KR100610289B1 - Method and apparatus for polymer processing treatment - Google Patents

Abstract

Reacting the polymer compound with a medicament in a reaction vessel to produce a polymer treatment, depressurizing and introducing a polymer treatment including the medicament from the reaction vessel into a degassing extruder, and upstream of the degassing extruder Connecting a vent box having a volume of one or more times the volume of the reaction vessel to the side, introducing a chemical agent or the like contained in the polymer treated material supplied to the degassing extruder into the vent box, and separating the polymer; A method of treating a polymer compound, comprising the step of extruding a treated product from the extruder.

Degassing Extruders, Vent Boxes, Hoppers, Polymer Processes, Heaters

Description

METHOD AND APPARATUS FOR POLYMER PROCESSING TREATMENT}

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 shows a first embodiment of a treatment apparatus for a polymer compound according to the present invention.

Fig. 2 shows a second embodiment of the treatment apparatus for polymer compound according to the present invention.

3 is a view showing a vent box and a pressure adjusting mechanism according to the present invention.

4 is a view showing a polymer processing apparatus of a first comparative example.

Fig. 5 shows a third embodiment of the treatment apparatus for polymer compound according to the present invention.

Fig. 6 shows a fourth embodiment of the treatment apparatus for the polymer compound according to the present invention.

7 is a view showing a polymer processing apparatus of a third comparative example.

<Explanation of symbols for the main parts of the drawings>

1: extruder for material supply

1a, 2a: screw

2: extruder for degassing

4: chiller

5: strand

6: strand cutter

8: vent box

9: vent

10: heating heater

11: pressure reducing valve

11a, 23: valve

12, 212: pressure regulator valve

13: hopper

14: pharmaceutical heating heater

15: pharmaceutical infusion pump

16: impurity separation tank, trap

17: pharmaceutical tank valve

18: pharmaceutical tank

19: blower, vacuum pump

20: combustion device

21: pharmaceutical shatterproof box

22: fan

24: gas sensor

25 instrument

31: Breaker Plate

70: pressure transmitter

71: pressure control device

72: signal transmission line

100: flow-type reaction vessel

208: Pharmaceutical Separation Tank

209: polymer processed material

210: chemical separation tank heating heater

[Document 1] Japanese Unexamined Patent Publication No. 2001-253967

[Document 2] Japanese Unexamined Patent Publication No. 2002-249618

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method and apparatus for treating a polymer compound in which the polymer compound is a thermoplastic resin or a wax by a modification reaction, a decomposition reaction, and a crosslinking and cutting reaction. In particular, a polymer workpiece and a drug in a supercritical state are reacted using an extruder. The present invention relates to a processing method and a processing apparatus for a polymer compound.

In recent years, environmental problems are becoming more important, and waste disposal costs are increasing year by year. The energy of recycling is increasing also about a high molecular compound. In this movement, since the thermoplastic resin can be molded again by increasing the fluidity when heated, material recycling is in progress. On the other hand, thermosetting resins, crosslinked polymers, rubbers, etc. do not fluidize due to the three-dimensional network of molecules even when heated, so that molding cannot be performed. For this reason, most of the cases are provided for disposal such as landfill, except that some thermal recycling is performed.

In such thermosetting resins and crosslinked polymers, the movement to perform material recycling increases, and the technology which enables this is also shown. For example, a method of disintegrating a three-dimensional network structure in a molecule and making it thermoplastic is used, or waxing by cutting and polymerizing a polymer main chain, and recycling it as an additive to a resin is considered. have.

In order to make this method practical, a process of continuously treating the polymer is essential, and the use of an extruder is suitable for this. Heat and pressure are required to disintegrate and thermally plasticize three-dimensional networks among stable thermosetting resins and crosslinked polymer molecules. By using an extruder, the conditions required for this can be obtained easily. The same applies to waxing. In the case of thermal plasticization, a thermoplastic resin or a drug is often added together with a thermosetting resin or a crosslinked polymer, but such an additive can also be easily introduced by using an extruder.

