JPH09263642A - Continuous polycondensation reaction and device therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a continuous polycondensation reaction method capable of obtaining a high polymerization product in a short time without reducing the flow rate (forming a extremely thin film) of a liquid to be treated by accelerating the evaporation of volatile substances contained in the liquid to be treated, and to provide a device therefor. SOLUTION: A carrying member 3 is spread over plural wheel-like rotators 2a arranged in the upper and lower parts of a container main body 1 and over cylindrical rolls 2b arranged outside the container main body 1. A liquid to be treated is fed on the carrying member 3 with a slit device 4 for feeding the liquid in a film-like shape. Cylindrical rotors 12 for renewing the surface of the liquid to be treated passing on the wheel-like rotators 2a are arranged on the wheel rotators 2a arranged in the container main body 1. A scraper 7 for scraping the treated liquid from the carrying member 3 passing the cylindrical rolls 2b is disposed outside the container main body 1.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polycondensation polymer such as polyethylene terephthalate, polybutylene terephthalate, polycarbonate, polyamide, polybutylene (or butylene) naphthalate, liquid crystal polymer, etc. Manufacturing of
The present invention relates to a continuous polycondensation reaction method and apparatus suitable for removing volatile substances from highly viscous substances.

[0002]

2. Description of the Related Art A conventional technique is disclosed in Japanese Patent Laid-Open No. 63-104602.
As described in Japanese Patent Publication, two cylindrical rotating bodies are installed inside the apparatus body covered with a heat medium jacket, and a conveying member such as a metal plate is stretched over them by belts, and they are electrically heated. Thus, volatile matter is removed from the surface of the liquid to be treated, which is supplied in a thin film form on the surface of the conveying member.

[0003]

When producing a polycondensation polymer, a high polymer cannot be obtained unless the volatile substances generated in the reaction process are removed from the liquid to be treated. The diffusion rate of volatile substances in the liquid to be treated is much slower than the evaporation rate on the liquid surface because the liquid to be treated is usually a highly viscous solution. In order to reduce the amount, it is necessary to make the inside of the reactor a high vacuum or to reduce the thickness of the liquid to be treated.

However, in the former method of making a high vacuum, the design conditions of the reactor are made strict, and a vacuum pump for achieving a high vacuum is required, so that the equipment cost is increased. In the latter method of reducing the thickness of the liquid to be treated, if it is attempted to increase the treatment cost per unit time, in the case of a device such as the prior art, it is necessary to increase the reactor size and the equipment cost is large. Becomes

According to the present invention, by promoting the evaporation of volatile substances in the liquid to be treated, it is possible to obtain a high polymer in a short time without reducing the flow rate of the liquid to be treated (extremely thin film). It is an object to provide a polycondensation reaction method and an apparatus therefor.

[0006]

According to the present invention, in order to solve the above-mentioned problems, a plurality of wheel-shaped rotating bodies are installed in the apparatus main body, and a conveying member such as a metal plate stretched in the rotating bodies is moved. While supplying the liquid to be processed to one side surface of the member in the form of a film, a cylindrical shape installed so as to come into contact with the liquid to be processed when they pass over the wheel-shaped rotating body installed in the upper part of the main body of the device. Provided is a continuous polycondensation reaction method and apparatus in which a polycondensation reaction is allowed to proceed while a surface of a liquid to be treated is renewed by a rotor.

According to the present invention, since the surface of the liquid to be treated can be renewed by the cylindrical rotor installed so as to be in contact with the liquid to be treated, the evaporation of the volatile substances inside the liquid to be treated is promoted and the concentration of the volatile substances is reduced. It becomes possible to produce a high polymer.

Further, the apparatus can be made compact by using a plurality of lines for conveying the liquid to be treated, and the surface can be renewed a plurality of times per pass, so that the evaporation of volatile matter can be further promoted.

Further, according to the present invention, the wheel-shaped rotating body is used for the cut-back portion in the moving direction of the transfer member, so that the cut-back portion at the lower part of the apparatus main body in which the liquid to be treated on the transfer member faces inward. Since the rotating body does not hinder the movement of the liquid to be treated, it is possible to form the transfer line in a plurality of rows, and the apparatus can be made compact.

In the continuous polycondensation reaction method according to the present invention, the inside of the apparatus main body is made into an atmosphere of an inert gas such as nitrogen under atmospheric pressure or a slightly pressurized state of about several mmH ₂ O, and volatile matter generated in the reaction process is removed. The contained inert gas is preferably used without waste by reheating and circulating it in the apparatus body after separating and collecting the contained volatile matter through a condenser installed outside the apparatus body.

Further, in the polycondensation reaction apparatus according to the present invention, a scraping device for scraping the liquid to be treated from the conveying member passing over the cylindrical roll installed outside the main body of the apparatus is provided to keep the conveying member clean. To be kept.

Further, in the polycondensation reaction apparatus according to the present invention, in addition to the above-mentioned structure, a cooling device for cooling the liquid to be treated on the carrying member is provided immediately after the exit of the carrying member of the apparatus main body. The object to be treated that adheres to the conveying member that comes out is solidified to facilitate its removal, and a heating device for preheating the conveying member is provided immediately before the entrance of the conveying member of the apparatus body, and the temperature of the conveying member entering the apparatus body is set. Is preferably maintained at a temperature suitable for the polycondensation reaction.

