JPH03188936A - Method and device for producing high-viscosity material - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to stirring and mixing treatment of high viscosity liquids, particularly for example, liquid crystal polymers (Liquid Crystal Plast).
icsl, polyarylate (Po1.yarylate
This invention relates to the production of highly viscous substances suitable for the production of high-performance engineering plastics such as ).

[Conventional technology]

Generally, in the production of high viscosity substances such as crosstalk and reaction,
Various devices have been devised that reduce the adhesion and circulation of the liquid to be treated within the apparatus, as well as reduce the retention area of the liquid to be treated to prevent quality deterioration. For example, as shown in Japanese Patent Publication No. 56-116721 and the literature (Basics and Analysis of Polymerization Reaction Apparatus: Written by Yasuhiro Murakami: P33-P37), a structure in which ribbon wings are arranged and the entire inner surface of the container can be scraped off is shown. There is something like that. A concrete embodiment of this structure using a cylindrical container will be explained with reference to FIG. 21.

In the figure, stirring power is transmitted from a drive source via a rotary power transmission shaft (hereinafter referred to as a rotary ear shaft) 2 to a rotary shaft 5 in a stirring tank main body 1. A plurality of support arms 4a, 4b are attached to the rotating shaft 5 in the horizontal direction, and ribbon blades 3a, 3b are spirally arranged at the tips of the support arms 4a, 4b so as to scrape the inner wall of the stirring tank body 1 all over. is installed.

A supply port 6 for the liquid to be treated and additives from the prepolymerization device 23 is provided in the upper part of the stirring tank main body 1, and a discharge lower for the liquid to be treated is provided in the lower part. When a high viscosity liquid is stirred and mixed using this device, the viscosity of the liquid to be treated is several hundred to 1 kPa-s (
However, when the viscosity of the liquid to be treated reaches several kPa・S (several hundred poise), the liquid to be treated adheres to the ribbon blades 3a and 3b, causing a co-rotation phenomenon. It happens.

Furthermore, since the peripheral speed of the surface of the rotating shaft 5 is slow, when the liquid becomes highly viscous, the liquid to be treated adheres and rotates together, creating a dead space and deteriorating the stirring and mixing performance. Therefore, in conventional equipment, the viscosity of the liquid to be treated is up to 1 kPa・s (10,000 poise), and when the viscosity becomes higher than that, the time required for stirring becomes longer, and the quality of the treated liquid decreases due to dead space. There were some problems such as:

In addition, regarding conventional manufacturing methods for general-purpose plastics, etc., please refer to the literature (Basics and Analysis of Polymerization Reaction Apparatus, Yasuhiro Murakami: P1
37 to P140). When manufacturing high-performance engineering plastics using the above-described process, the following problems occur. Improving the functionality of plastics includes, for example, increasing mechanical strength, increasing heat resistance, and improving weather and chemical resistance. The goal is to increase molecular weight. When the molecular weight of a resin increases, the melt viscosity of the resin increases.

The processing viscosity of a stirrer used in conventional manufacturing processes is limited to 1 kPa-s (10,000 poise). For this purpose, high-performance resins (super engineering plastics) are produced by the process shown in FIG. 23.The conventional process will be explained with reference to FIG. 23. The raw materials are adjusted by adding 1,000 ml of raw materials for the resin and a catalyst, and then a resin solvent is added and fed into a stirring tank in a low viscosity liquid state. The mixture is stirred while maintaining the predetermined reaction temperature. Perform solution polymerization. At this time, polymerization byproducts generated as the reaction progresses are removed as needed. As the reaction progresses, the molecular weight of the resin increases, but since it is being stirred in the solvent, the viscosity of the solution does not increase and is only several hundred P.
It is maintained at about a-5 (several thousand poise). When the reaction progresses and reaches a predetermined degree of polymerization, the next step is to recover the solvent. This process includes a demonomer equipment,
Dehydration equipment, drying equipment, etc. are installed, and only the final polymer separated from the solvent is obtained.

Next, another method of manufacturing a high-performance resin (super engineering plastic) will be explained with reference to FIG. 24. In this process, a catalyst is added to the raw material for the resin, which is prepared by adding a catalyst, and then fed into a stirring tank. The stirring tank is maintained at a predetermined reaction temperature and atmospheric conditions, and the mixture is stirred and mixed. If the polymerization byproducts generated by the reaction are removed as needed at this time, the molecular weight of the resin will increase as the reaction progresses, and the viscosity of the stirred treatment liquid will increase and become lumpy, resulting in bulk polymerization. As the reaction progresses further, the viscosity of the treatment liquid reaches the processing limit viscosity of the stirring device.

