JP2853605B2 - Method and apparatus for producing highly viscous substance - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a stirring and mixing process for a high-viscosity liquid, and more particularly to, for example, a liquid crystal polymer (Liquid Crystal Plast).
The present invention relates to a method and an apparatus for producing a high-viscosity substance suitable for producing a high-performance engineering plastic such as ics) and polyarylate (Polyarylate).

[0002]

2. Description of the Related Art Generally, in the production of kneading and reaction of a highly viscous substance, the adhesion and co-rotation of a liquid to be treated in an apparatus is reduced, and the remaining portion of the liquid to be treated is reduced to deteriorate the quality. Various proposals have been proposed to prevent this. For example, Japanese Patent Publication No. 56-116721 and literature (basic and analysis of polymerization reactor: Yasuhiro Murakami: P33-P
As shown in 37), there is a structure in which ribbon wings are arranged so that the entire inner surface of the container can be scraped off. FIG. 21 illustrates an example in which this structure is embodied by a cylindrical container. In the figure, stirring power is transmitted from a drive source to a rotation shaft 5 in the stirring tank main body 1 via a rotation power transmission shaft (hereinafter, referred to as a rotation ear shaft) 2. A plurality of support arms 4a and 4b are attached to the rotating shaft 5 in the horizontal direction.
At the tip of b, ribbon wings 3a and 3b are attached spirally so as to scrape the inner wall of the stirring tank body 1 all over. A supply port 6 for the liquid to be treated and the additive from the prepolymerization device 23 is provided at an upper portion of the stirring tank main body 1, and a discharge port 7 for the liquid to be treated is provided at a lower portion. When the high-viscosity liquid is stirred and mixed by this apparatus, the viscosity of the liquid to be treated is several hundred to 1 kPa.
s (several thousands to 10,000 poises), but when the viscosity of the liquid to be treated reaches several kPa · s (tens of thousands poises),
The liquid to be treated adheres to the ribbon blades 3a and 3b, causing a corotation phenomenon. In addition, since the peripheral speed of the surface of the rotating shaft 5 is low, when the liquid becomes a high-viscosity liquid, co-rotation of the liquid to be treated occurs, a dead space is generated, and the stirring / mixing performance deteriorates. Therefore, in the conventional apparatus, the viscosity of the liquid to be treated is 1 kPa · s (10,000 poise).
If the viscosity becomes higher than that, the time required for stirring becomes longer, and there is a problem that the quality of the object to be treated is deteriorated due to the dead space.

Further, a conventional method for producing general-purpose plastics and the like is produced by a polymerization reaction process as described in a literature (basic and analysis of polymerization reaction apparatus: written by Yasuhiro Murakami: P137-P140). When a high-performance engineering plastic is manufactured by the above-described process, the following problems occur. Higher functionality of plastics includes, for example, an increase in mechanical strength, an increase in heat resistance temperature, and an improvement in weather resistance and chemical resistance.However, in general, higher functionality increases the degree of polymerization of the resin, that is, the molecular weight. It is to increase. As the molecular weight of the resin increases, the melt viscosity of the resin increases.

The processing viscosity of the stirrer used in the conventional production process is limited to 1 kPa · s (10,000 poise). Therefore, in order to manufacture a high-performance resin (super engineering plastic), it is manufactured by a process shown in FIG. The conventional process will be described with reference to FIG. The raw material is adjusted by adding a monomer and a catalyst, which are the raw materials for the resin, and then the solvent for the resin is added, and the mixture is fed into a stirring tank in a low-viscosity liquid state. I do. At this time, polymerization by-products generated as the reaction proceeds are removed as needed. Although the molecular weight of the resin increases with the progress of the reaction, the viscosity of the solution does not increase and is kept at about several hundred Pa · s (several thousands of poises) because the resin is stirred in the solvent. When the reaction proceeds and reaches a predetermined degree of polymerization, there is a process of recovering the solvent as the next step. In this step, a demonomer device, a dehydration device, a drying device, and the like are provided, and finally, only a final polymer separated from the solvent is obtained.