For example, Patent Document 1 (Japanese Patent Laid-Open No. 2001-253967) supplies cross-linked polyethylene and water to an extruder, and the water becomes supercritical or subcritical in an extruder, that is, a temperature of 200 ° C to 1000 Disclosed is a method in which a thermoplastic material is extruded at a pressure of 2 to 100 MPa at 0 ° C.

Patent document 2 (Japanese Patent Laid-Open No. 2002-249618) discloses a crosslinked polymer extruded from an extruder and introduced into a reactor together with a high temperature and high pressure fluid to generate a reactant, and the reactant is introduced into a separator to separate the reactant and the hot fluid. And a method of discharging the reactant to the outside from the extruder.

(1) Patent Document 1 does not disclose an effective means for separating the reactant and the thermosetting resin after mixing them.

(2) In patent document 2, in order to isolate | separate after mixing a reaction agent and a thermosetting resin, the separation tank for separating the mixture of a polymer and a gas is provided. However, this method is expensive because it is necessary to arrange the extruder in three dimensions. In addition, when the polymer coming out of the separation tank is attached to the separation tank, it is difficult to supply it to the extruder for degassing smoothly.

(3) In these conventional examples, high pressures are maintained in the extruder, but effective measures have been disclosed for countermeasures when such high pressure water, gas, and chemicals flow back to the hopper side of the extruder. There is a problem to deal with.

Accordingly, it is an object of the present invention to prevent the sudden pressure fluctuations due to vaporization and expansion of the drug when discharging the polymer from the reaction vessel from affecting the molding of the polymer treated product by the degassing extruder, so that the polymer treated product It is to provide a processing method and apparatus for treating a high molecular compound that enable continuous and homogeneous molding.

In addition, another object of the present invention is a polymer treatment that prevents gas from spreading around even when the gas flows back into the hopper upstream of the material supply extruder, thereby enabling continuous and homogeneous molding of the polymer treated product. It is to provide a method and apparatus for producing water.

(1) According to the first aspect of the present invention,

Reacting the polymer compound with a medicament in a reaction vessel to produce a polymer treated product,

Introducing a polymer treated product including the drug from the reaction vessel into a degassing extruder;

A vent box having a volume of one or more times the volume of the reaction vessel is connected to an upstream side of the degassing extruder, and a drug or the like contained in the polymer treated product supplied to the degassing extruder is introduced into the vent box and separated. Fair,

Thereafter, there is provided a method for treating a polymer compound, which comprises a step of extruding a polymer product from the extruder for degassing.

The processing method of the said high molecular compound may add the following characteristics.

(i) The degassing extruder is a twin screw extruder.

(ii) A vent mechanism is provided on the discharge side of the degassing extruder, and the chemicals remaining in the polymer to be extruded are further removed through the vent mechanism.

(iii) The reaction vessel is composed of a flow type reaction vessel connected to an extruder for supplying a polymer material and an extruder for supplying a polymer material.

(iv) The polymer treatment product and the medicine are introduced into the degassing extruder from the reaction vessel in a reduced pressure state by the decompression means, and the polymer treatment material from which the medicine is separated from the vent box is molded by the exhalation extruder.

and (v) an impurity separation step of separating the drug from the drug after separating the drug from the vent box, and a drug storage step of storing the drug from the impurity and introducing the drug into the extruder for supplying the polymer material. .

(vi) A cooling step of cooling the polymer processed material extruded from the extruder for degassing, and a cutting step of cutting the cooled polymer processed material.

(vii) The reaction between the polymer compound and the drug in the reaction vessel is a modification reaction, decomposition reaction or crosslinking reaction of the polymer compound.

(viii) the polymer compound is a crosslinked polymer, and the drug is an alcohol or a mixture containing alcohols,

(ix) The polymer compound is pulverized in advance.