The intermediate polymer that has reached this critical viscosity is discharged outside the stirring tank,
The temperature of the processing liquid is lowered below its melting point to solidify it and make it into chips. The intermediate polymerized product in the form of chips is fed into a different type of stirring device and stirred while maintaining predetermined atmospheric conditions to further progress the polymerization reaction. The final polymer is produced by this in-phase polymerization reaction.

Further, a stirring device used for solution polymerization and bulk polymerization in conventional manufacturing processes is usually composed of a prepolymerization device 23 and a polymerization device 25, as shown in FIG. The prepolymerization device 23 is equipped with stirring blades 24 for low viscosity.
is installed. The prepolymerization device 23 mainly stirs and mixes raw materials and catalysts, and mainly processes low-viscosity liquids, and the stirring blades 24 for low viscosity use turbine blades, paddle blades, or the like. The treatment liquid that has been pretreated for polymerization by the prepolymerization device 23 is supplied to the polymerization device 25 . Here, predetermined reaction conditions are set to allow the polymerization reaction to proceed. This polymerization device 2
The stirring blades 3a and 3b for medium viscosity used in No. 5 are usually several hundred P.
Ribbon blades capable of processing from a-5 to 1 kPa-s (several thousand poise to 10,000 poise) are used. The polymer treated by the polymerization device 25 to a predetermined level of polymerization is sent to the next step according to the process described above. Incidentally, a related example of this type of device is the Zero Ryo 1133.

[Problems to be Solved by the Invention] The above-mentioned prior art does not take into consideration the stirring and mixing treatment of highly viscous substances, and as the viscosity of the liquid to be treated increases, its adhesion becomes more severe, and as a result, The flow of the liquid to be treated is caused only by the ribbon blades which have a large shearing effect due to stirring, and there is almost no flow in the center of the stirring tank where the shearing force does not reach. Furthermore, as the viscosity of the liquid to be treated increases, the adhesion force of the liquid to be treated on the surface of the ribbon blade becomes greater than the shearing force caused by stirring, and the liquid to be treated is attached to the surface of the ribbon blade.
It becomes a co-rotating state without moving with the clothes on. As a result, stirring and
This has the disadvantage that mixing becomes poor, and the liquid to be treated adheres to the stirring shaft, which is not susceptible to shearing force, resulting in quality deterioration of the adhered substance, which is agitated and mixed with other substances to be treated, causing a deterioration in the quality of the product. Ta. Furthermore, since conventional equipment can only process viscosities up to about 1 kPa-s (10,000 poise), other high-viscosity processing equipment must be used, which complicates the manufacturing process for high-performance resins and lengthens the manufacturing time. There was a drawback.

An object of the present invention is to provide an apparatus for producing a highly viscous substance that has a small amount of stagnation of the liquid to be treated and can improve quality.

Another object of the present invention is to simplify the manufacturing process by using a stirring device capable of processing even high viscosity liquids in the manufacturing of high-performance resins.

Another object of the present invention is to simplify the manufacturing equipment for high-performance resin,
The goal is to reduce equipment costs.

Furthermore, another object of the present invention is to provide an apparatus and method for producing polycondensation polymers, etc., which can promote circulation flow in a container and improve surface renewal performance by using the apparatus for producing a highly viscous substance of the present invention. There is a particular thing.

Furthermore, another object of the present invention is to provide an apparatus and method for producing addition polymerization polymers, etc., which uses the apparatus of the present invention and enhances the effect of removing polymerization heat by promoting heat transfer within a container. There is a particular thing.

[Means for Solving the Problem] In order to achieve the above object, the rotating shaft is eliminated and a stirring blade is constructed by connecting rectangular frames.

In addition, in order to form a circulating flow of the liquid to be treated, the horizontal member of the rectangular frame is twisted in the rotational direction, and the side members of the rectangular frame are tilted and connected to form a stirring blade. be.

Furthermore, in order to improve the discharge operation of highly viscous substances, the stirring device is provided with an internal pressure device and a mechanism for extracting the liquid to be treated.

Furthermore, in order to improve the discharge operation of highly viscous substances, the shape of the lower part of the stirring tank is cone-shaped.

Furthermore, in order to prevent the liquid to be treated from being scraped up to the top of the tank and forming a stagnation area while stirring a highly viscous substance, the inclination of the stirring blades at the top of the tank is set in the opposite direction to the slope of the stirring blades at the bottom. This is what I did.

Furthermore, in order to achieve the above object, a stirring device equipped with stirring blades connected to a rectangular frame member is used in the polymerization reaction apparatus.