Next, another method for producing a high-performance resin (super engineering plastic) will be described with reference to FIG. In this process, a catalyst is added to a monomer, which is a raw material of the resin, and adjusted to be supplied into a stirring tank. The stirring tank is kept at a predetermined reaction temperature and at an atmospheric condition, and is stirred and mixed. At this time, if the polymerization by-product generated by the reaction is removed as needed, the molecular weight of the resin increases with the progress of the reaction, the viscosity of the stirring treatment liquid increases,
It becomes a lump state and becomes lump polymerization. As the reaction progresses further,
The viscosity of the processing liquid reaches the processing limit viscosity of the stirring device. The intermediate polymer having reached the critical viscosity is discharged out of the stirring tank, and the temperature of the treatment liquid is lowered to the melting point or lower and solidified to form chips. The chip-shaped intermediate polymer is supplied into another type of agitator, and is stirred while maintaining a predetermined atmospheric condition, whereby the polymerization reaction further proceeds. A final polymer is produced by this solid-phase polymerization reaction.

A stirrer used for solution polymerization and bulk polymerization in a conventional production process is usually composed of a pre-polymerization device 23 and a polymerization device 25 as shown in FIG. The prepolymerization device 23 is provided with a stirring blade 24 for low viscosity. This pre-polymerization apparatus 23 mainly processes a low-viscosity liquid mainly by stirring and mixing a raw material and a catalyst, and a turbine blade or a paddle blade or the like is used as the low-viscosity stirring blade 24. The treatment liquid that has been subjected to the pre-polymerization treatment by the preliminary polymerization device 23 is supplied to the polymerization device 25. Here, predetermined reaction conditions are set and the polymerization reaction proceeds. The stirring blades 3a and 3b for medium viscosity used in the polymerization apparatus 25 usually have several hundred Pa ·
A ribbon wing capable of processing from s to 1 kPa · s (thousands of poise to 10,000 poise) is used. The polymer that has been processed up to the predetermined polymerization by the polymerization apparatus 25 is sent to the next step according to the above-described process. In addition, as a device related to this type, for example, Japanese Patent Application Laid-Open No. 62-95122 and Japanese Utility Model Application No. 47-38289 are cited.

[0007]

In the above prior art, no consideration is given to the stirring and mixing of high-viscosity substances.
As the viscosity of the liquid to be treated becomes higher, the adherence becomes more intense. As a result, the flow of the liquid to be treated acts only on the ribbon wing part having a large shearing action due to stirring, and the flow of the liquid in the center of the stirring tank where the shearing force cannot reach. There is almost no flow. Furthermore, if the viscosity of the liquid to be treated increases, the adhesion of the liquid to be treated that adheres to the surface of the ribbon blade becomes larger than the shearing force due to the stirring, and the liquid to be treated co-rotates while remaining attached to the surface of the ribbon blade. As a result, agitation and mixing deteriorate, and the liquid to be treated adheres to the agitation shaft that is less susceptible to shearing force, and the adhered substance deteriorates in quality. There was a disadvantage. Furthermore, since the conventional apparatus can process only a viscosity up to about 1 kPa · s (10,000 poise), another processing apparatus for a high-viscosity substance must be used, and the manufacturing process of a high-performance resin is complicated and the manufacturing time becomes long. There was a disadvantage.

It is an object of the present invention to provide a method and an apparatus for producing a high-viscosity substance, in which a portion of the liquid to be treated stays little and quality can be improved.

Another object of the present invention is to provide a method and an apparatus for producing a highly viscous substance suitable for producing a polycondensation polymer or the like which can promote the circulation flow in the vessel and improve the surface renewal performance. .

[0010]

In order to achieve the above object, according to the present invention, for example, a raw material and a catalyst are supplied,
These are stirred by the rotation of the low-viscosity stirring blade to generate a low-viscosity treatment liquid, and the low-viscosity treatment liquid is supplied, and the supplied treatment liquid is rotated by the high-viscosity stirring blade. Agitation, perform bulk polymerization, and a stirring step of producing a polycondensation polymer such as polyethylene terephthalate, polybutylene terephthalate, polyamide, polyacetal, and polycarbonate. A first rectangular frame provided in the stirring vessel main body and a second rectangular frame joined in a different direction from the first rectangular frame. A configuration in which a polymerization reaction operation is performed by rotating a stirring blade through a rotary ear shaft is adopted.

[0011]

The liquid to be treated can be prevented from adhering to the rotating shaft by making the structure of the high-viscosity stirring blade a connecting structure in which the directions of rectangular frames having no rotating shaft are different.