(2) According to the second aspect of the present invention,

In the processing apparatus of a high molecular compound which produces a polymer processing material by reacting a high molecular compound and a drug in a reaction vessel,

Decompression means for decompressing and discharging the polymer treated product including the medicament from the reaction vessel;

A degassing extruder for introducing a polymer processing material containing a drug from the decompression means and extruding the polymer processing material;

A back vent formed at an upstream side of the extruder for degassing;

Provided is a processing apparatus for a polymer compound which is connected to the back vent and has a volume of one or more times the volume of the reaction vessel, and comprises a vent box for separating a drug or the like contained in the polymer treated product supplied to the degassing extruder. do.

The processing apparatus of the said high molecular compound may add the following characteristics.

(i) an impurity separation tank for separating impurities from the separated medicine is connected to the vent box, and heating means for heating the vent box to a high temperature is provided on an outer circumference of the vent box, and between the vent box and the impurity separation tank. Adjusting pressure adjusting means for maintaining a constant pressure in the impurity separation tank is provided.

(ii) The said heating means is an electrothermal heater installed in the outer peripheral part of the polymer-processing material storage part of the said vent box.

(iii) The said heating means is comprised by the jacket provided in the outer peripheral part of the polymer processing material storage part of a vent box, and a heating medium body circulation apparatus which supplies a heating medium body to the said jacket.

(iv) the impurity separation tank is connected with a storage tank for storing the drug which has separated the impurity, and the drug of the storage tank is introduced into the extruder for supplying the polymer material for heating and stepping up to supply the polymer compound, and the polymer From the extruder for material supply, it is supplied with a high molecular compound to a reaction vessel.

(v) The degassing extruder includes a cooler for cooling the molded polymer processed material and a cutter for cutting the cooled polymer processed product.

(vi) The pressure reducing means is a discharge valve.

(vii) The pressure reducing means is a resistor having a plurality of holes.

(viii) The pressure reducing means is a resistor having a plurality of holes, a flow regulating valve, or a combination thereof.

(Features of the first and second aspects)

In the processing apparatus in which the decompression extruder is connected to the reaction vessel and the degassing extruder is connected to the reaction vessel as described above, the degassing extruder has a back vent, and the vent having a volume of one or more times the reaction vessel in the back vent. By connecting the boxes, the polymer and the drug can be stably separated, and the gas can be degassed from the resin stably. Thus, the polymer treatment can be formed continuously and homogeneously.

In addition, even when the resin containing a large amount of chemicals is discharged from the outlet of the material supply extruder, the vent box is sufficiently large, so that problems such as clogging the intake vent of the vent box can be avoided and pressure can be sufficiently lowered.

In this way, the vent box serves as a buffer against pressure fluctuations, the pressure fluctuations at the rear end thereof are reduced, and continuous and homogeneous molding is achieved.

In order to prevent the drug from overflowing due to excessive pressure rise of the drug, the volume of the vent box is increased to about Pv times or more with respect to the pressure [Pv (MPa)] of the reaction container so that all the gases in the reaction container are vent boxes. It is more preferable to design so that a pressure may be 1 Mpa or less, even when it flows in.

The polymer used in the present invention includes not only a synthetic polymer of a crosslinked polymer, a thermosetting resin such as plastic or rubber, but also a natural polymer such as lignin, cellulose and protein, or a synthetic polymer and a natural polymer mixture. It also includes a polymer such as shredder dust and a mixture of other materials.

In particular, when a crosslinked polymer is used as the polymer and a mixture containing alcohols or alcohols as the drug, the treatment apparatus of the present invention functions effectively. In addition, the treatment apparatus of the present invention can effectively suppress the pressure fluctuation while sufficiently securing the reaction time when high pressure conditions such as supercritical conditions are used to facilitate the reaction by the drug.