Furthermore, in order to achieve the above-mentioned object, the structure is such that a heating medium is caused to flow through the stirring blade member so as to enhance the effect of removing the polymerization heat generated during the polymerization reaction, particularly during the production of addition polymer polymers.

[Function] 3 4 By making the stirring blade structure a connected structure of rectangular frames without a rotating shaft, it is possible to prevent the liquid to be treated from adhering to the rotating shaft,
Furthermore, by twisting the installation angle between the horizontal blade members of multiple connected rectangular frames in the rotational direction to form stirring blades, it is possible to easily create a circulating flow that rises up the tank wall and descends in the center of the tank. 6 Furthermore, since the processing liquid does not adhere to the shaft and the co-rotation phenomenon, which is a problem when processing high viscosity liquids, does not occur, it is possible to Stirring is possible. For this reason, in the conventional process, it was necessary to lower the stirring viscosity or use a different type of stirring device midway through the process, but with this stirring device, the same stirring device can be used even for the final high-viscosity polymer. The manufacturing process can be simplified.

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

5 [Example] An example 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 with a circular cross section, and although not shown, the outside has a heat medium jacket that can be heated and cooled. The stirring blades include a rotary power transmission shaft (hereinafter referred to as a rotary ear shaft) 2 and stirring blade members 8a, 8.
b, 8C18d, 9a, 9b, and 9c are combined and connected to form a rectangular frame, and the frames are connected at 0 degree intervals to form one stirring blade component (lattice blade). As shown in FIG. 2, this embodiment shows the case where θ is 90 degrees, but the value of θ may take any value. In addition, stirring blade members 8a, 8b, 8c, 8d and 9
For a, 9b, 9C19d, and 9f, round rods or plate-like members are used.

In the above configuration, the stirring action of the highly viscous substance will be explained. Rotation is transmitted to the stirring blade member 8a by the rotary ear shaft 2. A rectangular frame constituted by stirring blade members 8a, 8b, 9a, and 9d rotates along the inner wall of the stirring tank water body 1 to stir and mix the liquid to be treated. Stirring blade members 8a, 8b, 8c installed in the horizontal direction,
8d rotates horizontally within the tank and contributes to stirring and mixing in the radial direction. Further, vertical stirring blade members 9a, 9d, 9b
, 9c, 9e, and 9f completely scrape the tank wall surface, so that there are no areas where the liquid to be treated remains. Further, this rectangular stirring blade element and the next rectangular stirring blade element are attached with an attachment angle θ, and furthermore, the next rectangular stirring element is also configured to be continuous with an attachment angle θ.

Therefore, the horizontal stirring blade members 8a, 8b, 8c, 8d and the vertical members 9a, 9b, 9c, 9d, 9e, 9
When high viscosity liquids are stirred and mixed at f, the positions of the blade members are distributed at different positions in the tank, so the shape of the liquid to be treated created by stirring becomes complex, and the volume of the tank is The ratio of the surface area of the liquid to be treated to that of the liquid increases. This leads, for example, to improved degassing performance of volatiles in polymerization reaction operations. In addition, since there is no rotating shaft, there is no possibility of highly viscous substances to be treated to adhere and remain, and good stirring and mixing performance can be obtained. In this embodiment, the stirring blade member 9a,
Although the case where round bars are used for 9b, 9C19d, 9e, and 9f is shown, the same effect can be obtained even if plate-shaped members or the like are used.

Next, FIGS. 3 and 4 show other embodiments of the present invention.
This will be explained using figures. In the figure, the stirring tank main body 1 is a cylindrical container with a circular cross section, and although not shown, the outside has a heat medium jacket that can be heated and cooled. The stirring blade combines and connects the rotating ear shaft 2 and the stirring blade members 8a, 8b, 9a, and 9d to form a rectangular frame and forms one stirring blade component (lattice blade). Of the stirring blade components, the stirring blade members 8a and 8b, which are installed in the horizontal direction, are at a position where θ2 is twisted in the rotational direction with the center of the tank as the rotation center, and are formed so as to scrape the tank wall surface thoroughly. The vertical stirring blade members 9a and 9d are respectively connected to the vertical stirring blade members 9a and 9d. The next stirring blade component has a similar shape, and the horizontal stirring blade members 8b and 8e are connected at an angle θ1. Further stirring blade components are also attached at similar angles to form one stirring blade. The illustrated shape shows a case where the mounting angle θ1 is 90 degrees, but θ1, θ2
may be set to any angle.

