JP3396367B2 - Continuous polycondensation reaction method and apparatus - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to forming high molecular weight polymers by condensation reaction or the like, such as polyethylene terephthalate, polybutylene terephthalate, polycarbonate,
The present invention relates to a continuous polycondensation reaction method and apparatus suitable for production of polycondensation polymers such as polyamide, polyethylene naphthalate, polybutylene naphthalate, and liquid crystal polymer, and removal of 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. Further, in the latter method of reducing the thickness of the liquid to be treated, if the amount of treatment per unit time is to be increased, 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]

In order to solve the above-mentioned problems, the present invention has a plurality of cylindrical rotors installed in an upper part and a lower part in a main body of an apparatus, and includes a metal plate spread between the rotors. While moving the member at a constant speed, the liquid to be treated is supplied in a film form on one surface of the member, and the inert gas injected from the rotor surface when they pass over the cylindrical rotor installed in the lower part. Thus, there is provided a continuous polycondensation reaction method and apparatus in which the surface of the liquid to be treated is renewed (the inner liquid is newly exposed to the surface) to allow the polycondensation reaction to proceed.

According to the continuous polycondensation reaction method and apparatus of the present invention, the surface of the liquid to be treated can be renewed by injecting an inert gas onto the surface of the liquid to be treated. When the liquid mass also comes into contact with the gas phase portion, the evaporation of the volatile substance is promoted and the concentration of the volatile substance in the liquid to be treated can be reduced.

[0008] In addition, the apparatus can be made compact by using a plurality of lines for conveying the liquid to be treated in the main body of the apparatus, and the number of times of renewal of the surface of the liquid to be treated can be increased to promote evaporation of volatile matter. .

As described above, in the continuous polycondensation reaction method and apparatus according to the present invention, the inert gas is jetted from the surface of the cylindrical rotor installed in the lower part of the main body of the apparatus to the surface of the transfer member to transfer the material to the cylindrical rotor. Since the member and the member can be held in a non-contact state, it is possible to form a plurality of lines of the transfer line, which cannot be performed by the conventional method, and the device can be made compact.

In the continuous polycondensation reaction method according to the present invention, the inside of the apparatus main body is made to have an atmosphere of an inert gas such as nitrogen under a normal pressure or a slightly pressurized state of several mmH ₂ O, and volatile substances generated in the reaction process are removed. The inert gas contained is preferably sent to a condenser installed outside the apparatus main body to recover the volatile substances contained therein, and then heated to a predetermined temperature to be circulated in the apparatus main body.

In addition, in the continuous polycondensation reaction apparatus according to the present invention, in addition to the above-mentioned structure, a scraping apparatus is provided outside the apparatus main body for scraping the liquid to be treated on the conveying member. As a result, the surface of the transport member is always kept clean.

Further, in the continuous polycondensation reaction apparatus according to the present invention, a heater for preheating the carrying member is provided immediately before the entrance of the carrying member of the apparatus body, and on the carrying member immediately after the exit of the carrying member of the apparatus body. It is preferable to provide a cooler for cooling the liquid to be treated. As a result, the liquid to be treated adhering to the conveying member coming out of the apparatus main body is solidified to facilitate its removal, and the temperature of the conveying member entering the apparatus main body is maintained at a temperature that does not hinder the reaction. be able to.

[0013]

BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the present invention will be described below with reference to FIGS. In the figure, reference numeral 1 is a container body of a continuous polycondensation apparatus, in which a heater (not shown) for heating is installed, and the outer circumference is covered with a heat insulating material or a heat medium jacket. Reference numerals 2a and 2b denote cylindrical rotors installed in an upper portion and a lower portion, respectively, inside the container main body, and a compressor 8 for injecting heated inert gas from the surface thereof is connected to the lower cylindrical rotor 2b. Has been done.

Reference numeral 2c is a cylindrical rotor installed outside the container body. A transport member 3 for the liquid to be treated is stretched between the cylindrical rotors 2a, 2b and 2c. On the line of the transport member 3, a cylindrical roll 7 for sending the transport member 3, a heating device 5 for preheating the transport member immediately before the entrance of the container body, and a liquid to be treated on one surface of the transport member are treated. A supply slit device 4 for supplying a film, and a cooling device 6 for cooling the liquid to be treated immediately after the outlet of the container body,
A scraping device 13 for scraping the cooled liquid to be processed from the transport member is installed.

