JPH0852334A - Continuous stirring device for high viscosity solution and continuous bulk polymerization method - Google Patents

Abstract

PURPOSE:To accelerate reaction by efficiently mixing an addition soln. with a high viscosity soln. to be treated by allowing stirring members on an inlet side to approach each other to increase the surface areas of them and reducing the surface areas of stirring members on an outlet side to increase the stagnation quantity of the soln. to be treated. CONSTITUTION:The outer periphery of an oblong cylindrical main body container 1 is covered with a heating medium jacket and two rotary shafts 2 are attached to both ends in the internal longitudinal direction of the container 1. Drop-shaped flat stirring members are attached to the rotary shafts 2a, 2b in a zigzag fashion and rotated in close vicinity to the flat surfaces and leading ends of the respective adjacent members 3. The surface areas of the stirring members 3 on the inlet side of a soln. to be treated are increased to apply shearing to the soln. to be treated. Rod like rectangular stirring members 4 are provided between rotary shafts 2c, 2d to be rotated so that the leading ends of them approach each other. The surface areas of the stirring members 4 on the outlet side of the soln. to be treated are reduced to increase the stagnation amt. of the soln. to be treated.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a stirring method and apparatus for highly viscous substances, and more particularly to polyethylene terephthalate,
The present invention relates to an apparatus suitable for polymerizing a polycondensation polymer such as polycarbonate.

[0002]

2. Description of the Related Art Conventionally, as a continuous processing apparatus in which another substance is added to a highly viscous substance and mixed and reacted, JP-A-63-2
As disclosed in Japanese Patent No. 68734, there is a twin-screw kneading machine in which another substance is added to a part of the highly viscous substance and mixed, and then the mixture is reacted in another horizontal twin-screw disc stirrer.

[0003]

However, the above-mentioned prior art requires a twin-screw kneader to add and mix another substance, and further requires a pipe and a transfer device from the kneader to the horizontal twin-screw disk stirrer. Met.

The object of the present invention is to improve the above-mentioned prior art,
It is an object of the present invention to provide a continuous processing apparatus and method in which another substance is added to a highly viscous substance in one device, mixed and reacted.

[0005]

The above-mentioned object is to increase the surface area of the stirring member that gives a shear to the liquid to be treated by bringing the stirring members on the inlet side of the liquid to be treated close to each other.
This is achieved by reducing the surface area of the stirring member that gives shear to the liquid to be treated by bringing the stirring members on the outlet side of the liquid to be processed closer to each other and increasing the retention amount of the liquid to be treated.

[0006]

[Function] The high-viscosity liquid to be treated has the shearing force strengthened at the inlet side of the container to efficiently mix the added liquid, and then the residence amount is increased at the outlet side of the container to cause a stirring action and the reaction proceeds. .

[0007]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT An embodiment of the present invention is shown in FIGS. 1, 2, 3 and 4. In FIG. 1, reference numeral 1 denotes a horizontally elongated main body container, the outer periphery of which is covered with a heat medium jacket (not shown), and two rotary shafts 2 are attached to both ends in the inner longitudinal direction. Among these rotary shafts 2, a drop-shaped plate-shaped stirring member 3 is attached to the rotary shafts 2a and 2b on the inlet side of the liquid to be treated (left side in FIG. 1) in a small pattern, and each member 3 The plate-shaped surface and the tip of the member 3 are arranged so as to rotate in proximity to the surface and the tip of the stirring member 3 on the other side. A plurality of rod-shaped rectangular frames are provided between the rotating shafts 2a and 2b on the inlet side (left side in FIG. 1) and the rotating shafts 2c and 2d on the outlet side (right side in FIG. 1) of the liquid to be treated.
Stirring members 4 having a shape connected at a phase angle of degrees are attached such that the tips of the respective rectangular frames rotate close to the rotation center of the stirring member 4 on the other side. The horizontally long cylindrical main body container 1 has an eyeglass-shaped cross section as shown in FIG. 3 on the inlet side (left side of FIG. 1) of the liquid to be treated, and a drop-shaped plate-shaped stirring member 3 is formed on the inner wall of the main body container 1. It is a structure that can be scraped over the entire surface. On the other hand, the outlet side of the liquid to be treated (right side in FIG. 1)
Then, as shown in FIG. 4, the cross section of the main body container 1 has a stirring member 4
Has a space in the upper part and a lower part in cross section formed in a W shape so that the stirring member 4 can scrape off the inner wall of the lower half of the main body container 1.

