JPS63104601A - Method and device for continuously removing volatile matter - Google Patents

Abstract

PURPOSE:To improve the quality of soln. to be treated by forming a thin film of a viscous material between the transfer members to transfer the material, and reducing the velocity distribution of the thin film between the transfer members and retention time at the time of continuously removing volatile matter from the viscous material. CONSTITUTION:Freely rotatable rotors 3a and 3b are provided at the upper and lower parts in a main body 1 with the outer periphery covered with a heating jacket 2, and wires 3a and 3b are respectively hung in plural grooves provided on the rotors 3a and 3b as the transfer members for the soln. to be treated. A slit 7 at the lower end of a feed hopper 6 for the soln. to be treated provided at the upper end of the main body 1 is brought into contact with the wire 5 on the lower side of the upper rotor 3a, a scraper plate 8 is brought into contact with the surface of the lower rotor 3b, and a discharge screw 9 is provided at the lower part. The soln. to be treated such as the intermediate polymer of polyethylene terephthalate is formed into a film by the slit 7, kept between the surfaces of the wires 5, and moved downward along with the rotation of the rotors 3a and 3b.

Description

Detailed Description of the Invention [Industrial Field of Application] The present invention relates to a continuous volatile removal method ELCJ# from a highly viscous material suitable for continuous polycondensation such as polyethylene terephthalate.
It is related to the device.

[Conventional technology]

As described in Japanese Patent Application Laid-Open No. 60-44527, a conventional device holds an initial polymer in a thin film form between two wires hanging from a slit-shaped cap, and continues the process in the vertical direction. The system was designed to perform polycondensation by removing by-produced volatile substances.

However, since the thin film-like liquid to be treated moves by gravity, it moves quickly in the center of the film between the wires, and moves slowly at both ends, especially on the wire surface, resulting in a large moderate distribution. .

[Problem that the invention seeks to solve]

The above conventional technology does not take into account the fact that the moderate distribution of the thin film becomes large, and the problem is that the residence time distribution of the liquid to be treated becomes large, and the quality of the outlet liquid to be treated, that is, the quality of the polymer product, deteriorates. was there.

An object of the present invention is to improve the quality of the liquid to be treated by reducing the appropriate distribution within the thin film and narrowing the residence time distribution of the liquid to be treated.

(Means for solving the RMM point) The above purpose is to move the conveying member, which is belted between two cylindrical rotors provided in the main body of the apparatus, at a predetermined speed, and to apply the liquid to be treated on the surface of one end of the conveying member. This is achieved by supplying a thin film to form a thin film and moving it to the other end to evaporate and remove volatiles.

[For production]

By adjusting the rotation speed of the cylindrical rotor so that the movement of the conveying member is larger than the movement of the liquid to be treated between the wires due to gravity, the liquid to be treated is transferred together with the conveying member from the population side to the outlet side. Therefore, the distribution of the liquid to be treated in the liquid film, that is, the residence time distribution of the liquid to be treated can be made small.

〔Example〕

An embodiment of the present invention will be described below with reference to FIGS. 1 to 3. In the figure, reference numeral 1 denotes a main body of a continuous volatile matter removal apparatus formed in an elongated rectangular shape and installed vertically, and the outer periphery of which is covered with a heating jacket 2. 3m.

3b is the main body! A cylindrical rotor is rotatably installed in the upper and lower parts of the rotor, and the outer peripheral surface is provided with a plurality of grooves 4 as shown in FIG. One end is the driving equipment! (not shown). Between these two cylindrical rotors 3m and 3b, a plurality of metal wires (stainless steel wires, etc.) 5 are fitted into grooves 4 on the surfaces of the cylindrical rotors 3a and 3b as conveying members for the liquid to be treated. It is hung. metal wire 5
The outer diameter of used is Q, Q5+am-m2mm.

Reference numeral 6 denotes a hobper for supplying the liquid to be treated, which is provided at the upper end of the main body 1. The lower end thereof forms a slit 7, and is in contact with the metal wire 5 below the upper cylindrical rotor 3m. Reference numeral 8 denotes a scraping plate for the liquid to be treated, which is disposed at the lower end of the main body l, and its upper end is in contact with the surface of the lower cylindrical rotor 3b. Reference numeral 9 denotes a screw for extracting the liquid to be treated, which is provided at the lower part of the scraping plate 8, and is connected to a drive device FIl (not shown). Reference numeral 10 indicates an outlet nozzle for the liquid to be treated provided at the lower part of the extraction screen 9, 11 an outlet nozzle for volatile matter provided in the main body 1, and 13 an inlet nozzle and an outlet nozzle for the heating medium.

