JP5558402B2 - Method for producing particulate polymer - Google Patents

Description

  The present invention relates to a method for producing a particulate polymer, and more particularly, to a method for producing a particulate polymer that can produce a particulate polymer having a uniform size.

  Resin polymers such as polycarbonate are subjected to a polymerization reaction or the like in the production apparatus, additives are added by an extruder, extruded into a strand shape by a die head, cooled, and then pelletized particles by a cutter or the like. Usually, it is molded into a polymer and becomes a product.

Here, if the size of the final product pellet is non-uniform, when the polymer is plasticized again and formed into a predetermined shape, the uniformity of the pellet length and diameter distribution is fluid. It greatly affects the plasticization time. That is, the more uniform the length and diameter distribution of the pellets, the more stable the pellet supply speed and the more uniform the plasticizing time.
Therefore, it is preferable that the distribution of the length and diameter of the pellet is as uniform as possible. As the accuracy, when the shape of the pellet is a cylindrical shape, the average length of the pellet is within ± 0.1 mm, and a perfect circle It is calculated | required that what is less than conversion average diameter +/- 0.1mm is 85% or more.

  As a method for solving this problem, it has been pointed out that, for example, the melt extrusion temperature is important (see, for example, Patent Document 1).

JP 2004-114486 A

  However, there has been a problem that the above-mentioned accuracy cannot be achieved because the distribution of the length and diameter of the pellets is not sufficiently uniform simply by controlling the melt extrusion temperature.

The present invention has been made in view of the above-described problems of conventional techniques.
That is, the objective of this invention is providing the manufacturing method of the particulate polymer which can manufacture particulate polymers, such as a pellet shape of a uniform magnitude | size.

Thus, the inventions according to the following (1) to (4) are provided.
(1) The invention according to claim 1 is a method for producing a particulate polymer by producing a particulate polymer using a granulating apparatus that cuts a strand obtained by passing a molten polymer through a die head having a plurality of holes. The granulator is installed around the die head and heated by the heater, a plurality of temperature measuring devices for measuring the temperature of the molten polymer at the outlet of the die head, and the temperature measuring device. A controller for controlling the heater according to the temperature of the molten polymer, and the controller determines a difference between the maximum value and the minimum value of the temperature of the molten polymer measured by the temperature measuring device. It is a manufacturing method of the particulate polymer characterized by controlling within 5 degreeC.
(2) The invention according to claim 2 is characterized in that the control is performed by dividing the die head into a plurality of sections and independently for each section. It is.
(3) The invention according to claim 3 is the method for producing a particulate polymer according to claim 1, wherein a take-up speed of the strand is 50 m / min to 250 m / min.
(4) The invention according to claim 4 is characterized in that the molten polymer is a polycarbonate obtained by melt polycondensation by a transesterification reaction between a dihydroxy compound and a carbonic acid diester. It is a manufacturing method of a polymer.

  According to the present invention, a particulate polymer having a uniform size can be produced from a strand of molten polymer.

It is a perspective view explaining the die head which comprises the granulation apparatus to which this Embodiment is applied. It is the rear view which looked at the die head from the direction shown by A in FIG. It is a figure explaining the structure of a die head plate. It is a figure explaining the granulation apparatus with which this Embodiment is applied.

  Hereinafter, modes for carrying out the present invention (hereinafter, embodiments of the present invention) will be described in detail. The present invention is not limited to the following embodiments, and various modifications can be made within the scope of the invention. The drawings used are for explaining the present embodiment and do not represent the actual size.

  Here, this embodiment will be described using polycarbonate as an example of the polymer.

  Polycarbonate is an engineering plastic that has excellent mechanical properties such as impact resistance, heat resistance, and transparency, and has been widely used in recent years for OA parts, automobile parts, building materials, and the like.

As a method for producing this polycarbonate, a so-called interfacial method using an aromatic diol such as a bisphenol compound and phosgene as a raw material, and a dihydroxy compound and a carbonic acid diester are transesterified in a molten state, and a low molecular weight such as phenol produced as a by-product. obtaining a polycarbonate while removing objects from the system, the so-called melting method is that is known.

Here, the case of producing a polycarbonate by the melt method, as Fang aromatic dihydroxy compound, 2,2-bis (4-hydroxyphenyl) propane (generally called "bisphenol A".) And the like, and as the carbonic acid diester Diphenyl carbonate, etc., and alkali metal compounds, such as cesium carbonate, are used as a transesterification catalyst. These are mixed, melted, and subjected to a polycondensation reaction in multiple stages using a plurality of reactors (polycondensation step). Manufacturing is performed.