Here, in order to increase the shearing force at the inlet side of the liquid to be treated, the blade width L1 (FIG. 1) of the stirring member 3 is set to 0.05 to 0.2 times the blade radius R, and the outlet of the liquid to be treated is set. On the side, it is recommended to set the blade width L2 of the stirring member 4 to 0.3 to 1.5 times the blade radius R in order to increase the retention amount.

One end of the rotary shaft 2 is connected to a driving device (not shown), and the stirring members 3 and 4 rotate in a direction to lift the liquid inside. An inlet nozzle 5 for the liquid to be treated is provided below one end (left side in FIG. 1) of the main body container 1, and a small amount of the additive liquid is added to the side face of the inlet nozzle 5 by the additive liquid inlet nozzle 6
Is attached. The lower part of the other end of the main body container 1 (see FIG.
An outlet nozzle 7 for the liquid to be treated is provided on the right side of the figure, and an outlet nozzle 8 for volatile matter is provided on the upper part of the container 1.
The volatile matter outlet nozzle 8 is connected to a condenser and a vacuum pump (not shown) by piping. Further, 9 is a shaft sealing device for the rotary shaft 2.

In such an apparatus, the low-viscosity liquid to be treated continuously supplied from the inlet nozzle 5 and the small amount of additive liquid supplied from the additive liquid inlet nozzle 6 are first a drop-shaped plate-shaped stirring member 3. The liquid to be treated is agitated by a strong shearing force and the trace amount of low viscosity liquid in the liquid to be treated is efficiently mixed. Then, the liquid to be treated, in which a small amount of low-viscosity liquid is sufficiently dispersed, is continuously stirred by a stirring member 4 constituted by a rod-shaped rectangular frame while maintaining a predetermined retention amount, and a surface renewal action is given to perform a treatment such as a polymerization reaction. It becomes a highly viscous liquid. Then, the high-viscosity liquid to be treated is discharged from the system through the outlet nozzle 7. On the other hand, the by-products and the like generated by the reaction and vaporized are discharged from the system through the volatile matter outlet nozzle 8. At this time, the liquid to be treated is given a strong shearing force on the inlet side of the main body 1 to efficiently mix a small amount of low-viscosity liquid in the liquid to be treated, and agitate while maintaining a predetermined retention amount on the outlet side of the main body 1. Since a renewal action is given, it is possible to add another substance to a highly viscous substance and mix them in one device to cause a reaction.

When the polyethylene terephthalate is polymerized by such an apparatus, the intermediate polymer of the liquid to be treated is continuously supplied from the inlet nozzle 5 and a small amount of the additive liquid mixed with the catalyst, the inorganic pigment and the like is added to the additive liquid inlet. Nozzle 6 is continuously added to the main body 1
On the inlet side of the inside, the liquid is agitated by the drop-shaped plate-shaped agitating member 3 and the trace amount of the additive liquid is efficiently mixed with the liquid to be treated. Then,
By stirring with the stirring member 4 on the outlet side of the main body 1, volatile substances such as ethylene glycol generated in the polymerization reaction are removed by evaporation, and the polycondensation reaction proceeds to form a highly viscous polymer. Volatile substances such as ethylene glycol separated during this period are discharged from the outlet nozzle 8. The operating conditions at this time are, for example, a temperature of 260 to 300.
C, pressure 0.01 to 10 kPa, rotation speed 5 to 30 rpm
It is done in the range of. Then, the polymer is discharged from the system through the outlet nozzle 7. At this time, since the polymer is agitated in the container 1 in a substantially complete self-cleaning state, deterioration due to retention does not occur, and a product polymer of good quality can be obtained.

As described above, the present invention can be applied to continuous bulk polymerization of polycondensation resins such as polyamide and polycarbonate in addition to polyethylene terephthalate. It can also be applied to continuous bulk polymerization of addition polymerization resins such as polystyrene.

According to the preferred embodiment of the present invention, FIG.
As shown in FIGS. 6 and 6, two rotary shafts 2 are penetrated through the main body 1, and the stirring member 4 on the outlet side of the liquid to be treated is a member 4a in which a scraping plate 10 is attached to the tip of an annular plate at a right angle. There is one in which the tip ends of the respective members are attached to the respective rotating shafts 2 so that the tips of the respective members rotate close to the rotation center of the stirring member 4a on the other side. According to the present embodiment, the scraping plate 10 scoops up and drops the liquid to be treated to enhance the surface renewal action and improve the reaction efficiency in the medium viscosity range.

