JPH0790164B2 - Apparatus and method for producing high-viscosity substance - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a stirring and mixing treatment of a high-viscosity liquid, and particularly to the production of highly functional engineering plastics such as liquid crystal polymers (Liquid Crystal Plastics) and polyarylates. The present invention relates to the production of a highly viscous substance suitable for.

[Conventional technology]

Generally, in the production of kneading and reaction of highly viscous substances,
Various types of devices have been devised, in which the adhesion and co-rotation of the liquid to be treated in the apparatus are reduced and the accumulated portion of the liquid to be treated is reduced to prevent the deterioration of quality. For example, as shown in Japanese Patent Publication No. Sho 56-116721 and a document (Basic and Analysis of Polymerization Reactor: Yasuhiro Murakami: P33 to P37), ribbon blades are arranged so that the entire inner surface of the container can be scraped off. There is something. A concrete example of this structure with a cylindrical container will be described with reference to FIG. In the figure, stirring power is transmitted from a drive source to a rotary shaft 5 in a stirring tank main body 1 via a rotary power transmission shaft (hereinafter referred to as a rotary ear shaft) 2. A plurality of supporting arms 4a and 4b are horizontally attached to the rotary shaft 5, and ribbon blades 3a and 3b are spirally attached to the tips of the supporting arms 4a and 4b so as to scrape the inner wall of the agitation tank main body 1 thoroughly. Is attached. At the upper part of the stirring tank main body 1, a prepolymerization device 23
A supply port 6 for the liquid to be treated and the additive is provided, and a discharge port 7 for the liquid to be treated is provided in the lower part. When stirring and mixing high-viscosity liquid with this device, the viscosity of the liquid to be treated is several hundred to 1k.
Works well up to Pas (thousands to 10,000 poises),
When the viscosity of the liquid to be treated reaches several kPa · s (tens of thousands of poise), the liquid to be treated adheres to the ribbon blades 3a and 3b, and a co-rotation phenomenon occurs. Further, since the peripheral speed of the surface of the rotary shaft 5 is slow, when the liquid becomes a high viscosity liquid, co-rotation of the liquid to be treated occurs, a dead space is generated, and stirring / mixing performance is deteriorated. Therefore, in the conventional apparatus, the viscosity of the liquid to be treated is up to 1 kPa · s (10,000 poise), and if the viscosity is higher than that, the time for stirring becomes long, and further the quality of the substance to be treated deteriorates due to dead space. There was a problem such as.

Regarding conventional methods for producing general-purpose plastics, etc., refer to the literature (Basic and analysis of polymerization reactor: Yasuhiro Murakami: P13
It is manufactured by the polymerization reaction process as described in 7-P140). When manufacturing a high-performance engineering plastic by the above-mentioned process, the following problems occur. High-performance plastics include, for example, increase in mechanical strength, increase in heat resistance temperature, improvement in weather resistance and chemical resistance, but generally high-performance means increasing the degree of polymerization of the resin, that is, the molecular weight. 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 manufacturing process is limited to 1 kPa · s (10,000 poise). Therefore, it is the 23rd to manufacture high-performance resin (super engineering plastic).
It is manufactured by the process shown in the figure. The conventional process will be described with reference to FIG. Prepare the raw material by adding the monomer and catalyst that are the raw materials for the resin, and then add the solvent for the resin and supply it to the stirring tank in a liquid state with low viscosity, and stir it while maintaining it at the prescribed reaction temperature to carry out solution polymerization. I do. At this time, polymerization by-products generated by the progress of the reaction are removed at any time.
Although the molecular weight of the resin increases with the progress of the reaction, the viscosity of the solution does not increase and is maintained at about several hundred Pa · s (several thousand poises) because it is stirred in the solvent. When the reaction progresses to reach a predetermined degree of polymerization, there is a process of recovering the solvent as the next step. In this process, a demonomerizer, dehydrator,
A drying device or the like is arranged so that only the final polymer separated from the solvent is finally obtained.

Next, another manufacturing method of the high-performance resin (super engineering plastic) will be described with reference to FIG. In this process, a catalyst is added to the monomer, which is the raw material of the resin, and the monomer is adjusted and supplied into the stirring tank. Stir and mix while maintaining the reaction temperature and atmospheric conditions in the stirring tank. At this time, if the polymerization by-products generated by the reaction are removed at any time, the molecular weight of the resin increases with the progress of the reaction, the viscosity of the stirring treatment liquid increases, and a bulk state is formed, resulting in bulk polymerization. When the reaction proceeds further, the viscosity of the treatment liquid reaches the treatment limit viscosity of the stirrer. The intermediate polymer having reached this critical viscosity is discharged to the outside of the stirring tank, and the temperature of the treatment liquid is lowered to the melting point or lower to solidify to form chips. When the chip-shaped intermediate polymer is supplied into another type of stirring device and stirred under a predetermined atmospheric condition, the polymerization reaction proceeds further. The final polymerized product is produced by this solid-state polymerization reaction.