Further, as the stirring blade members 8a, 8b, 8c, 8d, 8e, 8f and 9a, 9b, 9c, 9d, 9e, 9f, round rods or plate-shaped members are used. In the above configuration, the stirring action of the highly viscous substance will be explained. Rotation is transmitted to the stirring blade member 8a by the rotary 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 to stir and mix the liquid to be treated.

Stirring blade members 8a and 8b installed horizontally rotate horizontally within the tank and contribute to stirring and mixing in the radial direction. In addition, since the stirring blade members 9a and 9d rotate while scraping the wall surface along the tank inner wall surface, the stirring blade members 8a and 8b are installed with a phase advance of 02 in the rotation direction, so that the liquid to be treated near the tank wall surface is rotated. A force that lifts the material upward acts.

Therefore, by rotating this stirring blade component, an upward flow is generated in the liquid to be treated at the periphery of the tank, and a downward flow is thereby generated in the center of the tank. Further, this stirring blade component is connected to the next stirring blade component while maintaining the attachment angle θ, and the next stirring blade component is also connected in the same manner to form a stirring blade. Therefore, each stirring blade component generates a flow upward from the bottom of the tank near the inner wall surface of the tank, and a flow downward from the top of the tank in the center of the tank, creating a circulating flow throughout the tank. There is no stagnation of liquid and good stirring and mixing can be achieved. Here, the flow of the liquid to be treated near the tank wall surface of the stirring device of this embodiment will be explained with reference to FIG. The content of the present invention is particularly suitable when the liquid to be treated has a high viscosity of several hundred poise. FIG. 5 shows the case where the cylindrical inner circumferential wall surface of the stirring tank main body 1 of the apparatus shown in FIG. 3 is developed into a plane. In the figure, since the rectangular frame stirring blade members 9a, 9d, 9b, 9e, 9f, and 9c each have a rotational phase angle θ2, they have a slope inclined backward with respect to the advancing 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 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 member 9a,
9d, 9b, 9e, 9f, and 9C are each divided and distributed in the tank. Therefore, for example, a part of the liquid to be treated being mixed by the stirring blade member 9b overflows backward from the upper and lower ends of the stirring blade member. A portion of this overflowing liquid to be treated joins and mixes with the liquid to be treated which is being stirred and mixed by stirring blade members 9a and 9f that advance later, and the entire tank is uniformly stirred.・Contributes to improving mixing performance. In addition, Fig. 2 shows the case where the ribbon blades of the conventional device shown in Fig. In the stirring blade, the liquid to be treated is stirred and mixed only by the front surfaces of the stirring blade members 3a and 3b, and the entire liquid is pushed upwards and stirred.When the viscosity of the liquid to be treated increases, the adhesive force of the liquid to be treated increases. The amount increases and adheres to the surfaces of the stirring blades 3a and 3b, and movement to the upper side decreases, causing the liquid to be treated to rotate together and the stirring/mixing performance to deteriorate.In the method shown in FIG. Since the agitation blades are divided, they do not rotate together.Also, since the agitation blade members are uniformly distributed throughout the tank, the shape of the liquid to be treated created by agitation becomes complex, and the volume of the tank increases. This increases the ratio of surface area of the liquid to the liquid, leading to improved degassing performance of volatile components, which has the advantage of shortening the reaction time in polymerization reaction operations.Also, since there is no rotating shaft, there is no longer any accumulation of highly viscous substances to be processed. Good stirring performance can be obtained.Although this example shows the case where a round bar is used as the stirring blade member, the same effect can be obtained even if a plate-shaped member or the like is used.

Next, another embodiment of the present invention will be described with reference to FIGS. 6 and 7. This embodiment has the same basic components and operations as the previous embodiment, and has similar effects. In this embodiment, the mounting phase θ of the stirring blade components 8a and 8b is set to 90 degrees. Further, the stirring blade constituent members 9a and 9d are plate-shaped ribbon blades, and the stirring blade portion 1 2 components are connected at an attachment angle θ1 of 90 degrees to form the stirring blade. By using ribbon blades as the stirring blade component, the action of scraping up the processing liquid is further increased, the circulation flow throughout the tank is strengthened, and good mixing and stirring effects can be obtained.

In addition, ribbon wings are placed intermittently on the tank wall, so
Compared to the case where the ribbon blades are configured continuously, the amount of the liquid to be treated that adheres to and remains on the stirring blades is reduced, and the stirring/mixing performance is improved.

Next, another embodiment of the present invention will be described with reference to FIGS. 8 and 9. This embodiment is the same as the above-mentioned embodiment in terms of basic components and operations, and similar effects can be obtained. In this embodiment, in particular, the lower part of the stirring tank body l is conical, and the conical tank wall is formed into a rectangular shape. This structure has the effect that the liquid to be treated can be easily discharged in a short time when the liquid to be treated is discharged.