After the polycondensation reaction, various additives are respectively supplied by a kneader such as an extruder, and then the strand-like polycarbonate discharged from the die head is cooled with cooling water and then cut and pelletized.
As conditions for polymer stranding, for example, the flow rate of the molten polymer discharged from the die hole is 100 to 1000 s-1 in terms of shear rate, and the resin temperature is in the range of 200 to 2000 Pa · s in melt viscosity. Usually, it is set in the range of 250 to 370 ° C. At this time, a granulating apparatus to which the present embodiment is applied is used.
Finally, after removing water with a dehydrator, it is introduced into a storage silo that is a storage container.

Next, the manufacturing method and granulation apparatus of the particulate polymer to which this embodiment is applied will be described in detail.
FIG. 1 is a perspective view for explaining a die head constituting a granulation apparatus to which the present embodiment is applied.
FIG. 2 is a rear view of the die head viewed from the direction indicated by A in FIG.
FIG. 1 shows a die head 11 to which a molten polymer is supplied, a die head plate 13 for extruding the molten polymer in a strand shape, and thermocouples 14a and 14b which are temperature measuring devices for measuring the temperature of the molten polymer discharged from the die head 11. , 14c, and plate heaters 15a, 15b, 15c, 16a, 16b, 17a, 17b, 17c, 18a, and 18b arranged around the die head 11 to heat the die head 11.
The heaters 15a, 15b, and 15c are installed side by side on the front surface of the die head 11 as shown in FIG. 1, and the heaters 16a and 16b are side surfaces of the protrusions 12 of the die head 11 as shown in FIG. Respectively. The heaters 17a, 17b, and 17c are installed side by side on the back surface of the die head 11 as shown in FIG. 2, and the heaters 18a and 18b are installed on both sides of the die head as shown in FIG.

The molten polymer is supplied from the direction indicated by A to the protrusion 12 of the die head 11 and is extruded from the die head plate 13.
FIG. 3 is a view for explaining the structure of the die head plate 13.
The die head plate 13 has 40 holes 19 for discharging the melted polymer, and is processed into a strand shape through the holes 19 and taken out.

Here, the three thermocouples 14 a, 14 b, and 14 c shown in FIG. 1 measure three different outlet temperatures of the molten polymer discharged from the die head plate 13. In this case, the temperature of the molten polymer discharged from the three points of the left part, the central part, and the right part of the die head 11 when viewed from the front surface of the die head 11 is measured.
The data of the temperature of the molten polymer measured by the three thermocouples 14a, 14b, and 14c is sent to a control unit (not shown), and the control unit is the maximum value of the temperature of the molten polymer measured by the thermocouples 14a, 14b, and 14c. The 10 heaters 15a, 15b, 15c, 16a, 16b, 17a, 17b, 17c, 18a, and 18b are independently controlled so that the difference between the minimum value and the minimum value falls within the range of 5 ° C.
That is, the die head is divided into a plurality of sections, and control is performed independently for each section. It is more preferable that the difference between the maximum value and the minimum value of the measured outlet temperature is within a range of 3 ° C. or less. In addition, since both ends of the die head 11 emit a large amount of heat, the die head 11 may be controlled at a temperature higher than other portions within the above temperature range.
Also, it is possible to manually control the temperature without providing a control unit.

The polymer extruded from the die head 11 in FIG. 1 is taken up while being cooled and cut by a cutter to become a particulate polymer.
FIG. 4 is a diagram illustrating a granulation apparatus to which the present embodiment is applied.
In FIG. 4, the strand extruded from the die head 11 is sent to the strand cooling device 20, where it is cooled by cooling water.
Then, although cut | disconnected by the cutter 30, the take-up speed | rate in that case has preferable 50m / min-250m / min.

  By using a granulating apparatus having the die head 11 having such a configuration, it is possible to produce a particulate polymer having a uniform size. That is, the variation in the outlet temperature of the molten polymer is reduced, so that the variation in the take-up speed of each strand taken from the hole 19 of the die head plate 13 is reduced. As a result, the shape of the particulate polymer becomes uniform.

In the above example, the melted polymer used is polycarbonate, but if the polymer has a step of producing a particulate polymer by obtaining a strand using the die head as described above and cutting it, There is no particular limitation. Examples thereof include polyethylene terephthalate and nylon.
In addition, the particulate polymer is a pellet and a cylindrical shape in the above example, but the shape is not particularly limited, and any shape can be used as long as it can be realized by cutting the strand polymer with a cutter. For example, a case where the cut surface is circular or elliptical, or a quadrangular shape is used.
The size of the particulate polymer is not particularly limited, but when the particulate polymer is a columnar pellet, it is preferably processed into a length of 10 mm or less.
Although there is no restriction | limiting in particular about the melt viscosity of the polymer extruded with an extruder, It is preferable that it is 200-2000 Pa * S.