Further, as shown in FIG. 21, the stirring device used for the solution polymerization and bulk polymerization in the conventional manufacturing process is usually composed of a preliminary polymerization device 23 and a polymerization device 25. The prepolymerization device 23 is provided with a stirring blade 24 for low viscosity. This prepolymerization apparatus 23 mainly processes a low-viscosity liquid by stirring and mixing the raw material and the catalyst, and a turbine blade or a paddle blade is used as the low-viscosity stirring blade 24. The treatment liquid that has undergone the pretreatment for polymerization by the prepolymerization device 23 is supplied to the polymerization device 25. Here, predetermined reaction conditions are set and the polymerization reaction proceeds. Medium viscosity stirring blades 3a, 3b used in the polymerization apparatus 25
Usually uses a ribbon blade capable of processing several hundred Pa · s to 1 kPa · s (several thousand poises to 10,000 poises). The polymerized product that has been processed by the polymerization device 25 up to a predetermined polymerization is sent to the next step according to the above-described process. A device related to this type is disclosed in, for example, Japanese Patent Laid-Open No. 62-95122.
No. and Jitsuko Sho 38-38289.

[Problems to be Solved by the Invention]

The above-mentioned prior art does not take into consideration the stirring / mixing treatment of highly viscous substances, and as the liquid to be treated becomes more viscous, the adhesiveness becomes stronger, and as a result, the flow of the liquid to be treated has a large shearing action by stirring. It works only by the ribbon blades, and there is almost no flow in the center of the stirring tank where the shear force does not reach. Further, when the viscosity of the liquid to be treated becomes higher, the adhesive force of the liquid to be treated adhered to the surface of the ribbon blade becomes larger than the shearing force due to the stirring, and the liquid to be treated remains attached to the surface of the ribbon blade and does not move but corotates. As a result, stirring and mixing deteriorate, and the liquid to be treated adheres to the stirring shaft that is less susceptible to shearing force.
There is a drawback that the quality of the adhered matter deteriorates and the quality of the product is deteriorated by stirring and mixing with other processed objects. Furthermore, since the conventional equipment can only handle viscosities up to about 1 kPa · s (10,000 poise), it is necessary to use treatment equipment for other highly viscous substances, which complicates the manufacturing process for high-performance resins and lengthens the manufacturing time. There was a drawback that

It is an object of the present invention to provide an apparatus for producing a highly viscous substance, which has a small amount of retained liquid and can improve quality.

Another object of the present invention is to simplify the manufacturing process by using a stirrer capable of processing even a high-viscosity liquid in the manufacture of a highly functional resin.

Another object of the present invention is to simplify a high-performance resin manufacturing apparatus,
It is to reduce the equipment price.

Further, another object of the present invention is to provide an apparatus and method for producing a polycondensation polymer or the like, which uses the apparatus for producing a highly viscous substance of the present invention, promotes a circulating flow in a container, and can improve surface renewal performance. Especially.

Further, another object of the present invention is to provide an apparatus and a method for producing an addition-polymerized polymer or the like, which uses the apparatus of the present invention to promote the heat transfer action in the container to enhance the effect of removing the heat of polymerization. Especially.

[Means for Solving the Problems]

In order to achieve the above object, the stirring shaft is formed by eliminating the rotating shaft and connecting rectangular frames.

Further, in order to form a circulating flow of the liquid to be treated, a horizontal blade of a rectangular frame is twisted in the rotational direction to incline the side members of the rectangular frame, and a plurality of them are connected to form a stirring blade. is there.

Further, in order to improve the discharge work of the highly viscous substance, the agitating device is provided with a tank pressurizing device and a liquid extraction mechanism for the liquid to be treated.

Further, in order to improve the discharge work of the highly viscous substance, the lower part of the stirring tank has a conical shape.

Furthermore, in order to prevent the liquid to be treated from being lifted up to the upper part of the tank and forming a retention part while stirring the highly viscous substance, the inclination of the stirring blade on the upper part of the tank is set in the opposite direction to the inclination of the stirring blade on the lower side. It was done.

Further, in order to achieve the above-mentioned object, a stirring device having stirring blades connected to a rectangular frame member is used as the polymerization reaction device.

Further, in order to achieve the above object, a heating medium is circulated in the stirring blade member so as to enhance the effect of removing the polymerization heat generated during the polymerization reaction, particularly the addition polymerization type polymer.