Further, in this embodiment, the lower part of the stirring tank main body l is conical, and a discharge device 10 is provided at the apex of the conical portion, and a pressurizing device 11 capable of pressurizing the inside of the tank is provided on the upstream side of the supply port. The stirring blade has a rectangular shape on the conical side wall.

Further, the stirring blade members 8a and 8b are twisted in the rotational direction at θ2 with the center of the tank as the center of rotation, and the vertical members 9a and 9d are formed to scrape the tank wall surface all over.
are connected to each other. The next stirring blade component has a similar shape, and the horizontal members 8b and 80 are connected at an attachment angle θ1, and the following stirring blade components are also connected in the same manner to form a stirring blade. In this embodiment, when discharging the treated liquid after the completion of the stirring or reaction operation, the stirring blade is rotated in the opposite direction to that during the reaction operation, and at the same time the discharge device 10 is operated.
Further, the inside of the tank is pressurized by a pressurizing device 11 to perform a discharge process. According to this method, since the stirring blades are reversed, the liquid to be treated is pushed down below the tank wall surface and concentrated at the bottom of the tank. Furthermore, since the inside of the tank is under pressure, it is easy to supply the liquid to the discharge device IO, which has the advantage of shortening the time for discharging the liquid to be treated.

In addition, in this embodiment, in particular, 3 4 of the stirring blade constituent members (9a9a2.9d
,,9cL ,9b,,9b,,9e1.9e2.9
c +, 9f1) are extended upward and downward from the joint with the horizontal stirring blade member, respectively, to constitute a stirring blade component, and these stirring blade components are connected to form a stirring blade. The flow of the liquid to be treated near the tank wall surface of the vertical stirring device of this configuration will be explained. FIG. 10 shows a case where the cylindrical circumferential wall surface of the apparatus shown in FIG. 8 is developed into a plane.

Since the content in FIG. 10 is almost the same as that explained in FIG. 5, detailed explanation will be omitted. In this embodiment, the stirring blade members 9a, 9d, 9b, 9e, 9f, and 9C are each divided and distributed in the tank, and the ends of the stirring blade members are inside the locus of each blade. This further improves the mixing of the liquid to be treated that overflows 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, contributing to improved uniform stirring and mixing performance throughout the tank. Also, the mounting angles of the end portions 9a + and 9d of the wing member are 9a and 9d.
If the blade member is formed in a direction opposite to the inclination of the blade member, it is effective to prevent the processing liquid from adhering and staying in the upper part of the tank. Although the discharge device 10 is shown 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 embodiment in terms of basic components and operations, and similar effects can be obtained. In this example, the shape of the stirring tank body l is particularly conical.
At the same time, the shape of the stirring blades is also conical along the tank wall surface. By adopting the shape of this example, the liquid to be treated spreads along the tank wall surface during stirring, and since the cross-sectional area of the upper part is larger than that of a cylindrical tank, the surface area per volume of the liquid to be treated increases. The surface renewal effect is improved. In polymerization reaction operations of high-viscosity liquids, surface renewal performance is the rate-limiting factor for reaction time, and improving this performance contributes to shortening 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 embodiment with respect to basic components and operations, and similar effects can be obtained. In this embodiment, reinforcing members 20a and 20d are installed vertically inside the rectangular frame of the stirring blade component, and reinforcing members 20e and 20b are attached to another rectangular frame to strengthen the rigidity of each stirring blade component. It is something. By attaching this reinforcing member, the strength of the stirring blade can be improved, and stirring and mixing within the rectangular frame can be improved, contributing to improved stirring and mixing performance.

Next, another embodiment of the present invention will be described with reference to FIGS. 13 and 14. This embodiment is the same as the above-mentioned embodiment in terms of basic components and operations, and similar effects can be obtained. In this embodiment, the stirring blade components 8a, 9a, 8b are particularly connected to the rotary ear shaft 2 among the stirring blade components.
, 9b and 8g, 21b, 8e, and 21a are connected to form a stirring blade. With this configuration, the number of members of the stirring power transmission section is increased, so that the rigidity of the stirring blade is strengthened. In addition, although not shown, the stirring blade component 8b
A similar effect can be obtained by connecting 7 and 80.