In the configuration described above, the lower cylindrical rotor 3b is the first
When the metal wire 5 rotates in the direction of the arrow in the figure, the upper cylindrical rotor 38 also rotates in the direction of the arrow via the metal wire 5, and the metal wire 5 moves downward on the right side of FIG. 1 and upward on the left side of FIG. In such an apparatus, a liquid to be treated, such as an intermediate polymer of bolier acupuncture tylene terephthalate, is introduced into the main body 1 from a supply hopper 6, and is supplied to the surface of the metal wire 5 in the form of a thin film through a slit 7 at the lower end. Here, the liquid to be treated is held in the form of a thin film between the respective metal wires 5, and the cylindrical rotor 3a.

As the metal wire 3b rotates, it moves downward together with the metal wire 5. Since the inside of the main body 1 is maintained at a high vacuum by the depressurization operation from the volatile matter outlet nozzle 11, volatile matter in the liquid to be treated, that is, ethylene glycol, etc. produced as a by-product in the polycondensation reaction, is removed by a thin film. It is efficiently separated by evaporation from the surface to be treated. In this way, the volatile matter removal operation of the liquid to be treated progresses, and at the same time, the polycondensation reaction is promoted, and a highly polymerized product reaches the lower cylindrical rotor 3b. The liquid to be treated that has reached the surface of the cylindrical rotor 3b is scraped off from the surface of the cylindrical rotor 3b by the scraping plate 8, and is transferred by the extraction screw 9 to the outlet nozzle 10.
The strands are taken out. At this time, the metal wire 5 is attached to the cylindrical rotor 3b! ! Since it fits into the groove 4 on the surface, the scraping operation of the liquid to be treated by the scraping plate 8 is performed smoothly, and the scraping efficiency is increased.

In the embodiment described above, since the thin film of the liquid to be treated moves together with the metal wire 5, the moderate distribution within the thin film becomes small, and the residence time distribution of the liquid to be treated can be made small.

When performing polycondensation of polyethylene terephthalate, etc. using the continuous volatile removal*a described above, the temperature inside the main body 1 is increased from 270°C to 320°C by passing a heating medium through the heating medium jacket 2.
℃, connect a pressure reducing device to the volatile matter outlet nozzle 11, and maintain the pressure inside the main body 1 at 0.degree. 1 to 5 Torr.
An intermediate polymer having a degree of polymerization of 10 to 60 is continuously supplied into the main body 1 from a supply hopper 6. The supplied intermediate polymer becomes a thin film from the slit 7 and is sent onto the metal wire 5.
It forms a thin film in between and moves downward. During this time, volatile substances such as by-produced ethylene glycol are evaporated and separated to promote the polycondensation reaction, resulting in a highly polymerized product with a degree of polymerization of 90 to 130, which is scraped off by the scraping plate 8 and removed by the extraction screw 9.
The yarn is then taken out from the outlet nozzle 1o. here,
The gap between the slits 7 is adjusted to a dimension of 0°11III11 to 2 mm.

As another recommended embodiment of the present invention, as shown in FIG. 4, the inside of the cylindrical rotor 3b on the outlet side of the liquid to be treated is made hollow, and rotary Raj winds 14 are installed at both ends of the cylindrical rotor 3b. A refrigerant is provided in the cylindrical rotor 3b to allow the refrigerant to flow through the rotor 3b.

According to this embodiment, the liquid to be treated that has reached the cylindrical rotor 3b on the outlet side is cooled and solidified or has a high viscosity, so that the liquid to be treated can be easily scraped off by the scraping plate 8. The solidified liquid to be treated is caught in the lower extraction screw 9, melted again, and taken out from the outlet nozzle 10.

Still other preferred embodiments of the present invention include FIG.
As shown in Fig. 96, the liquid to be treated is supplied from the lower part of the main body 1, and the thin film of the liquid to be treated formed between the metal wires 5 is moved upward and scraped off with the surface of the upper cylindrical rotor 3a. This is what I did. In the figure, "I" is a supply chamber for the liquid to be treated, which is provided close to the upper side of the cylindrical rotor 3b at the bottom of the main body 1.