According to another preferred embodiment of the present invention,
As shown in FIG. 7, there is one in which the additive liquid inlet nozzle 6 is directly attached to the lower portion of the main body 1 on the inlet side of the liquid to be treated. According to the present embodiment, since the additive liquid can be added to the liquid under stirring and flowing, it is possible to prevent the additive liquid from staying in the inlet nozzle 5 of the liquid to be treated, and efficiently add the liquid and the liquid to be treated. Can be mixed.

According to still another preferred embodiment of the present invention, as shown in FIG. 8, the second inlet nozzle 1 for the liquid to be treated is provided.
1 is additionally attached near the lower part of the connecting portion of the inlet side stirring member 3 and the outlet side stirring member 4 of the liquid to be treated of the main body 1. According to the present embodiment, the additive liquid can be premixed at the inlet portion of the main body 1 in a state where the additive liquid concentration is high, and then finally mixed into the liquid to be treated supplied from the second inlet nozzle. When the amount is very small, efficient mixing is possible.

[0016]

According to the present invention, it is possible to add another substance to a highly viscous substance and mix them with one device to cause a reaction.
A product polymer of good quality can be efficiently obtained.

[Brief description of drawings]

FIG. 1 is a plan sectional view showing an embodiment of the present invention.

FIG. 2 is a sectional view taken along line II-II in FIG.

3 is a sectional view taken along line III-III in FIG.

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

FIG. 5 is a sectional plan view showing another embodiment of the present invention.

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

FIG. 7 is a vertical sectional view showing still another embodiment of the present invention.

FIG. 8 is a vertical sectional view showing still another embodiment of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Main body container, 2 ... Rotating shaft, 3 ... Drop-shaped plate-shaped stirring member, 4 ... Stirring member having a shape in which a rod-shaped rectangular frame is connected, 5 ... Inlet nozzle for liquid to be treated, 6 ... Additive liquid inlet nozzle, 7 ... Exit nozzle for liquid to be treated, 8 ... Exit nozzle for volatile matter, 9 ... Shaft sealing device.

Claims (6)

[Claims] 1. A substantially horizontal container having an inlet and an outlet for a liquid to be treated at one end and the other end in the longitudinal direction, respectively, and a stirring member attached to each of two rotary shafts provided in the longitudinal direction inside the container. In the device in which the stirring members rotate close to each other inside the other stirring member, the stirring members on the inlet side of the liquid to be treated are brought close to the other stirring members to give shear to the liquid to be treated. Increase the surface area of the stirring member, reduce the surface area of the stirring member that makes the stirring member on the outlet side of the liquid to be processed close to each other's stirring member and shear the liquid to be treated, and increase the retention amount of the liquid to be processed. By doing so, the shearing force is strengthened on the inlet side of the liquid to be treated and the retention amount is increased on the outlet side of the liquid to be treated. 2. The blade width of the stirring member on the inlet side of the liquid to be treated is 0.05 to 0.2 times the radius of the blade, and the blade width of the stirring member on the outlet side of the liquid to be treated is claim 2. Wing radius 0.3 ~
Continuous stirring device for high-viscosity liquid that is 1.5 times. 3. The stirring member according to claim 1, wherein the stirring member on the inlet side of the liquid to be treated is a drop-shaped plate member, and the surfaces of the members rotate in proximity to each other's stirring member. As described above, the rotary shaft on the outlet side of the liquid to be treated is eliminated, and a stirring member having a shape in which a plurality of rod-shaped rectangular frames are connected to the rotary shaft is connected to the rotary shafts so that they are opposed to each other. Continuous stirring device for high-viscosity liquid that rotates close to the center of rotation of the side stirring member. 4. The agitation member on the inlet side of the liquid to be treated is a drop-shaped plate-like member, and the surfaces of the members rotate in proximity to each other's agitation member. As described above, the stirring member on the outlet side of the liquid to be treated is a member in which the scraping plate is attached at a right angle to the tip of the annular plate as described above. Continuous stirring device for high-viscosity liquids installed on each rotating shaft so as to rotate close to the center of rotation. 5. The second inlet nozzle for the liquid to be treated according to claim 1, wherein the second inlet nozzle for the liquid to be treated is additionally attached near the lower portion of the connecting portion between the inlet-side stirring member and the outlet-side stirring member for the liquid to be treated,
A continuous stirring device for high-viscosity liquids, which is capable of additionally mixing the liquid to be treated. 6. The method according to claim 1, 2 or 3, wherein the stirring member on the inlet side of the liquid to be treated continuously mixes with a small amount of the liquid added to the high-viscosity liquid, and subsequently the stirring on the outlet side of the liquid to be treated. A continuous bulk polymerization method of a polycondensation resin, in which a mixed liquid is continuously reacted by a member.