Next, regarding other embodiments of the present invention, FIG.
This will be explained with reference to Figure 6. This embodiment is the same as the above-mentioned embodiment in terms of basic components and operations, and similar effects can be obtained. (In this example, in the stirring/mixing operation, especially when processing a liquid to be treated of several kPa-si, tens of thousands of poise, and hundreds of liquids, the liquid to be treated that has scraped up the tank wall remains at the top of the tank and is stirred uniformly. In order to prevent a phenomenon in which it is difficult to
A stirring blade component is formed by twisting the mounting phase angle of 8b by 02 in the opposite direction to the rotation direction. 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 operating direction. Therefore, the lower stirring blade component acts to push the liquid to be treated upward along the tank wall surface, and the upper stirring blade component pushes down the liquid to be treated, so that the liquid to be treated stays near the top of the tank. can be prevented and good stirring/mixing performance can be obtained.

8 Another embodiment of the present invention will be described with reference to FIGS. 17 and 18. In this example, the stirring blade component is formed hollow,
There is one in which the rotary ear shaft 2 is a double tube and a rotary joint 50 is provided at the upper end of the rotary ear shaft 2. In this embodiment, the stirring blade constituent members 8a and 9a are connected to the rotary join h50.
, 8b, 8e, 9b, and further 9e, 8e, 8b, and 9b, a heat transfer medium can be supplied and circulated inside, so heating and cooling of the liquid to be treated can be performed rapidly, and the processing time for polymerization can be shortened. Can be shortened.

Furthermore, when discharging the treatment liquid, by supplying a heat medium into the stirring blade component, the amount of liquid adhering to the surface of the stirring blade can be reduced.

In yet another embodiment, a change in the viscosity of the liquid to be treated is detected by detecting the rotational torque of the rotary ear shaft 2, and the rotational speed of the rotary ear shaft 2 is changed in accordance with the viscosity. In this embodiment, when the viscosity of the liquid to be treated is low, the rotation speed is increased to enable powerful stirring, and when the viscosity is high, the rotation speed is lowered to prevent excessive torque.

In this case, the viscosity of the liquid to be treated can be detected not only by the rotational torque but also by direct measurement by sampling from a preliminary nozzle (not shown) at regular intervals.

Next, another example 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 material) of the present invention. A monomer that is a raw material for a highly viscous substance is mixed with a catalyst, and a desired final polymer is produced by bulk polymerization through 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 hundred kPa-sf tens of thousands of poise. When a liquid of several kPa-s (several hundred poise) is processed using a normal stirring device, the mixing and stirring performance is poor, and the degree of polymerization distribution of the product varies greatly, resulting in a significant drop in quality. Therefore, a highly viscous substance stirring apparatus shown in FIG. 8 is used to process the final polymer without deteriorating the stirring performance.

The structure and operation of the highly viscous substance stirring device shown in FIGS. 8 and 9 have been described above, and will therefore be omitted.

90 The agitation blade forming the frame-like member of the present invention allows the processing liquid to circulate throughout the tank, eliminating a stagnant portion of the liquid and providing good agitation and mixing of the high viscosity liquid. Therefore, if a polymerization reaction is carried out using this stirring device, a final polymer having a uniform degree of polymerization can be obtained. Furthermore, the final polymer can be produced using one stirring device from the beginning of the polymerization reaction.

Next, another embodiment of the present invention will be described with reference to FIG. 20. This example uses the prepolymerization device 23 and the stirring device 18 explained in FIG. It is manufactured by polymerization. In this example, the low viscosity liquid in the preliminary stage of the polymerization reaction is treated with a prepolymerization device 23 equipped with a conventional stirring blade 24 for low viscosity,
The medium to final treatment viscosity is processed in the stirring tank 1 of the stirring device 18 equipped with stirring blades 19 for high viscosity. The stirring blade 19 for high viscosity has the same structure and function as those explained in FIG. 8 or 20. With the above configuration, the high-performance resin 1 (highly viscous material) can be manufactured using only a 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 l can be 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. In addition, according to this example, the heat transfer performance of the liquid to be treated is improved, so in the polymerization of addition polymerization polymers such as polystyrene,
Reaction heat from the liquid to be treated can be easily removed, allowing stable polymerization operations.

Furthermore, according to this example, the surface renewal performance with a high viscosity liquid to be treated and the heat transfer performance from the wall of the main body are improved, so in addition to the polymerization operation, demonomer operation and solvent removal operation from polymers can be performed. The device of the present invention is suitable for.

Furthermore, according to this example, the circulation speed within the main body is increased even in the volatile matter removal operation of powder and sticky powder, so the apparatus of the present invention is suitable. It is also suitable for solid phase polymerization of powder-like polymers such as terephthalate and polybutylene terephthalate.