A slit 16 is provided through which the metal wire 5 passes.

Reference numeral 17 denotes a scraping plate for the liquid to be treated, which is provided at the upper part of the main body 1, and whose tip is in contact with the surface of the upper cylindrical rotor 3m, and which is connected to the outlet nozzle 10' via the extraction screw 9'. ing. In this embodiment, the liquid to be treated is supplied into the supply chamber and is supplied to the surface of the metal wire 5 in a thin film through the slit 16 moving in the direction of the arrow in the figure, thereby forming a thin film between the metal wires 5 . As the metal wire 5 moves upward, *g also moves upward, and during this time, volatile substances such as ethylene glycol are evaporated and removed. Upper cylindrical rotor 3
The liquid to be treated that has reached the point a is scraped off by the scraping plate 17, passed through the extraction screw 9', and is taken out of the thread from the outlet nozzle 10'.

According to this embodiment, the liquid to be treated whose viscosity has increased due to the removal of volatile matter and the progress of polycondensation is likely to adhere to the metal wire 5.
It moves at the same rate as the metal wire 5.

On the other hand, the liquid to be treated with a low degree of polymerization and low viscosity from which volatile matters have not been removed moves upward while flowing downward little by little, and the residence time becomes longer by that amount. The viscosity increases and the distribution of the degree of polymerization at the outlet can be further reduced.

In yet another embodiment of the present invention, as shown in FIG. 7, the liquid to be treated is supplied from a supply chamber provided at the bottom of the main body 1,
The thin film of the liquid to be treated formed between the metal wires 5 is moved upward through the slit 16, passed through the outer periphery of the upper cylindrical rotor 3m, and further moved downward, and is scraped off from the surface of the lower cylindrical rotor 3b by the scraping plate 8. It was designed to be scraped off.

According to this embodiment, the liquid to be treated can be kept in a thin film state by using almost the entire circumference of the metal wire 5, and the residence time or amount of residence of the liquid to be treated in the thin film state can be increased. The efficiency of the device can be increased. In FIG. 7, the upper side of the supply chamber above the lower cylindrical rotor 3b has one end with the metal wire 5 as a conveying member, and the lower cylindrical rotor 3b
It is clear that the contact portion b with the scraping plate 8 is the other end.

In yet another embodiment of the present invention, as shown in FIG. 8, the cylindrical rotors 3m, 3b and the metal wire 5 are arranged diagonally, and the liquid to be treated is placed above the upper cylindrical rotor 3m. A thin liquid film 19 is supplied between the metal wires 5 from a supply hopper.

According to this embodiment, the liquid to be treated is a thin film liquid 1119.
For example, if an initial or intermediate polymer of polyethylene terephthalate is supplied, it becomes a thin film and the degree of polymerization and viscosity are increased during the fall, and the temperature between the metal wires 5 and 5 is increased. A stable liquid film with high viscosity can be formed.

In another embodiment of the present invention, as shown in Figs.
0 fits into the grid-like grooves 4' provided on the surface of the cylindrical rotors 3a and 3b and is hung with a belt. 2
The wire diameter of 0 is 0.05111111~2M.

The size of the mesh used is 3 mm to 301 m.

According to this embodiment, since a thin film of the liquid to be treated is formed on the mesh of the wire mesh, a stable thin film of the liquid to be treated can be formed on the surface of the wire mesh (9).

In yet another embodiment of the present invention, as shown in FIG. 11, a porous metal plate 4 is hung between cylindrical rotors 3a and 3b with a belt as a conveying member for the liquid to be treated, and the porous metal plate The diameter of the hole 4 is set to 3 mm to 30 mm, and a protrusion into which the hole n fits is provided on the outer peripheral surface of the cylindrical rotors 3m and 3b. The liquid to be treated is on the porous metal plate 4! ! supplied to the surface,
A thin film is formed within the interior of the porous metal plate 4, and is also attached to the surface of the porous metal plate 4, where volatile matter is evaporated and polycondensation reaction takes place.

According to this embodiment, by using the metal perforated plate 4 as a transporting member for the liquid to be treated, the strength of the transporting member can be sufficiently maintained, and also because the shape of the holes 4 is circular. It is possible to form the most stable thin film.

In still another embodiment of the present invention, an initial polymer such as polyethylene terephthalate is prepolymerized by a bulk polymerization method using a stirring tank to increase the degree of polymerization and viscosity, and then is fed into the main body of the apparatus. A stable saliva film can be formed at the supply section to the component.