(3) According to the third aspect of the present invention,

Injecting the polymer compound into the extruder for feeding the material through the hopper;

Injecting a medicament into the material supply extruder while extruding a polymer compound;

A polymer compound and a drug are kneaded in the extruder for supplying the material, and a mixture of the polymer compound and the drug is introduced into a reaction vessel at a high temperature and high pressure to react to produce a polymer processed product.

There is provided a method for treating a polymer compound in which the hopper is provided with a drug diffusion prevention box, and a drug gas generated in the extruder for supplying material is locally exhausted through the drug diffusion prevention box.

(4) According to the fourth aspect of the present invention,

An extruder for material supply for kneading a polymer compound and a drug and reacting with each other to produce a polymer processed product,

A hopper for introducing a polymer compound into the extruder for supplying the material;

Consists of a drug diffusion prevention box installed in the vicinity of the hopper,

The said chemical | diffusion diffusion prevention box is a processing apparatus of the high molecular compound provided with the local exhaust apparatus which locally exhausts the chemical | medical agent gas which generate | occur | produces in the said material supply extruder via the said hopper.

The processing method and the processing apparatus of the said high molecular compound may add the following characteristics.

(i) The drug diffusion prevention box is connected to a trap via an on / off valve, and the trap is connected to a vacuum pump.

(ii) the drug diffusion prevention box includes a gas sensor, and the gas sensor includes the opening / closing valve provided between the medicine diffusion prevention box and the trap when the medicine gas flows back into the medicine diffusion prevention box. Open.

(iii) The extruder for material supply has a reaction vessel connected in the extrusion direction, and a valve provided between the extruder for material supply and the reaction vessel.

(iv) Furthermore, it has the degassing extruder connected to the rear end of the said material supply extruder, and the vent box connected to the upstream side of the said degassing extruder.

(v) The drug diffusion prevention box is connected to the trap via an on / off valve, the trap is connected to a vacuum pump, and the vent box is connected to the trap via a pressure regulating valve.

(Features of the third and fourth aspects)

As described above, by attaching a box for preventing the diffusion of the medicine to the hopper of the material supply extruder, even if the chemical gas flows back into the hopper located upstream of the material supply extruder, it is stably without spreading the gas around. Polymer treatments can be obtained.

The drug diffusion prevention box needs to be provided with the exhaust means (for example, a local exhaust apparatus) which exhausts the gas of the backflow chemical | medical agent. When this exhaust means is not provided, there is a possibility that a gas may stay in the drug diffusion prevention box or overflow from the drug diffusion prevention box, and in particular, when the drug is a flammable gas, there is a possibility of ignition.

The drug diffusion prevention box is preferably connected to a trap of the vacuum pump via a valve. When the gas flows back, the valve can be opened and the gas can be recovered and reused.

The drug diffusion prevention box is preferably wrapped around the shooter, which is generally attached to the hopper of the extruder for material supply. If the gas flows back, it is intended to prevent the gas that is expected to overflow from the shooter to diffuse around.

The size (volume) Vt of the trap of the vacuum pump to which the drug diffusion prevention box is connected is preferably equal to or larger than the size (volume) V of the high pressure vessel (extruder for material supply + reaction vessel). More preferably, when the volume (Vt) = P x V calculated from the pressure P (atm), the gas backflowed more reliably can be collected.

It is preferable that a fan is not attached to the inlet of the local exhaust fan to which the chemical | diffusion diffusion prevention box is connected, and a powder etc. of the polymeric material which may be ejected with a gas ejection.

When the vent mechanism of the drug diffusion prevention box and the degassing extruder are connected to the same trap, the trap and the vacuum pump can be used for two purposes, namely, recovery of countercurrent gas and separation of drug gas.

EMBODIMENT OF THE INVENTION Hereinafter, embodiment of this invention is described, referring an accompanying drawing.

[First Embodiment]

BRIEF DESCRIPTION OF THE DRAWINGS The 1st Embodiment of the processing apparatus (the crosslinking | crosslinking cutting processing apparatus of crosslinked polyethylene) of a high molecular compound concerning this invention is shown.

