure can be applied to the reaction target by the screw pattern and the screw rotation speed. Further, the reaction device may have a closed structure, and a deaeration / decompression / pressurization device may be incorporated as an auxiliary device. preferable. By providing the auxiliary device, the reaction state can be arbitrarily changed.

Since the reaction apparatus of the present invention can secure a stable circulation amount, temperature control and pressure control ability even for a high viscosity substance, it has been difficult to mix and disperse a high viscosity substance, which has been conventionally difficult. It can be applied to reactions. For example, investigation of the influence of component changes that occur in the product when subjected to excessive reaction treatment such as temperature and pressure, continuous production of high-viscosity ester synthesis, sterilization of high-viscosity food materials, uniform dispersion of products including emulsion, It can be used as a novel reaction apparatus for improving texture of dairy products, emulsifying and stirring a small lot, inorganic substance synthesis reaction, flavor synthesis and the like.

[0042]

EFFECT OF THE INVENTION Since the extruder type reactor of the present invention is provided with at least a reaction object circulation mechanism interlocking with a screw and a temperature control mechanism, it is possible to uniformly knead or continuously process a high viscosity reaction object. Can be performed by changing the reaction temperature and the reaction time. As a result, it can be used as a novel reactor for a highly viscous reaction target.

Further, since the pressure control mechanism for applying a pressure to the reaction object is provided by changing the screw pattern and the screw rotation speed, the pressure can be controlled. As a result, it is possible to obtain a reaction device that can handle a reaction in which the amount of substance changes before and after the reaction.

The extruder type reactor of the present invention is
Since the screw has a hollow structure and has an internal circulation mechanism for circulating the reaction target in the hollow structure by the conveying force of the screw, a long reaction time can be easily obtained. Also, the reactor becomes smaller.

Since the reaction object circulation mechanism has an external circulation mechanism that circulates the reaction object by the screw conveying force and the external circulation means, even a high viscosity product can be reliably circulated.

Since the electric heating of the reaction object is used as the temperature control mechanism, the temperature control can be easily performed even with a high viscosity product.

The extruder type reactor of the present invention is
Since the screw is at least one connected body selected from a screw body and a disc body fitted to the screw shaft core, the reaction object is transferred, filled and pressurized, and kneaded by changing the combination of the screw body and the disc body. Etc. can be set to any reaction state. as a result,
It can be used as a novel reactor for highly viscous substances.

[Brief description of drawings]

FIG. 1 is a diagram showing an example of a reaction apparatus.

FIG. 2 is a perspective view of a screw.

FIG. 3 is a perspective view of a screw body and a disc body.

FIG. 4 is a diagram showing a screw pattern.

FIG. 5 is a result of investigating the relationship between the product temperature and the heating time by using the water content as a parameter.

FIG. 6 is a result of examining the relationship between the product temperature and the heating time using the frequency as a parameter.

FIG. 7 is a result of examining the relationship between the product temperature and the heating time using the waveform as a parameter.

FIG. 8 is a diagram showing an example of a reaction apparatus.

[Explanation of symbols]

1 reactor 2 barrels 3 screws 4 screw shaft core 5 screw body 6 disk body 7 Reaction target 8 supply departments 9 electrodes 10 2-axis extruder type reactor 11 heat exchanger 12 Circulation pump 13 jacket 14 Circulation path 15 Drive 16 Product take-out section 17 Sample collection section 18 heating device 19 Cooling system

   ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Hideyo Yoshida             2-4 Suehirocho, Yokkaichi-shi, Mie Co., Ltd.             In Suheroy PGM F-term (reference) 4G035 AB37 AB41 AC29 AE01 AE15                 4G037 CA03 CA11 CA18 EA01                 4G075 AA34 AA62 AA63 BB05 CA02                       CA03 CA13 EA01 EA06 EB50                       EC21 ED03 FB02 FB04 FB12                 4G078 AA22 AA24 AB09 BA05 BA07                       DA09 DB01 DC08 DC10 EA03

Claims (6)

[Claims] 1. An extruder type reaction apparatus having a barrel and a screw provided in the barrel, wherein a reaction object circulation mechanism for circulating a reaction object at least in conjunction with the screw, and the reaction And a temperature control mechanism for controlling the temperature of the object. 2. The reaction apparatus according to claim 1, further comprising a pressure control mechanism that applies a pressure to the reaction target by changing a screw pattern and a screw rotation speed. 3. The reaction object circulating mechanism has a hollow structure inside the screw, and circulates the reaction object inside the hollow structure by a conveying force of the screw. Item 2. A reactor according to item 2. 4. The reaction apparatus according to claim 1, wherein the reaction object circulation mechanism circulates the reaction object by a conveying force of the screw and an external circulation means. 5. The reaction apparatus according to claim 3, wherein the temperature control mechanism is provided by electrically heating the reaction target. 6. The screw according to claim 1, wherein the screw is at least one connecting body selected from a screw body and a disc body that fit into a screw shaft core. Reactor.