[Action]

By setting the stirring blade structure to a connecting structure of rectangular frames without a rotating shaft, it is possible to prevent the liquid to be treated from adhering to the rotating shaft,
Further, by constructing a stirring blade by twisting the mounting angle between the horizontal blade members of the rectangular frame connecting a plurality of them in the rotation direction, the circulation flow that rises the tank wall surface and descends the tank center part is facilitated. Since it can be formed, it is possible to provide a stirrer having a small retention portion.

Further, since the treatment liquid does not adhere to the shaft and the co-rotation phenomenon does not occur which is a problem when treating the high viscosity liquid, stirring with high viscosity can be performed. For this reason, in the conventional process, it was necessary to reduce the stirring viscosity for processing or use a stirring device of a different type from the middle, but if this stirring device is used, even the high-viscosity final polymerized product can be obtained with the same stirring device. Since it can be manufactured by, the manufacturing process can be simplified.

Further, the discharge time of the liquid to be treated can be shortened by using the discharge mechanism for discharging the liquid to be treated provided in the lower part of the stirring tank and the pressurizing mechanism provided in the stirring tank for pressurizing the inside of the tank.

〔Example〕

An embodiment of the present invention will be described below with reference to FIGS. 1 and 2. In the figure, the stirring tank main body 1 is a cylindrical container 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 a rotary power transmission shaft (hereinafter, referred to as a rotating ear shaft) 2 and stirring blade members 8a, 8b,
8c, 8d, 9a, 9b and 9c are combined and connected to form a rectangular frame, and the frames are shifted by θ degrees and connected to form one stirring blade constituent element (lattice blade). As shown in FIG. 2, the present embodiment illustrates the case where θ is 90 degrees, but the value of θ may be any value. As the stirring blade members 8a, 8b, 8c, 8d and 9a, 9b, 9c, 9d, 9f, round rods or plate members are used.

The stirring action of the highly viscous substance in the above configuration will be described. Rotation is transmitted to the stirring blade member 8a by the rotating shaft 2. The rectangular frame constituted by the stirring blade members 8a, 8b, 9a, 9d rotates along the inner wall of the stirring tank main body 1 to stir and mix the liquid to be treated. A stirring blade member 8a installed in a horizontal direction,
8b, 8c, and 8d rotate horizontally in the tank and contribute to stirring and mixing in the radial direction. The vertical stirring blade members 9a, 9d, 9
In b, 9c, 9e, and 9f, since the tank wall surface is scraped all over the tank wall surface, there is no retained portion of the liquid to be treated. Further, the rectangular stirring blade element and the next rectangular stirring blade element are attached at an attachment angle θ, and the next rectangular stirring element is also continuously formed at the attachment angle θ. Therefore, when the high-viscosity liquid is stirred and mixed by the horizontal stirring blade members 8a, 8b, 8c, 8d and the vertical members 9a, 9b, 9c, 9d, 9e, 9f, the position of each blade member is the tank. Since the liquid is distributed to each position inside, the shape of the liquid to be treated formed by stirring 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. Further, since there is no rotary shaft, high-viscosity substances to be treated do not adhere and accumulate, and good stirring and mixing performance can be obtained. In this embodiment, the round blades are used for the stirring blade members 9a, 9b, 9c, 9d, 9e, 9f, but the same effect can be obtained by using plate members.