In Fig. 1, the crosslinked polyethylene pulverized into pellets is introduced into the extruder 1 (cylinder diameter 33 mm, L / D = 50) for supplying the polymer material via the hopper 13. On the other hand, ethanol as a chemical required for the reaction is pressurized by the chemical injection pump 15 from the chemical tank 18 via the chemical tank valve 17, and heated by the chemical heating heater 14 to supply materials. It is injected into the extruder 1. It is preferable that the injection position is downstream from the position where the crosslinked polyethylene is sufficiently densified in the extruder 1 for supplying material, thereby preventing leakage to the upstream side due to vaporization of the drug.

The extruder 1 for material supply used the twin screw extruder which has two screws 1a so that the chemical | medical agent of high temperature and high pressure may not flow back and sufficient kneading may be performed. In the chemical | medical agent infusion pump 15, it is necessary to pressurize more than the pressure of the inside of the extruder 1 for material supply. Moreover, it is preferable to heat up so that the temperature of the polymer heated up in the extruder 1 for material supply by the chemical | medical agent heater 14 may not fall. In the extruder 1 for material supply, the injected crosslinked polyethylene and the injected chemical | medical agent are mixed and stirred by the screw 1a. At this time, if at least part of the extruder 1 for supplying material is subjected to the temperature and pressure conditions at which the ethanol as a drug is in a supercritical state, the crosslinking and cleavage reaction between the crosslinked polyethylene and ethanol proceeds sufficiently to obtain a good polymer treated product. You can get it. Here, in order to ensure reaction time sufficiently, the flow-type reaction vessel 100 of 50L in volume was connected to the extruder 1.

The mixture of crosslinked polyethylene, which is a plasticized polymer treated product, in the material supply extruder 1 and the flow-type reaction vessel 100, and ethanol, which is a drug, is depressurized by a pressure reducing valve 11 (or a discharge valve) as a pressure reducing means. In order to lower the pressure in steps, a breaker plate 31 serving as a resistor in which a plurality of holes are opened is attached to decompress the resin in steps.

In addition, a degassing extruder 2 is connected to the rear end, wherein the viscous liquid polymer processed material is extruded in the discharge direction of the extruder 2 by a screw 2a, and the gas is a bag having a low pressure. By flowing into the vent box 8 of the vent, the polymer treatment product and the drug are separated.

The vent box 8 is heated by the vent box heating heater 10 as the heat transfer heater, and maintained at a temperature at which the polymer treated material exhibits fluidity.

In addition, instead of using the heating heater 10, a jacket (not shown) through which the heating medium body provided in the outer periphery of the polymer processed material storage part of the vent box 8 circulates, and a heating medium body for supplying the heating medium body to the jacket The vent box 8 may be heated using a circulation device.

The vent box 8 was made into 2 times and 100L of the volume of the reaction container 100. Thus, when the vent box 8 is made larger than the volume of the reaction container 100, even when discharge of resin and gas becomes intermittent, the pressure inside the vent box 8 is made 1/2 of the pressure of the reaction container 100. It can be lowered below. The inside of the vent box 8 is kept slightly above normal pressure and at a pressure lower than the reaction vessel 100, whereby the polymer product is easily discharged out of the vent box 8. In the vent box 8, the light gas is separated from the upper side of the tank, and the polymer processed material in a molten state is stored below the tank, and is sent to the degassing extruder 2 by self-weight from the hole provided in the lower part of the tank, Molded by 3).

The degassing extruder 2 can use any type of single screw or twin screw extruders. In the degassing extruder 2, the polymer treated product is molded as a threaded strand 5, and is cooled and solidified to almost room temperature by the cooler 4. The strands 5 become pellets 7 by the strand cutter 6. The degassing extruder 2 may be provided with a vent 9 as shown in FIG. 2 in order to completely remove the drug from the resin.