In still another embodiment of the present invention, a volatile gas such as ethylene glycol is removed by heating an inert gas such as nitrogen into the main body, passing it over a thin film of the liquid to be treated, and then discharging it. Lower the partial pressure and remove by evaporation. I can do two things. In this embodiment, it is possible to operate under atmospheric pressure, so
Extraction screen.

is no longer necessary, and the device can be simplified.

In each of the yellow embodiments described above, the cylindrical rotors 3m and 3b are arranged at the upper and lower parts, and the conveyance member is stretched vertically or diagonally. This method can also be applied when the direction of movement of the conveying member and the direction of gravity are changed, and especially when the inlet viscosity of the liquid to be treated is greater than 100 voids, the appropriate distribution within the liquid film can be further reduced. It is ranked 9th in terms of being able to do so.

〔Effect of the invention〕

According to the present invention, it is possible to evaporate and remove volatile matter while moving the transport member on which a thin film of the liquid to be treated is formed, so that the appropriate distribution of the thin film within the transport member is reduced, and the thin film of the liquid to be treated is reduced. It is possible to reduce the residence time distribution, improve the quality of the liquid to be treated such as polyethylene terephthalate, and increase productivity.

[Brief explanation of the drawing]

FIG. 1 is a vertical sectional side view of a continuous volatile matter removal apparatus showing an embodiment of the present invention, FIG. 2 is a cross-sectional view taken along line 1-1 in FIG. 1, FIG. The figure is a sectional view showing another embodiment of the cylindrical rotor, FIGS. 5 and 7 are longitudinal sectional side views of a continuous volatile matter removal apparatus showing other embodiments of the present invention, and FIG. ■-■ sectional view, FIG. 8 is a schematic diagram of a conveyance member and a supply hopper for the liquid to be treated, showing still another embodiment of the present invention;
FIG. 9 is a longitudinal sectional front view of a continuous volatile matter removal apparatus showing still another embodiment of the present invention, FIG. It is a front view. l...Continuous volatile matter removal*! The body of i, 2...
... Heating racket, 3m, 3b... Four-day cylindrical rotor, 4゜4'... Groove, 5... Metal wire, 6,
18...-Supply hover bar 17, 16...-Slit, 8, 17... Scraping plate, 9.9'...
...Extraction screen, 1, 10.10', 11
, 13... Outlet nozzle, ν... Artificial nozzle,
14...Rotary ridge seal Ishido, Takumi...
・・Supply chamber, 19 ・------Liquid film, field... Figure 111

Claims (1)

[Scope of Claims] 1. The liquid to be treated is supplied to the surface of one end of the conveying member while moving the conveying member, which is belted between two cylindrical rotors provided in the apparatus main body, at a predetermined speed. A continuous volatile matter removal method characterized by forming a thin film and moving it to the other end to evaporate and remove volatile matter from the liquid to be treated. 2. The continuous volatile matter removal method according to claim 1, wherein volatile matter is removed by evaporation from the liquid to be treated by reducing the pressure inside the apparatus main body. 3. The continuous volatile matter removal method according to claim 1, wherein volatile matter is evaporated and removed from the liquid to be treated by circulating an inert gas within the apparatus main body. 4. Two cylindrical rotors are rotatably arranged in the longitudinal direction of the apparatus main body, a conveying member for the liquid to be treated is stretched between the two cylindrical rotors on a belt hook, and a surface of one end of the conveying member is coated. A supply hopper is installed to supply the processing liquid in a thin film.
A continuous volatile matter removal device, characterized in that the other end of the conveying member is provided with a plate that scrapes off the liquid to be treated in contact with the cylindrical rotor. 5. The continuous volatile matter removal device according to claim 4, wherein the conveying member is composed of a plurality of metal wires, and a plurality of grooves into which the metal wires fit are provided on the outer peripheral surface of the cylindrical rotor. 6. The continuous volatile matter removal device according to claim 4, wherein the conveying member is made of a band-shaped wire mesh, and a lattice-shaped groove into which the wire mesh fits is provided on the outer peripheral surface of the cylindrical rotor. 7. The continuous volatile matter removal device according to claim 4, wherein the conveying member is made of a metal perforated plate, and a protrusion into which a hole in the metal perforated plate fits is provided on the outer peripheral surface of the cylindrical rotor.