According to the structure of the present invention, the high-viscosity agitation is possible because the adhesion of the treatment liquid to the shaft and the co-rotation phenomenon, which are problems when treating the high-viscosity liquid, do not occur. For this reason, in the conventional process, it was necessary to reduce the stirring viscosity or to use a different type of stirring device in the middle, but if this stirring device is used, the same stirring device can be used up to the high-viscosity final polymer. Therefore, the manufacturing process can be simplified.
That is, since bulk polymerization becomes possible, polyethylene terephthalate, polybutylene terephthalate, polyamide, polyacetal, polycondensation polymers such as polcarbonate, can be produced without using a solvent,
The manufacturing process can be simplified.

[0013]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The basic configuration on which the present invention is based will be described below with reference to FIGS. In FIG. 1, a stirring vessel main body 1 is a cylindrical vessel having a circular cross section, and the outside thereof has a heat medium jacket that can be heated and cooled, though not shown. The stirring blade has a rotating power transmission shaft (hereinafter, referred to as a rotating ear shaft) 2 and stirring blade members 8a, 8b, 8c, 8d, 9a, 9b, 9
c to form a rectangular frame.
One stirrer blade component (lattice blade) connected by being shifted by degrees
To form As shown in FIG. 2, this configuration shows a case where θ is 90 degrees, but the value of θ may take any value. Further, the stirring blade members 8a, 8b, 8
For c, 8d and 9a, 9b, 9c, 9d, 9f, round bars or plate-like members are used.

The stirring action of the highly viscous substance in the above configuration will be described. Stirring blade member 8a by rotating ear shaft 2
The rotation is transmitted to. Stirring blade members 8a, 8b, 9a, 9
The rectangular frame formed by d rotates along the inner wall of the stirring tank body 1 to stir and mix the liquid to be treated. The stirring blade members 8a, 8b, 8c, 8d installed in the horizontal direction rotate in the tank in the horizontal direction, and contribute to stirring and mixing in the radial direction. Also, the vertical stirring blade members 9a, 9d, 9b, 9c, 9e,
In the case of 9f, the tank wall surface is completely scraped off, so that there is no remaining portion of the liquid to be treated. Further, the rectangular stirring blade element and the next rectangular stirring blade element are mounted at an installation angle θ, and the next rectangular stirring element is also continuously formed at an installation angle θ. Therefore, the horizontal stirring blade member 8
a, 8b, 8c, 8d and vertical members 9a, 9
When the high-viscosity liquid is stirred and mixed at b, 9c, 9d, 9e, and 9f, the positions of the respective blade members are distributed at the respective positions in the tank. The shape becomes complicated, and the ratio of the surface area of the liquid to be treated to the volume of the tank increases. This leads, for example, to an improvement in the degassing performance of volatiles in the polymerization reaction operation. In addition, since there is no rotating shaft, there is no sticking of the high-viscosity substance to be treated, and good stirring / mixing performance can be obtained. In this configuration, the stirring blade members 9a, 9b, 9c, 9d, 9e, 9f
Although the case where a round bar is used is shown, the same effect can be obtained by using a plate-shaped member or the like.

Next, another configuration on which the present invention is based will be described with reference to FIGS. 3 and 4. FIG. In the figure, a stirring vessel main body 1 is a cylindrical vessel having a circular cross section, and although not shown, the outside has a heating medium jacket capable of heating and cooling. The stirring blade includes the rotating ear shaft 2 and the stirring blade members 8a, 8
b, 9a and 9d are combined and connected to form a rectangular frame to form one stirring blade component (lattice blade). Among the stirring blade components, the stirring blade members 8a and 8 installed in the horizontal direction.
b is located at a position twisted in the rotation direction about the center of the tank by θ 2 around the center of rotation, and is connected to the vertical stirring blade members 9a and 9d formed so as to scrape the tank wall. The next stirring blade component has the same shape, and the horizontal stirring blade members 8b and 8e are connected at an attachment angle θ 2. Further, the following stirring blade components are also attached at the same angle to form one stirring blade. Although the illustrated shape shows the case where the mounting angle θ is 90 degrees, arbitrary angles may be set for θ and θ.
Further, as the stirring blade members 8a, 8b, 8c, 8d, 8e, 8f and 9a, 9b, 9c, 9d, 9e, 9f, round bars or plate-like members are used. The stirring action of the high-viscosity substance in the above configuration will be described. Rotation is transmitted to the stirring blade member 8a by the rotating ear shaft 2. Stirring blade member 8a,
The rectangular frame constituted by 8b, 9a, and 9d rotates along the inner wall of the stirring tank main body 1, and stirs and mixes the liquid to be treated. The stirring blade members 8a and 8b installed in the horizontal direction rotate in the tank in the horizontal direction and contribute to stirring and mixing in the radial direction. Further, the stirring blade members 9a and 9d, which rotate while scraping the wall surface along the inner wall surface of the tank, are mounted with the stirring blade members 8a and 8b advanced by about θ in the rotation direction, so that the liquid to be treated near the wall surface of the tank is rotated by the rotation. A force to lift upward acts. Therefore, the rotation of the stirring blade component causes an upward flow in the liquid to be treated in the peripheral portion of the tank, and thereby a downward flow occurs in the central portion of the tank. Further, this stirring blade component is connected to the next stirring blade component while maintaining the mounting angle θ 1, and the next stirring blade component is connected in the same manner to form a stirring blade. Therefore, a flow from the lower part of the tank to the upper part is generated near the inner wall surface of the tank by the respective components of the stirring blade, and a flow from the upper part to the lower part is generated in the central part of the tank. There is no liquid stagnation, and good stirring and mixing can be obtained. Here, the flow of the liquid to be treated in the vicinity of the tank wall of the stirrer of this configuration will be described with reference to FIG.