Next, another embodiment of the present invention will be described with reference to FIGS.
It will be described with reference to the drawings. In the figure, the stirring tank main body 1 is a cylindrical container having a circular cross section, and although not shown, the outside has a heating medium jacket capable of heating and cooling. The stirring blade forms a rectangular frame by combining and connecting the rotating shaft 2 and the stirring blade members 8a, 8b, 9a, 9d to form one stirring blade constituent element (lattice blade). Of the constituent elements of the stirring blade, the stirring blade members 8a and 8b installed horizontally are twisted in the direction of rotation by θ ₂ with the center of the tank as the center of rotation, and are formed so as to scratch the wall surface of the tank. Vertical stirring blade member 9
It is connected to a and 9d respectively. The next stirring blade components also have the same shape, and the horizontal stirring blade member 8b and
It is connected to 8e at a mounting angle θ ₁ . Further, the next stirring blade component is also attached at the same angle to form one stirring blade. The illustrated shape has a mounting angle θ ₁ of 90.
Although the case of degrees is shown, θ ₁ and θ ₂ may be set to arbitrary angles. Also, the stirring blade members 8a, 8b, 8c, 8d, 8e, 8f
For 9a, 9b, 9c, 9d, 9e and 9f, a round bar or a plate-shaped member is used. The stirring action of the highly viscous substance in the above configuration will be described. Stirrer blade member by rotating shaft 2
The rotation is transmitted to 8a. The rectangular frame constituted by the stirring blade members 8a, 8b, 9a, 9d rotates along the inner wall of the stirring tank main body 1 to stir and mix the liquid to be treated. The stirring blade members 8a and 8b installed in the horizontal direction rotate horizontally in the tank and contribute to the radial stirring and mixing. The stirring blade members 9a and 9d, which rotate while scraping the wall surface along the inner wall surface of the tank, are attached by advancing the phase of the stirring blade members 8a and 8b by θ _{2 in the} rotation direction, so that the liquid to be treated near the wall surface of the tank is rotated. The force to lift the Therefore, the rotation of the stirring blade component causes an upward flow of the liquid to be treated in the peripheral portion of the tank, which causes a downward flow in the central portion of the tank.
Further, this stirring blade constituent element is connected to the next stirring blade constituent element while maintaining the mounting angle θ ₁ , and the next stirring blade constituent element is also similarly connected to form the stirring blade. Therefore, each stirring blade component causes a flow upward from the lower part of the tank near the inner wall surface of the tank, and a flow from the upper part to the lower part of the tank in the center part of the tank. No stagnant portion of liquid is obtained, and good stirring and mixing can be obtained.
Here, the flow of the liquid to be treated in the vicinity of the wall surface of the stirring apparatus of this embodiment 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 figure, each of the stirring blade members 9a, 9d, 9b, 9e, 9f, 9c having a rectangular frame has a rotation phase angle θ _{2 and} therefore has a gradient inclined rearward with respect to the traveling direction of the stirring blade. When the stirring blade is rotated in this state, a mass of the liquid to be treated 15 is formed on the front surface of the stirring blade member 9a. As the stirring blade rotates, the entire mass of the liquid to be treated is pushed upward.

At this time, the liquid to be treated 15 is mixed on the front surface of the stirring blade member 9a. In this embodiment, the stirring blade members 9a, 9d, 9b, 9e, 9f, 9c are divided and distributed in the tank. Therefore, for example, part of the liquid to be treated mixed by the stirring blade member 9b overflows rearward from the upper and lower ends of the stirring blade member. A part of this overflowed liquid to be processed merges and mixes with the liquid to be stirred and mixed by the stirring blade members 9a and 9f, which are advancing afterwards, and mixes to obtain uniform stirring and mixing performance in the entire tank. Contribute to the improvement of. Further, FIG. 22 shows a case where the ribbon blade of the conventional apparatus shown in FIG. 21 is developed on a plane. The conventional stirring tanks 3a and 3b are continuously installed in each tank. Therefore, in the conventional stirring blade, the liquid to be treated is pushed up and stirred with the whole liquid while stirring and mixing only the front surfaces of the stirring blade members 3a and 3b. When the viscosity of the liquid to be treated increases, the adhesive force of the liquid to be treated increases and adheres to the surfaces of the stirring blades 3a and 3b, and the movement to the upper side also decreases, and the liquid to be treated becomes a co-rotating state and the stirring / mixing performance Will fall. In the system shown in FIG. 5 described above, since the stirring blade member is divided, it is difficult to cause co-rotation. Further, since the stirring blade members are evenly distributed in the whole tank, the shape of the liquid to be treated by stirring becomes complicated, and the ratio of the surface area of the liquid to the tank volume increases to degas volatile components. This has the advantage of improving the performance and shortening the reaction time in the polymerization reaction operation.
In addition, since there is no rotating shaft, high-viscosity treated substances do not adhere and accumulate, and good stirring performance can be obtained. In this embodiment, a round bar is used as the stirring blade member, but the same effect can be obtained by using a plate member or the like.

Next, another embodiment of the present invention will be described with reference to FIGS. This embodiment is the same as the above-mentioned embodiments in terms of basic components and operation, and has the same effect. In this embodiment, in particular, the stirring blade constituent members 8a and 8b of the stirring blade constituent elements.
The case where the mounting phase θ of is set to 90 degrees is shown. Further, the stirring blade constituent members 9a and 9d are plate-shaped ribbon blades, and the stirring blade constituent elements are connected at a mounting angle θ ₁ of 90 degrees to form a stirring blade. By using the ribbon blade as the stirring blade constituent member, the scraping action of the treatment liquid is further increased, and the circulation flow in the entire tank is strengthened, so that good mixing and stirring effects can be obtained. Also,
Since the ribbon blades are intermittently arranged on the wall surface of the tank, the amount of the liquid to be treated adhering to and staying on the stirring blades is reduced as compared with the case where the ribbon blades are continuously configured, and the stirring / mixing performance is improved.

Next, another embodiment of the present invention will be described with reference to FIGS. This embodiment is the same as the above-mentioned embodiment in terms of basic constituent members and operation, and similar effects can be obtained. In this embodiment, in particular, the lower part of the stirring tank main body 1 has a conical shape, and the rectangular shape is formed on the conical tank wall. With this structure, the liquid to be processed can be easily discharged when the liquid to be processed is discharged, and the liquid can be discharged in a short time.