On the other hand, ethanol separated from the vent box 8 into the polymer treatment product is brought to atmospheric pressure through the pressure adjusting valve 12 as the pressure adjusting means and is sent to the impurity separation tank 16. In the impurity separation tank 16, impurities generated during the reaction and mixed in the ethanol are separated according to the difference in boiling point. Ethanol is returned to the chemical tank 18, and impurities are sucked in the blower 19, and incinerated by the combustion device 20 to be harmless.

The treatment apparatus is particularly effective in the case where the viscosity of the polymer treated product is high and does not flow unless a force is applied. When the flow-type reaction vessel 100 is not used as in Patent Documents 1 and 2, there is a limit to lengthening the cylinder of the extruder 1, so that the throughput per unit time is limited as long as a constant size extruder 1 is used. There is. On the other hand, when the flow type reaction vessel 100 is used, the throughput per unit time can be increased while arbitrarily securing the required reaction time by changing the size (length). Such an apparatus is effective for chemical reactions requiring a time of 30 minutes or more, for example, a silane crosslinking and cleavage reaction with an alcohol of silane crosslinked polyethylene.

When the thus-obtained polymer treatment product (molten polymer treatment product and gaseous agent) is discharged intermittently instead of continuously through the pressure reducing valve 11, the polymer treatment product is a liquid because the gas expands from the compressed state. Swept out and squirts vigorously. In this case, since the vent box 8 is sufficiently large in volume, a buffering function functions as a function of the pressure change, thereby suppressing the pressure fluctuation in the discharge direction of the resin. In this way, smooth molding can be achieved.

In addition, since the polymer treated product is directly injected into the extruder 2 for degassing through the piping from the reaction vessel 100, it is attached to the chemical separation tank as in Patent Document 2, so that the polymer treated product cannot be extruded, or the viscosity of the polymer processed product. Since it is high, there is no problem that resin is not supplied to the extruder 2 for degassing. For this reason, the fluctuation | variation of the supply amount of resin is small, and supply of a constant polymeric material is attained.

In the case where the vent box 8 is not provided, the pressure fluctuations due to expansion of the gas are large, and since this directly affects the molding side, the amount of material supplied to the degassing extruder 2 varies or the gas and the polymer of the chemical from the vent are changed. The processed product may be ejected.

As in the present embodiment, by providing the large vent box 8 in the degassing extruder 2, even after the plasticization reaction performed at a high pressure, there is little variation in the material supply to the degassing extruder 2 and kneading in the extruder. While the gas can be completely degassed from the resin. In addition, since the degassing tank is installed and the method of dropping the polymer processed material into its own weight is not used, the device can be arranged in a plan and the device can be configured at low cost.

Fig. 3 shows the pressure adjusting mechanism of the vent box 8 provided at the rear end of the extruder 1 for material supply, according to the present invention.

After the mixture of the polymer processing material discharged from the material supply extruder 1 of FIG. 1 and the drug is decompressed to 1 to several tens of atmospheric pressure from the pressure in the material supply extruder by the pressure reducing valve 11, the extruder for degassing It is introduced into (2), and is separated into a polymer processed material which is a viscous liquid and a chemical which is a gas. At the pressure reduction in the pressure reducing valve 11, the chemical component of the gas compressed at high pressure expands and is blown into the vent box 8 with this. At this time, since the volume of the vent box 8 is larger than the volume of the ejected gas, it is possible to suppress some pressure fluctuations, but by providing the following pressure adjusting mechanism, the stabilization of the pressure can be further achieved. Can be.

That is, the pressure in the vent box 8 is measured by the pressure gauge and the pressure transmitter 70 and transmitted to the pressure control device 71 via the signal transmission line 72. The pressure control device 71 transmits a valve opening / closing signal to the pressure adjusting valve 12 via the signal transmission line 72 according to the pressure signal sent. The pressure control valve 12 is an air operated valve, and adjusts the opening degree of the valve 12 according to a signal. At that time, the opening degree of the valve 12 is adjusted so that the internal pressure of the vent box 8 becomes constant.