The present invention is particularly suitable when the liquid to be treated has a high viscosity such as tens of thousands of poise. FIG. 5 shows a case where the cylindrical inner peripheral wall surface of the stirring tank main body 1 of the apparatus shown in FIG. In the drawing, a rectangular frame stirring blade member 9 is shown.
Since a, 9d, 9b, 9e, 9f, and 9c each have a rotational phase angle θ 2, they have a gradient inclined backward with respect to the traveling direction of the stirring blade. When the stirring blade is rotated in this state, a lump of the liquid to be treated 15 is formed on the front surface of the stirring blade member 9a. As the stirring blades rotate, the liquid mass to be treated is pushed upward as a whole. At this time, the liquid to be treated 15 is mixed on the front surface of the stirring member 9a. In this configuration, the stirring blade members 9a, 9d, 9b, 9e, 9f, 9c are divided and distributed in the tank. Therefore, for example, a part of the liquid to be treated mixed by the stirring blade member 9b overflows rearward from the upper end and the lower end of the stirring blade member. A part of the overflowed liquid to be treated is joined and mixed with the liquid to be stirred and mixed by the agitating blade members 9a and 9f that are advanced later, and the uniform stirring and mixing performance of the entire tank is achieved. Contribute to the improvement of FIG.
1 shows a case where the ribbon wing of the conventional device shown in FIG. The conventional stirring blades 3a and 3b are respectively installed continuously in the tank. Therefore, in the conventional stirring blade, the whole liquid is pushed up to the upper side and stirred while the liquid to be treated is stirred and mixed only on the front surfaces of the stirring blade members 3a and 3b. When the viscosity of the liquid to be treated increases, the adhesion of the liquid to be treated increases, and the liquid adheres to the surfaces of the stirring blades 3a and 3b, and the movement to the upper side decreases. Drops. In the method of FIG. 5 described above, since the stirring blade members are divided, co-rotation hardly occurs. In addition, since the stirring blade members are uniformly distributed throughout the tank, the shape of the liquid to be treated formed by stirring becomes complicated, the ratio of the surface area of the liquid to the tank volume increases, and degassing of volatile components occurs. There is an advantage that the performance can be improved and the reaction time can be shortened in the polymerization reaction operation. In addition, since there is no rotating shaft, adhesion and retention of the high-viscosity treatment substance are eliminated, and good stirring performance is obtained. Although the present configuration shows a case where a round bar is used as the stirring blade member, a similar effect can be obtained by using a plate-shaped member or the like.

Next, another configuration on which the present invention is based will be described with reference to FIGS. This configuration has the same basic components and operation as those described above, and has the same effects. This configuration shows a case where the mounting phase θ of the stirring blade components 8a and 8b of the stirring blade components is set to 90 degrees. Further, the stirring blade components 9a and 9d are plate-shaped ribbon blades, and the stirring blade components are connected to each other at an attachment angle θ of 90 ° to form a stirring blade. By using a ribbon blade as a component of the stirring blade, the action of scraping up the processing liquid is further increased, the circulation flow of the entire tank is strengthened, and a good mixing / stirring effect is obtained. In addition, since the ribbon blades are intermittently arranged on the tank wall, the amount of liquid to be treated adheres and stays on the stirring blades is reduced compared to the case where the ribbon blades are configured continuously, and the stirring and mixing performance is improved. I do.