[0013]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention is shown in FIG.
~ It demonstrates concretely by FIG. In these figures, 1
Is a container body of the continuous polycondensation reactor, the outer periphery of which is covered with a heat insulating material or a heat medium jacket (not shown), and a heating heater (not shown) is installed inside the container body 1. Reference numeral 2a is a wheel-shaped rotating body disposed in the upper and lower parts inside the container body 1, and 2b is a cylindrical roll installed outside the container body 1.

The wheel-shaped rotating body 2a and the cylindrical roll 2
A transport member 3 made of a metal plate or the like for transporting the liquid to be treated 14 is stretched between b. 13 is a transport member 3
Is a cylindrical roll for sending out the powder, and a rotary drive device (not shown) is connected to one end thereof.

On the line of the transfer member 3, there are a heating device 5 for heating the transfer member in advance in front of the entrance of the container body 1, and a supply slit device 4 for supplying the liquid to be treated on the transfer member 3 in the form of a film. A cylindrical rotor 12 for renewing the surface of the liquid to be processed 14 on the wheel-shaped rotating body 2a arranged in the upper part of the container main body 1, and a cooling device 6 for cooling the liquid to be processed 14 exiting the container main body 1. The cooled liquid to be treated 14 is the transport member 3
Each scraping device 7 is installed.

The inside of the container body 1 is filled with an inert gas such as nitrogen, and 8 is a gas sealing device at the entrance / exit of the conveying member 3. The inert gas is circulated by the pump 15 through the pipe 9, and in the middle of the line, condensation for recovering volatile substances in the liquid to be treated contained in the inert gas discharged from the container body 1. A vessel 10 and a heater 11 for reheating the inert gas leaving the condenser 10 are provided.

In the above construction, the cylindrical roll 13 is rotated in the direction shown by the arrow in the figure by the rotation driving device connected to one end of the cylindrical roll 13 installed outside the container body 1 to convey the member 3. Send out.

A liquid to be treated such as an intermediate polymer of polyethylene terephthalate is supplied as a film on the conveying member 3 by the supply slit device 4, moves in the container together with the conveying member 3, and is conveyed by the cylindrical rotor 12 several times on the way. The polycondensation reaction proceeds while the surface is renewed. In addition,
The cylindrical rotor 12 for renewing the surface of the liquid to be treated makes it easier to renew the surface of the liquid to be treated by making the rotational speed larger than that of the rotor 2a or by forming a groove on the rotor.

After completion of the reaction, the liquid to be treated which has come out of the container main body 1 is rapidly cooled and solidified by the cooling device 6 and separated from the conveying member by the scraping device 7 to recover the high polymer.

[0020]

As described above, according to the continuous polycondensation reaction method and apparatus of the present invention, the liquid to be treated supplied in the form of a film is brought into contact with the cylindrical rotor to renew its surface, and Since the contact efficiency between the treatment liquid and the inert gas can be increased, volatile substances in the treatment liquid can be efficiently removed, and the treatment time can be shortened.

[Brief description of drawings]

FIG. 1 is a schematic view of a continuous polycondensation reaction device according to an embodiment of the present invention.

2 is a perspective view partially showing details of a wheel-shaped rotating body and a conveying member used in the continuous polycondensation reaction device of FIG.

FIG. 3 is a detailed view of a contact surface between the wheel-shaped rotating body and the transport member shown in FIG.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Container body 2a Wheel-shaped rotating body 2b Cylindrical roll 3 Conveying member 4 Supply slit device 5 Heating device 6 Cooling device 7 Scraping device 10 Condenser 11 Heater 12 Cylindrical rotor 14 Liquid to be treated

Claims (4)

[Claims] 1. Wheel-shaped rotating bodies having discs attached to both ends of a shaft are installed in the upper and lower portions of the apparatus main body, and a conveying member made of a metal plate or the like stretched between the rotating bodies is moved. , Supplying the liquid to be processed to one surface of the member in a film form, and updating the surface of the liquid to be processed by a cylindrical rotor installed so as to come into contact with the liquid to be processed when they pass over the wheel-shaped rotating body. A continuous polycondensation reaction method, characterized in that the polycondensation reaction is allowed to proceed while being carried out. 2. The inside of the apparatus main body is at normal pressure or several mmH.
An inert gas atmosphere such as nitrogen in a slightly pressurized state of about ₂ O is used, and the inert gas containing volatile substances generated during the reaction process is separated and recovered through a condenser installed outside the main body of the device. After that, the continuous polycondensation reaction method according to claim 1, which is reheated and circulated in the apparatus main body. 3. A transport member made of a metal plate or the like is stretched between a plurality of wheel-shaped rotating bodies installed in the upper and lower parts of the apparatus main body and between cylindrical rolls installed outside the apparatus main body. Provided with a slit device for supplying the liquid to be treated in a film form, on the upper side of the wheel-shaped rotating body installed in the upper part of the apparatus body, of the liquid to be treated on the conveying member passing over the wheel-shaped rotating body. A continuous polycondensation device comprising a cylindrical rotor for renewing the surface, and a scraping device for scraping the liquid to be treated from the conveying member passing over a cylindrical roll installed outside the main body of the device. . 4. A heating device for preheating the transfer member of the apparatus main body is provided immediately before the entrance of the transfer member, and a cooling device for cooling the liquid to be treated on the transfer member immediately after the exit of the transfer member of the apparatus main body. The continuous polycondensation device according to claim 3, which is provided with a device.