As another pressure adjustment method, the pressure may be adjusted in accordance with the linkage of the pressure reducing valve 11 and the pressure adjusting valve 12. In this case, in addition to the pressure gauge and pressure transmitter 70 described above, a means for measuring the differential pressure before and after the pressure reducing valve 11 is provided, and both the former and the latter control is performed. In the case of controlling both of the pressure reducing valve 11 and the pressure adjusting valve 12, if both are controlled only by the signal of the pressure, the action of the valve is interrupted and the pressure retention becomes unstable. Therefore, as described above, the pressure reducing valve 11 The pressure difference of the vent box 8 is preferably used as a signal for the control of the pressure adjusting valve 12 before and after the differential pressure before and after the control.

By these mechanisms, the pressure in the vent box 8 is always kept substantially constant, which enables continuous and homogeneous extrusion for molding in the shaping means of the degassing extruder 2.

When using such a device, the throughput of the crosslinked polyethylene can be continuously processed for 5 hours or more in the range of 2 to 100 kg / h per unit time in which the ejection capacity of the extruder is allowed.

Second Embodiment

2 shows a second embodiment of a treatment apparatus for a polymer compound according to the present invention.

In this embodiment, the vent 9 is attached to the degassing extruder 2 demonstrated in FIG.

In the present embodiment, since the chemical liquid remaining in the polymer treated product is discharged from the vent 9 via the valve 91 to the combustion apparatus 20 side, the chemical liquid is more completely removed. When such an apparatus is used, the throughput of the crosslinked polyethylene can be continuously processed for 5 hours or more in the range of 2 to 100 kg / h per unit time allowed by the ejection capacity of the extruder as in the first embodiment.

[First Comparative Example]

4 shows a polymer processing apparatus of the first comparative example.

In the first comparative example, the pellet-like thermosetting resin or the crosslinked polymer is introduced into the extruder 1 for supplying material from the hopper 13 as shown in FIG. The extruder 1 for material supply is the same as that of FIG. On the other hand, ethanol is injected into the extruder 1 for material supply via the chemical | medical agent tank 18, the chemical | medical agent tank valve 17, the chemical | medical agent injection pump 15, and the chemical | medical agent heating heater 14 as a reaction chemical of crosslinking decomposition.

In the extruder 1 for material supply, the thermosetting resin or crosslinked polymer maintained at high temperature and high pressure in a supercritical state is plasticized by reacting with ethanol in a supercritical state. In this way, the mixture of the plasticized polymer treated product and the medicament is gradually reacted by the breaker plate 31 which is a resistance body in which the pressure reducing valve 11 and the plurality of holes are opened after fully reacting in the flow-type reaction vessel 100. Decompression Thereafter, the mixture is introduced into the drug separation tank 208 at a pressure slightly higher than normal pressure and lower than the pressure of the flow reaction vessel 100, unlike the embodiment of FIG.

In the chemical | medical agent separation tank 208, it isolate | separates into the polymeric processing material 209 of the viscous liquid and the chemical | medical agent of a gas. The chemical | medical agent separation tank 208 is heated by the chemical | medical agent separation tank heating heater 210 by an electrothermal heater, and the polymer processed material 209 is maintained at the temperature which has fluidity. In addition, the inside of the drug separation tank 208 is maintained higher than the normal pressure, whereby the polymer treated material 209 is easily discharged out of the drug separation tank 208. The polymer treated product discharged out of the chemical separation tank 208 is introduced into the extruder 2, and moves inside the extruder 2 and is molded by the die 3 at the tip end. The extruder 2 may be a single screw or twin screw extruder. The die 3 is shaped as a threaded strand 5 and is cooled and solidified to about room temperature by the cooler 4. The strand 5 is cut by the strand cutter 6 to be a pellet 7.

The extruder 2 may provide a vent port to completely remove the drug from the resin.