Next, an example of the configuration of a stirring tank suitable for use in the present invention will be described with reference to FIGS. This configuration is the same as the above-described configuration in basic constituent members and operation, and similar effects can be obtained. In this configuration, in particular, the lower part of the stirring tank body 1 has a conical shape, and a rectangular shape is formed on the conical tank wall. With this structure, it is easy to discharge the liquid to be treated when discharging the liquid to be treated, and there is an effect that the liquid can be discharged in a short time.

Further, in this configuration, the lower part of the stirring tank main body 1 has a conical shape, a discharge device 10 is provided at the apex of the conical portion, and a pressurizing device 11 which can pressurize the inside of the tank is provided upstream of the supply port. The stirring blades have a rectangular shape like that on the conical tank wall. Further, the stirring blade members 8a and 8b are located at positions twisted in the direction of rotation about the center of the tank as the center of rotation by θ 2, and are respectively connected to vertical members 9a and 9d formed so as to scrape the wall of the tank. . The next stirring blade component has the same shape and has horizontal members 8b and 8e.
Are connected at an attachment angle θ 2, and the following stirring blade components are similarly connected to form a stirring blade. In this configuration, when the treatment liquid is discharged after the completion of the stirring or the reaction operation, the stirring device is rotated in the opposite direction to that during the reaction operation, the discharge device 10 is operated at the same time, and the pressurizing device 11 pressurizes and discharges the inside of the tank. Perform processing. According to this method, since the stirring blade is reversed, the liquid to be treated is pushed down below the wall surface of the tank and concentrates on the lower part of the tank. Furthermore, since the inside of the tank is in a pressurized state, there is an advantage that the supply to the discharge device 10 is easy and the discharge time of the liquid to be treated can be shortened.

In this configuration, both ends (9a, 9a, 9a) of the stirring blade member that scrapes the tank wall surface among the stirring blade components are particularly used.
d, 9d, 9b, 9b, 9e, 9e, 9c, 9
f) is extended upward and downward from the connection with the horizontal stirring blade member to form a stirring blade component, and these stirring blade components are connected to form a stirring blade. The flow of the liquid to be treated in the vicinity of the wall surface of the tank of the vertical stirring device having this configuration will be described. FIG. 10 shows a case where the cylindrical circumferential wall surface of the device shown in FIG. 8 is developed in a plane. FIG. 10 is almost the same as the content described with reference to FIG. In this configuration, in particular, the stirring blade members 9a, 9d,
9b, 9e, 9f, and 9c are divided and distributed in the tank, and the end of the stirring blade member enters inside the trajectory of each blade. Since the mixing with the liquid to be treated on the front surface of the rear stirring blade member is further improved, it contributes to the improvement of the uniform stirring / mixing performance of the entire inside of the tank. Also, the ends 9a, 9 of the wing members
If the mounting angle d is formed in a direction opposite to the inclination of the blade members 9a and 9d, there is also an effect of preventing the treatment liquid from adhering and staying on the upper portion of the tank. In this example, the discharge device 10 is illustrated as a screw type, but the present invention is not limited to this. That is, the discharge device 10 may be configured by providing a discharge valve at the tip of the screw.

Next, another configuration on which the present invention is based will be described with reference to FIG. This configuration has the same basic components and operation as the above-described configuration, and the same effects can be obtained. In this configuration, the shape of the stirring tank body 1 is particularly conical (cone-shaped), and the shape of the stirring blade is conical so as to follow the tank wall. By adopting this configuration, the liquid to be processed spreads along the wall of the tank during stirring, and the surface area per volume of the liquid to be processed increases because the cross-sectional area of the upper tank is larger than that of the cylindrical tank. The surface renewal effect is improved. In the polymerization reaction operation of a high-viscosity liquid, the surface renewal performance determines the reaction time, and improvement of this performance contributes to shortening the reaction time.

Next, an embodiment of the present invention will be described with reference to FIG. The present embodiment has the same basic components and operation as the above-described configuration, and the same effects can be obtained.
In this embodiment, in particular, reinforcing members 20a and 20d are vertically attached to the inside of the rectangular frame of the stirring blade component, and 20e and 20b are attached to another rectangular frame, thereby enhancing the rigidity of each stirring blade component. Things. By attaching the reinforcing member, the strength of the stirring blade can be improved, and the stirring and mixing in the rectangular frame can be improved, which contributes to the improvement of the stirring and mixing performance.