[Effects of the Invention] According to the present invention, since the rectangular frame member scrapes all over the inside of the tank, it is possible to achieve good stirring and stirring without any stagnant parts.
Mixing performance is obtained. Furthermore, since there is no rotating shaft that causes the liquid to be processed to rotate together, it is effective in preventing deterioration in the quality of the liquid to be processed due to stirring and mixing. Furthermore, if the rectangular frame member has a scraping effect on the liquid to be treated, a large circulating flow will be generated within the tank, improving the stirring and mixing performance.

In addition, since the rectangular frame members are connected and rotated, the shape of the liquid to be treated that is 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 increases. This has the effect of improving the degassing performance of evaporated components. Furthermore, by rotating the stirring blade in the opposite direction, the liquid to be treated can be concentrated in the lower part of the tank, thereby shortening the time for discharging the liquid to be treated.

Furthermore, according to the present invention, a highly functional resin (highly viscous material) can be manufactured only by bulk polymerization, so the manufacturing process can be simplified.

It also has the effect of lowering the cost of manufacturing equipment for high-performance resins.

Furthermore, it has the effect of shortening the reaction time required to produce high-performance resins.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram of an apparatus for producing a high viscosity substance according to an embodiment of the present invention, FIG. 2 is a sectional view taken along the line I-I in FIG. Schematic diagram of substance manufacturing device, 4th
The figure is a sectional view taken along the line II-If of FIG. 3, FIG. 5 is a developed view of the cylindrical circumferential wall surface of FIG. 7 is a sectional view taken along the line IIT-III in FIG. 6, FIG. 8 is a schematic diagram of a highly viscous substance manufacturing apparatus according to another embodiment of the present invention, and FIG. 9 is 1' in FIG. 8. A sectional view taken along the line V-TV, FIG. 1O is a developed view of the cylindrical circumferential wall surface of FIG.
3 4 A schematic diagram of a high viscosity substance manufacturing apparatus according to still another embodiment of the present invention, FIG. 13 is a schematic diagram of a high viscosity substance production apparatus according to still another embodiment of the present invention, and FIG. 15 is a schematic diagram of a highly viscous substance manufacturing apparatus according to another embodiment of the present invention, FIG. 16 is a sectional view taken along the VT-Vl line of FIG. 15, and FIG. A schematic diagram of a highly viscous substance manufacturing apparatus according to still another embodiment of the invention, FIG.
■ Line sectional view, Figure 19 is a flow diagram of the manufacturing process of one embodiment of the present invention, Figure 20 is a schematic explanatory diagram of a bulk polymerization apparatus of another embodiment of the present invention, and Figure 21 is a conventional high viscosity polymerization apparatus. A schematic explanatory diagram of a substance manufacturing apparatus, FIG. 22 is a developed view of the cylindrical circumferential wall surface of FIG. 21, and FIGS. 23 and 24 are flowcharts of a conventional manufacturing process, respectively. 1--11--Stirring tank body, 2-----One rotation ear shaft,
Supply port, 7-1---Discharge port, Stirring blade member, 9a to 9f---Stirring 10--1-
--Discharge device, 11-----1 Pressurized stirring device, 19
------1 High viscosity stirring 8a to 8d Blade member, 18 Stirring blade, 20a, 20b, 20e, 20d Prepolymerization device, 24 25-----1 Polymerization device, 31 Reinforcement member, 23 1 Stirring blade for low viscosity, 1111 blade joint member 5 6' 4/4 figure JP-A-3-188936 (14)

Claims (1)