Further, in the present embodiment, the lower part of the stirring tank main body 1 has a conical shape, the discharging device 10 is provided at the apex of this conical portion, and the pressurizing device 11 capable of pressurizing the inside of the tank is provided on the upstream side of the supply port. The stirring blades thus form a rectangular shape on the conical vessel wall. The stirring blade members 8a and 8b are located at a position twisted in the direction of rotation by θ ₂ with the center of the tank as the center of rotation, and are connected to vertical members 9a and 9d formed so as to scrape the wall surface of the tank, respectively. There is. The next stirring blade component has the same shape, and the horizontal members 8b and 8e are connected at an attachment angle θ ₁ and the following stirring blade components are similarly connected to form a stirring blade. In this embodiment, when the processing liquid is discharged after completion of the stirring or reaction operation, the stirring blade is rotated in a direction opposite to that in the reaction operation, and at the same time, the discharging device 10 is operated, and the pressurizing device is further operated.
The inside of the tank is pressurized by 11 and discharge processing is performed. According to this method, the stirring blade is reversed, so that the liquid to be treated is pushed down below the wall surface of the tank and concentrated in the lower part of the tank. Further, since the inside of the tank is in a pressurized state, it is easy to supply it to the discharge device 10, and there is an advantage that the discharge time of the liquid to be treated can be shortened.

Further, particularly in this embodiment, both ends (9a ₁ , 9a ₂ , 9d ₁ , 9d ₂ , 9b ₁ , 9b of the stirring blade member for scraping the tank wall surface among the stirring blade constituent members are used.
b ₂ , 9e ₁ , 9e ₂ , 9c ₁ , 9f ₁ ) are extended upward and downward respectively from the joint with the horizontal stirring blade member to form a stirring blade constituent element, and these stirring blade constituent elements are connected. And then use it as a stirring blade. The flow of the liquid to be treated in the vicinity of the wall surface of the vertical stirrer of this configuration will be described. FIG. 10 shows a case where the cylindrical circumferential wall surface of the apparatus shown in FIG. 8 is developed on a plane. Since FIG. 10 is almost the same as the content described with reference to FIG. 5, detailed description will be omitted. In this embodiment, in particular, the stirring blade members 9a, 9d, 9b, 9e, 9f, 9c are each divided and distributed in the tank, and since the stirring blade member ends enter the inside of the trajectory of each blade, The mixing of the liquid to be treated overflowing rearward from both ends of the stirring blade member and the liquid to be treated on the front surface of the rear stirring blade member is further improved, which contributes to improvement of uniform stirring / mixing performance in the entire tank. Further, if the mounting angles of the end portions 9a ₁ and 9d ₁ of the blade members are formed in the direction opposite to the inclination of the blade members 9a and 9d, there is also an effect of preventing the processing liquid from adhering and accumulating on the upper part of the tank. Although the discharging device 10 is illustrated as a screw type in this example, 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 embodiment of the present invention will be described with reference to FIG. This embodiment is the same as the above-mentioned embodiments in terms of basic components and operation, and similar effects can be obtained. In this embodiment, in particular, the shape of the stirring tank body 1 is conical (conical), and the stirring blade shape is also conical so as to follow the wall surface of the tank. With the shape of this example, the liquid to be treated spreads along the wall surface of the tank during stirring, and the tank cross-sectional area at the upper part is larger than that of the cylindrical tank, so that the surface area per volume of the liquid to be processed increases. The surface renewal effect is improved. In the polymerization reaction operation of a high-viscosity liquid, the surface renewal performance is the rate-determining reaction time, and improvement of this performance contributes to shortening the reaction time.

Next, another embodiment of the present invention will be described with reference to FIG. This embodiment is the same as the above-mentioned embodiments in terms of basic components and operation, and similar effects can be obtained. In this embodiment, in particular, reinforcing members 20a and 20d are attached vertically to the inside of the rectangular frame of the stirring blade constituents and 20e and 20b are attached to the other rectangular frames to enhance the rigidity of each stirring blade constituent. It is a thing. By attaching this reinforcing member, it is possible to improve the strength of the stirring blade and improve stirring / mixing in the rectangular frame, which contributes to improvement of stirring / mixing performance.

Next, another embodiment of the present invention will be described with reference to FIGS. This embodiment is the same as the above-mentioned embodiments in terms of basic components and operation, and similar effects can be obtained. In the present embodiment, particularly, the rotating ear shaft 2 among the components of the stirring blade is used.
8a, 9a, 8b, 9b and 8
Two sets of g, 21b, 8e, and 21a are connected to form a stirring blade. With this configuration, the number of members of the stirring power transmission portion is increased, 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 constituent elements between 8b and 8c.