Next, another configuration on which the present invention is based will be described with reference to FIGS.

This configuration has the same basic components and operation as those of the above-described configuration, and similar effects can be obtained. In this configuration, the stirring blade components 8a, 9a, 8b, 9b and 8 are particularly provided at the portions of the stirring blade components connected to the rotary ear shaft 2.
g, 21b, 8e, and 21a are connected to form a stirring blade. With this configuration, the number of members of the stirring power transmission unit increases, so that the rigidity of the stirring blade is enhanced. Although not shown, the same effect can be obtained by further connecting the stirring blade components between 8b and 8c.

Next, another configuration on which the present invention is based will be described with reference to FIGS. This configuration has the same basic components and operation as the above-described configuration, and the same effects can be obtained. Particularly in this configuration, in the stirring / mixing operation, particularly when treating a liquid to be treated of several kPa · s (tens of thousands of poise), the liquid to be treated that has scraped up the tank wall stays in the upper part of the tank, making uniform stirring difficult. In order to prevent such a phenomenon, the horizontal phase angle of the stirring blade members 8a and 8b among the stirring blade components above the stirring blade is twisted by θ 2 in the direction opposite to the rotation direction to form the stirring blade components. With this configuration, the inclination of the stirring blade members 9a and 9d that scrape the wall surface of the stirring tank acts to push down the processing liquid on the wall surface of the tank when the stirring blade rotates in the operation direction. Therefore, the lower stirring blade component acts to push the liquid to be processed upward along the tank wall surface, and the upper stirring blade component pushes down the liquid to be processed, so that the liquid to be processed stays near the upper portion of the tank. And good stirring / mixing performance can be obtained.

FIG. 1 shows another configuration on which the present invention is based.
7 and FIG. In this configuration, there is a configuration in which a stirring blade component member is formed in a hollow shape, and the rotary ear shaft 2 is a double tube and a rotary joint 50 is provided at an upper end of the rotary ear shaft 2.
In the present configuration, the stirring blade components 8a, 9a, 8b, 8e, 9b, and 9e, 8e, 8
Since the heat transfer medium can be supplied and circulated inside b and 9b, the heating and cooling operations of the liquid to be treated can be performed rapidly, and the processing time for polymerization can be shortened.

When the treatment liquid is discharged, the amount of liquid adhering to the surface of the stirring blade can be reduced by supplying a heating medium into the components of the stirring blade.

In still another configuration, a change in the viscosity of the liquid to be treated is detected by detecting the rotation torque of the rotary ear shaft 2, and the number of rotations of the rotary ear shaft 2 is changed according to the viscosity. In this configuration, when the viscosity of the liquid to be treated is low, the rotation speed is increased to achieve strong stirring, and when the viscosity is high, the rotation speed is reduced to prevent an excessive torque. In this case, the viscosity of the liquid to be treated can be directly measured by sampling at regular intervals from a spare nozzle (not shown) in addition to the rotational torque.

Next, one embodiment of the method for producing a high-viscosity substance according to the present invention will be described with reference to FIGS. FIG. 19 shows a schematic flow of a manufacturing process of a high-performance resin (high-viscosity substance). The desired final polymer is produced by bulk polymerization by mixing a monomer, which is a raw material of a highly viscous substance, and a catalyst, and performing an addition polymerization reaction or a condensation polymerization reaction. Since the high-performance resin increases the degree of polymerization, the melt viscosity increases, and the melt viscosity of the final polymer increases to several kPa · s (tens of thousands poise). When a liquid of several kPa · s (several tens of thousands of poises) is treated with a normal stirring device, the mixing and stirring performance is poor, so that the degree of polymerization distribution of the product greatly varies, and the quality is greatly reduced.
Therefore, using the high-viscosity substance stirring device shown in FIG. 8, the final polymer is treated without deteriorating the stirring performance. The configuration and operation of the high-viscosity substance stirring device shown in FIGS.

By the stirring blades forming the frame member of the present invention, the processing liquid can be circulated through the entire tank, and the stagnation portion of the liquid is eliminated, so that good stirring and mixing of the high viscosity liquid can be obtained. Therefore, a final polymerization product having a uniform polymerization degree can be obtained by performing a polymerization reaction using the present stirring device. Further, from the beginning of the polymerization reaction, the production of the final polymer can be carried out by one stirring device.