The interior of the container body 1 is filled with an inert gas such as nitrogen, and 9 is a sealing device at the entrance / exit of the conveying member. The inert gas is circulated by a pump 14 through a pipe 10, and a condenser 11 for separating and recovering a volatile substance generated in a reaction process contained in the inert gas on the way is discharged from the condenser 11. A heating device 12 is provided to reheat the inert gas to the temperature inside the container body.

In the continuous polycondensation reaction device having the above-mentioned structure, the cylindrical roll 7 is rotated in the direction of the arrow in the figure by the rotation driving device connected to one end of the cylindrical roll 7 installed outside the container body 1. Then, the transport member 3 is sent 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 and moves in the container body 1 together with the conveying member.

During the movement, the liquid to be treated transferred in the container body 1 is generated by the inert gas injected from the slit 15 (FIG. 2) on the surface of the cylindrical rotor 2b installed in the lower part of the container body 1. The polycondensation reaction proceeds while the surface is renewed. After completion of the reaction, the liquid to be treated that has left the container body 1 is cooled by the cooling device 6, and scraped and collected by the scraping device 13.

The present invention has been specifically described above based on the illustrated embodiments, but the present invention is not limited to these embodiments and within the scope of the present invention as set forth in the claims, a concrete structure thereof. It goes without saying that various changes may be added to the.

[0019]

As described above, according to the continuous polycondensation reaction method and apparatus of the present invention, the surface of the liquid to be treated supplied in the form of film is renewed by the inert gas jetted from the surface of the cylindrical rotor. While advancing the polycondensation reaction, the frequency of contact between the liquid to be treated and the inert gas is increased, and the evaporation of volatile substances generated in the reaction process in the liquid to be treated can be promoted, thus reducing the treatment time. It 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.

FIG. 2 is a detailed view of a cylindrical rotor 2b installed inside a container body in the continuous polycondensation reaction device of FIG.

[Explanation of symbols]

1 container body 2a Upper cylindrical rotor 2b Lower cylindrical rotor 3 Transport members 4 Liquid supply slitting device 5 heating device 6 Cooling device 7 Cylindrical roller 8 compressor 10 Piping for sending inert gas 11 condenser 12 Heating device 13 Scraping device 15 slits

Continuation of front page (56) References JP-A-63-104601 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) C08G 63/00-63/91 C08G 85/00

Claims (4)

(57) [Claims] 1. A plurality of cylindrical rotors are installed in an upper part and a lower part of an apparatus main body, and a conveying member made of a metal plate or the like stretched between the rotors is moved at a constant speed while one side surface of the conveying member. The liquid to be treated is supplied in the form of a film to the surface of the liquid to be treated by the inert gas sprayed from the rotor surface when the liquid passes over the cylindrical rotor installed at the lower part of the polycondensation reaction. A method for continuous polycondensation reaction, which is characterized in that 2. The inside of the apparatus main body is at normal pressure or several mmH ₂
After making the atmosphere of inert gas such as nitrogen in a slightly pressurized state of about O, the inert gas containing the volatile substances generated in the reaction process is sent to the condenser installed outside the main body of the device and the volatile substances contained are recovered. The continuous polycondensation reaction method according to claim 1, wherein the method is heated to a predetermined temperature and circulated in the apparatus main body. 3. A conveying member formed of a metal plate or the like stretched between a plurality of cylindrical rotors installed in an upper part and a lower part inside the apparatus main body and between cylindrical rotors installed outside the apparatus main body, on the surface of the conveying member. A supply slit device for supplying the liquid to be treated in a film shape, and a cylinder installed at the outside of the device body and having a scraping device for scraping the liquid to be treated on the conveying member, and a cylinder installed at the lower part in the device body. The cylindrical rotor injects a high-pressure inert gas from the surface of the cylindrical rotor so that the cylindrical rotor and the liquid to be treated on the conveying member are always kept in non-contact with each other, and part of the ejected gas A continuous polycondensation reactor having an injection nozzle for renewing the surface of a liquid to be treated. 4. A heater for preheating the carrying member is provided immediately before the entrance of the carrying member of the apparatus main body, and for cooling the liquid to be treated on the carrying member immediately after the exit of the carrying member of the apparatus main body. The continuous polycondensation reaction device according to claim 3, further comprising a cooler.