Another embodiment of the present invention will be described below with reference to FIGS. 15 and 16. This embodiment is the same as the above-mentioned embodiments in terms of basic components and operation, and similar effects can be obtained. In particular, in the present example, 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, which has been scratched up from the wall surface of the tank, stays in the upper part of the tank and is uniformly stirred. In order to prevent a difficult phenomenon, the stirring blade constituent elements are formed by twisting the installation phase angle of the stirring blade members 8a and 8b in the horizontal direction of the stirring blade constituent elements above the stirring blade by θ _{2 in the} direction opposite to the rotation direction. To do. With this configuration, the inclination of the stirring blade members 9a and 9d that scrape the wall surface of the stirring tank acts so as to push down the processing liquid on the wall surface of the tank when the stirring blade rotates in the operating direction. Therefore, the lower stirring blade component acts to push the liquid to be treated upward along the wall surface of the tank, and the upper stirring blade component pushes down the liquid to be treated, so that the liquid to be treated stays near the upper portion of the tank. Can be prevented and good stirring / mixing performance can be obtained.

Another embodiment of the present invention will be described with reference to FIGS. In the present embodiment, there is one in which the stirring blade constituting member is formed hollow and the rotary shaft 2 is a double tube and the rotary joint 50 is provided at the upper end of the rotary shaft 2. In this embodiment, the rotary joint 50 causes the stirring blade constituent members 8a, 9a, 8b, 8e, 9b.
Furthermore, since the heat transfer medium can be supplied to and circulated through 9e, 8e, 8b and 9b, the heating and cooling operations of the liquid to be treated can be performed rapidly, and the treatment time of the polymerization can be shortened.

Further, at the time of discharging the treatment liquid, the amount of liquid adhering to the surface of the stirring blade can be reduced by supplying the heat medium to the inside of the stirring blade constituent member.

In still another embodiment, there is a method in which a change in the viscosity of the liquid to be treated is detected by detecting the rotation torque of the rotating shaft 2, and the rotation speed of the rotating shaft 2 is changed according to the viscosity. In this embodiment, when the viscosity of the liquid to be treated is low, the rotation speed can be increased to perform strong stirring, and when the viscosity is high, the rotation speed can be decreased to prevent excessive torque. In this case, the viscosity of the liquid to be treated can be directly measured by sampling from a preliminary nozzle (not shown) at regular intervals other than the rotation torque.

Next, another embodiment of the method for producing a highly viscous substance using this apparatus will be described with reference to FIGS. 8 and 19. FIG. 19 shows a schematic flow of the manufacturing process of the high-performance resin (highly viscous substance) of the present invention. This is a method in which a monomer, which is a raw material of a highly viscous substance, and a catalyst are mixed, and an intended final polymer is produced by bulk polymerization by 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 rises to several kPa · s (tens of thousands of poise). When a liquid of several kPa · s (tens of thousands of poise) is treated with an ordinary stirring device, the mixing / stirring performance is poor, so that the degree of polymerization distribution of the product is largely varied and the quality is significantly deteriorated.
Therefore, the stirring apparatus for highly viscous substances shown in FIG. 8 is used to process the final polymer without deteriorating the stirring performance. 8th
The structure and operation of the agitator for highly viscous substances shown in FIGS.

By the stirring blades forming the frame-shaped member of the present invention, the treatment liquid can be circulated in the whole tank, and the stagnant portion of the liquid can be eliminated to obtain good stirring and mixing of the high-viscosity liquid. Therefore, when the polymerization reaction is carried out using the present stirring device, a final polymer having a uniform degree of polymerization can be obtained. Furthermore, the final polymerized product can be produced from the beginning of the polymerization reaction with a single stirrer.

Next, another embodiment of the present invention will be described with reference to FIG. In this embodiment, the prepolymerization device 23 and FIG. 8 or 20 are used.
A high-performance resin (highly viscous substance) is produced by addition polymerization reaction or polycondensation reaction using a stirring device 18 described with reference to the figure to produce an intended final polymer by bulk polymerization. In this example, the low-viscosity liquid at the pre-stage of the polymerization reaction was treated by the pre-polymerization device 23 equipped with the conventional low-viscosity stirring blade 24, and the stirring viscosity provided with the high-viscosity stirring blade 19 from the medium viscosity to the final processed viscosity Device 18
It is processed in the stirring tank 1 of 1. The high-viscosity stirring blade 19 has the same structure and operation as those described in FIG. 8 or FIG. With the above-described structure, the high-performance resin (highly viscous substance) can be manufactured by only 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 is increased, and the surface renewal performance can be improved.
The polymerization rate of polycondensation polymers (polyethylene terephthalate, polybutylene terephthalate polyamide, polyacetal, polycarbonate, etc.) can be increased. Further, according to the present example, since the heat transfer performance of the liquid to be treated is enhanced, it is easy to remove the reaction heat of the liquid to be treated in the polymerization of the addition polymerization type polymer such as polystyrene, and a stable polymerization operation can be performed. it can.