Next, another embodiment of the present invention will be described with reference to FIG.
0 will be described. In this embodiment, the pre-polymerization apparatus 23 and FIG.
Alternatively, a high-performance resin (high-viscosity substance) is produced by addition polymerization reaction or polycondensation reaction using the stirring device 18 described with reference to FIG. In this example, a low-viscosity liquid at the stage prior to the polymerization reaction is treated by a conventional prepolymerization apparatus 23 equipped with a conventional low-viscosity stirring blade 24, and a stirring device equipped with a high-viscosity stirring blade 19 from a medium viscosity to a final processed viscosity. The treatment is performed in 18 stirring tanks 1. The high-viscosity stirring blade 19 has the same configuration and operation as those described with reference to FIG. 8 or FIG. With the above configuration, by manufacturing a high-performance resin (high-viscosity substance), it can be manufactured only by the bulk polymerization process, so that the process can be simplified.

As described above, according to this embodiment, the circulation speed of the liquid to be treated in the main body 1 can be increased and the surface renewal performance can be improved, so that polycondensation polymers (polyethylene terephthalate, polybutylene terephthalate polyamide, polyacetal) can be obtained. , Polycarbonate, etc.). Further, according to the present embodiment, since the heat transfer performance of the liquid to be treated is enhanced, the heat of reaction of the liquid to be treated is easily removed in the addition polymerization type polymer polymerization such as polystyrene, and a stable polymerization operation can be performed. .

Furthermore, according to this embodiment, the surface renewal performance with a high-viscosity liquid to be treated and the performance of heat transfer from the walls of the main body can be enhanced. The operation of the present invention is suitable for the solvent operation.

Furthermore, according to the present embodiment, the circulation rate in the main body can be increased even in the operation of removing volatiles from the granular material and the sticky granular material, so that the apparatus of the present invention is suitable. It is also suitable for solid-phase polymerization of powdery or granular polymers such as polyethylene terephthalate and polybutylene terephthalate.

[0035]

According to the present invention, since the inside of the tank is scraped by the rectangular frame member, good stirring / mixing performance without a stagnant portion can be obtained. In addition, since there is no rotating shaft that causes the liquid to be processed to co-rotate, the quality of the liquid to be processed can be prevented from deteriorating due to stirring and mixing. Furthermore, when the rectangular frame member is provided with the action of scavenging the liquid to be treated, a large circulation flow is generated in the tank, and the stirring / mixing performance is improved.

Further, since the rectangular frame members are connected and rotated, the shape of the liquid to be treated stirred throughout the tank becomes complicated, the ratio of the surface area of the liquid to be treated per tank volume increases, and the surface renewal effect is obtained. Thus, there is an effect that the degassing performance of the evaporation component is improved. In addition, by rotating the stirring blade in reverse,
There is an effect that the liquid to be treated is concentrated at the lower part of the tank, and the discharge time of the liquid to be treated can be shortened.

[Brief description of the drawings]

FIG. 1 is a schematic diagram of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

FIG. 2 is a sectional view taken along line II of FIG. 1;

FIG. 3 is a schematic diagram of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

FIG. 4 is a sectional view taken along line II-II of FIG.

FIG. 5 is a development view of a cylindrical peripheral wall surface of the manufacturing apparatus shown in FIG. 3;

FIG. 6 is a schematic diagram of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

FIG. 7 is a sectional view taken along line III-III of FIG. 6;

FIG. 8 is a schematic view showing an example of a layer structure suitable for use in the present invention.

9 is a sectional view taken along line IV-IV in FIG.

FIG. 10 is a development view of a cylindrical circumferential wall surface of the manufacturing apparatus shown in FIG.

FIG. 11 is a schematic view of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

FIG. 12 is a schematic view showing one embodiment of an apparatus for producing a highly viscous substance according to the present invention.

FIG. 13 is a schematic diagram of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

FIG. 14 is a sectional view taken along line VV of FIG.

FIG. 15 is a schematic diagram of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

16 is a sectional view taken along line VI-VI of FIG.

FIG. 17 is a schematic view of a configuration example of an apparatus for producing a high-viscosity substance, which is a premise of the present invention.

18 is a sectional view taken along line VII-VII in FIG.

FIG. 19 is a flowchart showing one embodiment of a manufacturing method according to the present invention.

FIG. 20 is a flowchart showing another embodiment of the manufacturing method according to the present invention.

FIG. 21 is a conventional apparatus for producing a high-viscosity substance.

FIG. 22 is a development view of a cylindrical circumferential wall surface of the manufacturing apparatus shown in FIG. 21.