  EXAMPLES Hereinafter, although this invention is demonstrated in detail using an Example, this invention is not limited by these Examples, unless the summary is exceeded.

Example 1
Polycarbonate is used as the polymer, and the polycarbonate after completion of polymerization (viscosity average molecular weight (Mv) = 26000) is increased by using a granulator having a die head as shown in FIG. Was dropped into a strand cooling chute (strand cooling device) that was cooled with water while being extruded in a strand form from a die head plate having a hole diameter of 7 mm and a hole number of 40 mm. The take-up speed at this time was 150 m / min.

In addition, the temperature of the molten polymer at the outlet portion at this time was measured by installing five thermocouples side by side on the die head at equal intervals.
The outlet temperature is controlled by setting a predetermined center temperature. If the temperature is lower than this range, the heating intensity of the heater around the thermocouple is increased, and if it is too high, the temperature around the thermocouple is increased. This was done by reducing the heating intensity of the heater.
As a result, the measured outlet temperatures were 350 ° C., 352 ° C., 353 ° C., 352 ° C., and 350 ° C. in order from the left end of the front surface of the die head, all falling within the range of 5 ° C.
When the polymer taken up in the form of a strand was cut into pellets with a cutter, the obtained pellets had an average length of 3.0 mm and a true circle equivalent average diameter of 2.9 mm. And the ratio of the pellet which the magnitude | size deviated from 0.1 mm from either average value was 10%.
The number of pellets used for measuring the size is 1,000.

(Comparative Example 1)
Polycarbonate is used as the polymer, and the polycarbonate after completion of polymerization (viscosity average molecular weight (Mv) = 26000) is increased by using a granulator having a die head as shown in FIG. Was dropped into a strand cooling chute (strand cooling device) that was cooled with water while being extruded in a strand form from a die head plate having a hole diameter of 7 mm and a hole number of 40 mm. The take-up speed at this time was 150 m / min.

In addition, the temperature of the molten polymer at the outlet portion at this time was measured by installing five thermocouples side by side on the die head at equal intervals.
The outlet temperature was not particularly controlled.
As a result, the measured outlet temperature was 345 ° C, 349 ° C, 352 ° C, 348 ° C, 344 ° C in order from the left end of the front surface of the die head, and was not within the range of 5 ° C, from the lowest temperature to the highest temperature. There was a difference of 8 ° C.
When the polymer taken up in the form of a strand was cut into pellets with a cutter, the resulting pellets had an average length of 3.1 mm and a true circle equivalent average diameter of 2.85 mm. And the ratio of the pellet which the magnitude | size deviated from 0.1 mm from either average value was 20%.
The number of pellets used for measuring the size is 1,000.

DESCRIPTION OF SYMBOLS 11 ... Die head, 12 ... Projection part of die head 11, 13 ... Die head plate, 14a, 14b, 14c ... Thermocouple, 15a, 15b, 15c, 16a, 16b, 17a, 17b, 17c, 18a, 18b ... Heater, 19 ... Hole, 20 ... Strand cooling device, 30 ... Cutter

Claims (2)

In a method for producing a particulate polymer, a particulate polymer is produced using a granulating apparatus that cuts a strand obtained by passing a molten polymer through a die head having a plurality of holes at a take-up speed of 50 m / min to 250 m / min. There,
The molten polymer is a polycarbonate obtained by melt polycondensation by a transesterification reaction between a dihydroxy compound and a carbonic acid diester,
The stranding condition is such that the flow rate of the molten polymer discharged from the die hole part is a shear rate of 100 s ^{−1 to} 1000 s ⁻¹ and a resin temperature of 250 to 370 ° C., and
The granulator is
A heater installed around the die head for heating the die head;
A plurality of temperature measuring devices for measuring the temperature of the molten polymer at the outlet of the die head;
A controller that controls the heater according to the temperature of the molten polymer measured by the temperature measuring device,
The control unit divides the die head into a plurality of sections, and independently of each section, a difference between a maximum value and a minimum value of the temperature of the molten polymer measured by the temperature measuring device is within 5 ° C. A method for producing a particulate polymer, characterized by controlling. 2. The method for producing a particulate polymer according to claim 1 , wherein the polymer extruded from the extruder has a melt viscosity of 200 Pa · s to 2000 Pa · s.

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