Furthermore, according to this example, since the surface renewal performance and the heat transfer performance from the wall of the main body with the high-viscosity liquid to be treated can be improved, the demonomerization operation and the desolventization operation from the polymer can be performed in addition to the polymerization operation. The device of the present invention is suitable for.

Furthermore, according to the present example, since the circulation speed in the main body can be increased even in the volatile matter removing operation of the powdery particles and the adhesive powdery particles, the device of the present invention is suitable, and further, the chip-shaped polyethylene terephthalate It is also suitable for solid-state polymerization of powder-shaped polymers such as polybutylene terephthalate.

〔The invention's effect〕

According to the present invention, since the rectangular frame member is used to scrape the inside of the tank thoroughly, good stirring and no stagnant portion can be achieved.
Mixing performance is obtained. Further, since there is no rotating shaft that causes co-rotation of the liquid to be treated, it is possible to prevent deterioration of the quality of the liquid to be treated due to stirring and mixing. Further, when the rectangular frame member is provided with a scraping action for the liquid to be treated, a large circulating flow is generated in the tank, and stirring / mixing performance is improved.

Further, since the rectangular frame members are connected and rotated, the shape of the liquid to be treated that is agitated over the entire tank becomes complicated, the ratio of the surface area of the liquid to be processed per tank volume increases, and the surface renewal action increases. This has the effect of improving the degassing performance of the vaporized components. Further, by rotating the stirring blade in the reverse direction, the liquid to be treated can be concentrated in the lower portion of the tank, and the discharge time of the liquid to be treated can be shortened.

Furthermore, according to the present invention, since the high-performance resin (high-viscosity substance) can be produced only by bulk polymerization, the production process can be simplified.

It also has the effect of lowering the cost of manufacturing equipment for high-performance resins.
Further, there is an effect that the reaction time required for producing the high-performance resin can be shortened.

[Brief description of drawings]

FIG. 1 is a schematic view of an apparatus for producing a highly viscous substance according to an embodiment of the present invention, FIG. 2 is a sectional view taken along the line I-I of FIG. 1, and FIG. 3 is a highly viscous material according to another embodiment of the present invention. Schematic of the manufacturing equipment of the substance, 4th
FIG. 5 is a sectional view taken along the line II-II of FIG. 3, FIG. 5 is a development view of the cylindrical circumferential wall surface of FIG. 3, and FIG. 6 is a schematic view of a highly viscous substance manufacturing apparatus according to still another embodiment of the present invention. Figures and 7 are III of Figure 6.
-III sectional view, FIG. 8 is a schematic view of a highly viscous substance producing apparatus according to still another embodiment of the present invention, and FIG. 9 is IV- of FIG.
IV line sectional view, FIG. 10 is a development view of the cylindrical circumferential wall surface of FIG. 8,
FIG. 11 is a schematic view of an apparatus for producing a highly viscous substance according to still another embodiment of the present invention, FIG. 12 is a schematic diagram of an apparatus for producing a highly viscous substance according to yet another embodiment of the present invention, and FIG. FIG. 14 is a schematic view of a highly viscous substance device according to still another embodiment of the present invention, FIG. 14 is a sectional view taken along the line VV of FIG. 13, and FIG. 15 is a process for producing a highly viscous substance according to still another embodiment of the present invention. Schematic of the device, Fig. 16 is VI of Fig. 15
-VI line sectional view, FIG. 17 is a schematic view of a highly viscous substance manufacturing apparatus according to still another embodiment of the present invention, and FIG. 18 is VII-V of FIG.
II sectional view, FIG. 19 is a flow chart of the manufacturing process of one embodiment of the present invention, FIG. 20 is a schematic explanatory view of a bulk polymerization apparatus of another embodiment of the present invention, FIG. 21 is a conventional high viscosity FIG. 22 is a schematic explanatory view of a material manufacturing apparatus, FIG. 22 is a development view of a cylindrical circumferential wall surface in FIG. 21, and FIGS. 23 and 24 are flow charts related to a conventional manufacturing process. 1 ... Agitation tank main body, 2 ... Rotating ear shaft, 6 ... Supply port, 7
...... Discharge port, 8a to 8d …… Stirring blade member, 9a to 9f …… Stirring blade member, 10 …… Discharging device, 11 …… Pressurizing device, 18 …… Stirring device, 19 …… High viscosity stirring blade , 20a, 20b, 20e, 20d …… Reinforcing member, 23 …… Prepolymerization device, 24 …… Stirrer for low viscosity, 25
...... Polymerizer, 31 ...... Wing joint member