FIG. 23 is a flow chart relating to a conventional manufacturing process.

FIG. 24 is a flow chart related to a conventional manufacturing process.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... stirring tank main body, 2 ... rotating ear shaft, 6 ... supply port, 7 ... discharge port, 8a-8d ... stirring blade member, 9a-9f ... stirring blade member, 10 ... discharge device, 11 ... pressurizing device, 18 ... stirring device, 19 ... stirring blade for high viscosity, 20a, 20b, 20e,
20d: reinforcing member, 23: pre-polymerization device, 24: low-viscosity stirring blade, 25: polymerization device, 31: blade joint member.

──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Moruhisa Maruko 502 Kandachicho, Tsuchiura-shi, Ibaraki Pref. Machinery Research Laboratory, Hitachi, Ltd. Inside the Todo factory (72) Inventor Kinoshita Takashi Higashi-Toyoi, Kazamatsu City, Yamaguchi Prefecture Hitachi, Ltd.Kasato Factory, Ltd. Inside the factory (72) Inventor Kenichi Watanabe 794, Higashi-Toyoi, Kazamatsu-shi, Yamaguchi Prefecture Inside the Kasado Factory, Hitachi, Ltd. (56) References JP-A-63-28433 (JP, A) JP-A-63-322 (JP) JP-A-63-321 (JP, A) JP-A-53-36583 (JP, A) JP-A-58-96627 (JP, A) JP-A-51-27156 (JP, A) A) JP-A-2-58503 (JP, A) JP-A-3-60728 (JP, A) JP-A-63-135950 (JP, U) JP-A-51-1570 (JP, U) −90164 (JP, B2) (58) Field surveyed (Int. Cl. ⁶ , DB name) B01F 7/16 B01F 3/10 C08F 2/00

Claims (4)

(57) [Claims] 1. A pre-polymerization step of supplying a raw material and a catalyst, stirring them by rotating a low-viscosity stirring blade to produce a low-viscosity treatment liquid, and supplying the low-viscosity treatment liquid, A low-viscosity treatment solution is stirred by rotating a high-viscosity stirring blade to perform bulk polymerization, and a stirring step for producing polycondensation polymers such as polyethylene terephthalate, polybutylene terephthalate, polyamide, polyacetal, and polycarbonate. The high-viscosity stirring blade includes upper and lower horizontal members provided vertically separated in the stirring tank main body, and first and second vertical members respectively connecting these ends in a vertical direction. A first rectangular frame structure comprising:
And the upper horizontal member is crossed and connected to the lower horizontal member of the first rectangular frame structure to form the first rectangular frame structure. And a second rectangular frame structure disposed on the lower side. In the stirring step, the polymerization reaction operation is performed by rotating the high-viscosity stirring blade via a rotating ear shaft. Method for producing a highly viscous substance. 2. A method for producing a highly viscous substance according to claim 1.
And upper and lower horizontal members of each rectangular frame structure
Crosses the rotation direction at a predetermined angle at the center of rotation.
Of highly viscous substances characterized by having a positional relationship
Method. 3. A raw material and a catalyst are supplied, and these are stirred by rotation of a low-viscosity stirring blade to produce a low-viscosity treatment liquid; and the low-viscosity treatment liquid is supplied and supplied. The resulting treatment liquid is stirred by rotation of a high-viscosity stirring blade to perform bulk polymerization, and a stirrer that generates a polycondensation polymer such as polyethylene terephthalate, polybutylene terephthalate, polyamide, polyacetal, and polycarbonate, The stirring device has a stirring tank main body, and a rotating ear shaft for rotating the high-viscosity stirring blade in the stirring tank main body. The high-viscosity stirring blade is vertically separated in the stirring tank main body. And upper and lower horizontal members, and first and second vertical members for vertically connecting the ends of the upper and lower horizontal members, respectively. A first rectangular frame structure, and the upper horizontal member is configured similarly to the first rectangular frame structure, and the lower horizontal member of the first rectangular frame structure intersects with the lower horizontal member. Connected
An apparatus for producing a high-viscosity material, comprising: a second rectangular frame structure disposed below the first rectangular frame structure. 4. The apparatus for producing a highly viscous substance according to claim 3,
And upper and lower horizontal members of each rectangular frame structure
Crosses the rotation direction at a predetermined angle at the center of rotation.
Of highly viscous substances characterized by having a positional relationship
apparatus.