[Scope of Claims] 1. A cylindrical or cone-shaped container installed substantially vertically has a rotating ear shaft, and a stirring blade having one or more frame-shaped members connected to the rotating ear shaft is provided, An apparatus for producing a highly viscous substance, characterized in that the stirring blade is configured to stir the inside of the container. 2. Production of the highly viscous substance according to claim 1, wherein the stirring blade is constructed by maintaining the attachment angle between the horizontal blade members of one or more frame-like members connected to each other at a predetermined angle. Device. 3. The apparatus for producing a highly viscous substance according to claim 2, characterized in that a blade member is provided vertically or horizontally inside one or more frame-shaped members connected to each other to constitute a stirring blade. 4. A claim characterized in that a stirring blade component is provided in which a plurality of frame-like members are installed in the same rotating plane, and one or more of the stirring blade components are connected in a vertical direction to constitute a stirring blade. 3. The apparatus for producing a highly viscous substance according to item 1. 5. A claim characterized in that the lower part of the stirring tank has a cone shape, and a part of the stirring blade is constituted by a frame-shaped member in which the horizontal blade member is adjusted so as to scrape the inner wall surface of the cone-shaped container. 3. The apparatus for producing a highly viscous substance according to item 1. 6. The lower part of the stirring tank is shaped like a cone, and the lower part of the cone-shaped container is equipped with a discharge mechanism for extracting the liquid to be treated, and a pressurizing mechanism for pressurizing the gas phase inside the tank. The apparatus for producing a highly viscous substance according to claim 1. 7. The horizontally installed blade members of a plurality of connected frame-like members are twisted together at a predetermined angle around the rotation center of the stirring blade, and the frame-like members are twisted so that the members along the tank wall are inclined. Claim 1, characterized in that the agitating blade is formed to form an agitating blade and maintains a mounting angle between each frame member at a predetermined angle.
An apparatus for producing the highly viscous substance described above. 8. The stirring blade is configured such that the twisting direction of the horizontal blade member of the frame-shaped member at the top of the stirring tank is opposite to the twisting direction of the horizontal blade member of the frame-shaped member in the next stage. The apparatus for producing a highly viscous substance according to claim 1. 9. The inside of the frame-shaped or rectangular frame member has a hollow structure,
Claim 7, characterized in that the inside of the agitating blade constituted by the frame member is communicated, and the heating medium is circulated by a heating and cooling device for the heating medium provided externally in the hollow part. High viscosity substance manufacturing equipment. 10. A claim characterized in that the stirring blade component is formed by extending both ends of the stirring blade component that scrapes the tank wall surface upwardly or downwardly from the joining part with the horizontal stirring blade member, respectively. The apparatus for producing a highly viscous substance according to item 7. 11. The stirring tank is apparently divided into multiple stages in the direction of the central axis, and each stirring tank is provided with a band-shaped or rod-shaped spiral blade member symmetrically with respect to the center of rotation, and the upper and lower ends of the installed spiral blade members are respectively A stirring blade component is formed by connecting a plurality of stirring blade components by horizontally installed blade members, a stirring blade is constructed by connecting a plurality of the stirring blade components, and one end of the stirring blade is connected to a rotary ear shaft. Highly viscous substance manufacturing equipment. 12. Addition polymerization polymers or polycondensation polymers can be produced by connecting one or more of the device according to claim 7 or 11 and a stirring device for low viscosity equipped with turbine blades or paddle blades, etc. 1. An apparatus for producing a highly viscous substance, characterized in that the production is performed by bulk polymerization. 13. A cylindrical or cone-shaped container installed substantially vertically has a rotating ear shaft, and a stirring blade in which a plurality of roughly rectangular frames are connected to the rotary ear shaft is provided, and a container to be treated is placed at the bottom of the stirring tank. The stirring tank is equipped with a discharge mechanism that extracts the liquid and a pressurizing mechanism that pressurizes the inside of the tank. When discharging the liquid to be treated, the stirring blade is rotated in the direction of scraping down the deposits on the tank wall to the bottom of the tank, and the inside of the stirring tank is 1. An apparatus for producing a highly viscous substance, characterized in that it is configured to pressurize and operate a discharge mechanism. 14. The horizontally installed blade members of a plurality of connected frame-like members are twisted each other at a predetermined angle around the rotation center of the stirring blade, and the frame-like members are arranged so that the members along the tank wall are inclined. 14. The apparatus for producing a highly viscous substance according to claim 13, characterized in that the agitating blades are configured such that the frame members are formed at a predetermined angle and maintain a mounting angle between the respective frame members at a predetermined angle. 15. A method for producing a highly viscous substance, in which the liquid to be treated is stirred in the same stirring tank, and the viscosity of the liquid to be treated increases as the reaction progresses, which is a polymerization reaction operation until the final high viscosity polymer is produced. A method for producing a highly viscous substance, characterized in that it is carried out by reaction. 16. The method for producing a highly viscous substance according to claim 15, characterized in that the rotation speed of the stirring blade is changed in accordance with a change in the viscosity of the liquid to be treated. 17. Manufacture a polymer compound by bulk polymerization reaction until the final high-viscosity polymer is produced in the same cylindrical or cone-shaped stirring tank in which multiple frame-shaped members are held at a predetermined angle and connected to form stirring blades. 16. The method for producing a highly viscous substance according to claim 15. 18. The highly viscous substance according to claim 15, wherein the addition polymerization polymer or polycondensation polymer, in which the viscosity of the liquid to be treated increases as the reaction progresses, is produced by bulk polymerization. manufacturing method. 19. The method according to claim 15, characterized in that by rotating the stirring blade, the amount of heat transferred to the liquid to be treated is increased, the surface renewal performance is improved, and by-products from the liquid polymer are removed. Method for producing highly viscous substances.