Front Page Continuation (72) Inventor Maruko Moriku 502 Jinritsucho, Tsuchiura-shi, Ibaraki Machinery Research Institute, Hiritsu Manufacturing Co., Ltd. (72) Inventor Kazuo Ihara 794, Higashitoyoi, Kudamatsu City, Yamaguchi Prefecture Hitachi Kasado, Ltd. Inside the factory (72) Inventor Takashi Kinoshita 794 Azuma Higashitoyo, Shimomatsu City, Yamaguchi Prefecture Kasado Co., Ltd.Inside the factory (72) Keinobu Furukawa 794 Azuma Higashitoyo, Shimomatsu City, Yamaguchi Corporation Hitachi Kasa Co., Ltd. Inside the To Factory (72) Inventor Kenichi Watanabe 794 Azuma Toyoi, Kudamatsu City, Yamaguchi Prefecture Stock Company Hitachi Ltd. Inside the Kasado Factory

Claims (7)

[Claims] 1. A vertically-arranged cylindrical container or a lower part of the container is installed in a conical container with two horizontal members (8a, 8b) and a wall surface of the container with a minute gap maintained. A rectangular frame is formed by the two vertical members (9a, 9b), and the lower horizontal member (8b) is advanced in phase by θ ₂ degrees in the rotational direction with respect to the upper horizontal member (8a). ,
Frame structure (8a, 9a, 8b, 9
b) and other frame structures (8e, 9e,
8f, 9b) are vertically overlapped, and the lower horizontal member (8b) of the frame structure and the upper horizontal member (8e) of the other frame structure are rotated at the center of rotation. An apparatus for producing a highly viscous substance, characterized in that a stirring blade is formed by connecting the two to each other at a predetermined angle θ ₁ degree and connecting them. 2. The apparatus for producing a highly viscous substance according to claim 1, wherein both ends or one end of the vertical member is projected outside the frame from a position of a horizontal member connected to the vertical member. 3. The lower shape of the container is an inverted conical shape,
A discharge mechanism for extracting the liquid to be treated and a pressurizing mechanism for communicating with the upper portion of the container to pressurize the vapor phase portion in the container are provided at the top of the inverted cone, and the liquid to be treated is operated by operating the discharge mechanism. The high pressure according to claim 1 or 2, characterized in that, when discharging, the stirring blade is rotated in a direction of scraping off the deposits adhering to the inner wall of the container, and the inside of the container is pressurized by the pressing mechanism. Equipment for producing viscous substances. 4. The method according to claim 1, wherein the initial stage to the final stage of the polymerization reaction are carried out in the vessel in a consistent manner.
Or the apparatus for producing a highly viscous substance described in 3. 5. An addition polymerization system by connecting a low-viscosity stirring apparatus equipped with a low-viscosity stirring blade such as a turbine blade or a paddle blade to the high-viscosity substance producing apparatus according to claim 1, 2 or 3. A method for producing a highly viscous substance, which comprises producing a polymer or a polycondensation polymer by bulk polymerization. 6. A vertically-arranged cylindrical container or a container having a lower part of the container having a conical shape with two horizontal members (8a, 8b) and a wall surface of the container provided with a minute gap therebetween. It is formed by two vertical members (9a, 9d), and the lower horizontal member (8b) has a phase θ _{2 in the} rotational direction with respect to the upper horizontal member (8a).
The frame structure (8a, 9a, 8b, 9d) formed in a twisted frame shape by advancing, and other frame structures (8e, 9e, 8e, 9e,
8f, 9b) are vertically overlapped, and the lower horizontal member (8b) of the frame structure and the upper horizontal member (8e) of the other frame structure are rotated at the center of rotation. A method for producing a highly viscous substance, characterized in that a polymerization reaction operation is carried out by means of a stirring blade formed by intersecting and connecting at a predetermined angle θ ₁ degree. 7. A vertically-arranged cylindrical container or the lower part of the container is installed in a conical container with two horizontal members (8a, 8b) and a wall surface of the container with a minute gap maintained. A frame structure (8a, 9a, 8b, 9d) formed into a rectangular frame by two vertical members (9a, 9d), and another frame structure (8e, 9e) formed in the same manner as this frame structure. ,
8f, 9b) are vertically overlapped, and the lower horizontal member (8b) of the frame structure and the upper horizontal member (8e) of the other frame structure are rotated at the center of rotation. An apparatus for producing a highly viscous substance, characterized in that a stirring blade is formed by connecting the two to each other at a predetermined angle θ ₁ degree and connecting them.