On the other hand, the ethanol which is a drug separated from the drug separation tank 208 into the polymer processing material 209 becomes atmospheric pressure through the pressure control valve 212 and is sent to the impurity separation tank 16. In the impurity separation tank 16, the impurities produced during the reaction are separated from the ethanol which is the drug by the difference in boiling point. Ethanol is returned to the chemical tank 18, and impurities are sucked in the blower 19 and incinerated by the combustion device 20.

When the apparatus of the first comparative example was used, the ejection of the resin was intermittently, and the ejected resin adhered to the wall surface of the chemical separation tank 209 and was not supplied to the extruder 2. Therefore, stable continuous operation could not be continued for a long time.

Second Comparative Example

In the second comparative example, the volume of the vent box 8 of the back vent was 1/2 of the reaction vessel 100 in the processing apparatus shown in FIG.

As a result, when the discharge of the resin becomes intermittent, the pressure in the vent box 8 is higher than 1/2 of the pressure in the reaction container 100 by the ejected resin and alcohol, so that there is a risk that the vent box 8 is destroyed. Occurred. In addition, if the operation was continued in that state, the resin ejected from the vent box 8 would block the vacuum piping and the gas could not be degassed, and the operation had to be stopped.

[Third Embodiment]

5 shows a third embodiment of a treatment apparatus for a polymer compound according to the present invention.

The crosslinked polyethylene pulverized into pellets is introduced into the extruder 1 for material supply via the hopper 13.

The hopper 13 has a medicine diffusion prevention box 21 attached thereto, and a local exhaust fan 22 is attached thereto. When a small amount of gas flows back normally, the gas is exhausted by the fan 22. In addition, when the trap 16 and the vacuum pump 19 are connected via the valve 23 and a large amount of gas flows back at once, the valve 23 is opened to trap the gas together with the polymer. To be captured. The valve 23 is provided with the mechanism 25 which opens automatically when alcohol is detected by the gas sensor 24 attached to the hopper 13.

The extruder 1 for material supply uses cylinder diameter 30mm and L / D = 66. On the other hand, the ethanol required for the reaction is pressurized from the chemical tank 18 to the chemical injection pump 15 through the chemical tank valve 17 and heated by the chemical heating heater 14 to extruder 1 for material supply. ) At a pressure of 5 MPa. The injection position is downstream from the position where the crosslinked polyethylene is pressurized to 1 MPa or more in the extruder 1 for material supply and densified, and the length of the press portion is L / D = 5 or more, thereby upstream by vaporization of the drug. Leakage to the side is prevented. The extruder 1 for material supply used the twin screw extruder in order to send the crosslinked polyethylene which is hard to discharge.

The medicine to be supplied needs to be pressurized by the medicine injection pump 15 to a pressure higher than the inside of the extruder 1 for material supply. Moreover, it is preferable to heat the chemical | medical agent supplied by the chemical | medical agent heating heater 14 so that the temperature of the high molecular compound heated up in the extruder 1 for material supply may not fall.

In the extruder 1 for material supply, the injected crosslinked polyethylene and the injected chemical | medical agent are mixed and stirred by a screw. At this time, if at least a part of the extruder 1 for supplying material is subjected to the temperature and pressure conditions at which the ethanol as a drug becomes a supercritical state, the cross-linking reaction of the crosslinked polyethylene proceeds sufficiently to obtain a good polymer treated product. . In this embodiment, in order to ensure reaction time fully, the flow-type reaction container 100 of volume 50L was connected to the rear end of the extruder 1.

In the extruder 1 for material supply and the flow-through reaction vessel 100, a mixture of polymerized plasticized crosslinked polyethylene and ethanol, which is a drug, is a breaker plate as a pressure reducing valve 11 and a resistor having a plurality of openings. The pressure is reduced in stages by (31). In addition, a degassing extruder 2 is connected to the rear end, wherein the polymer processing material of the viscous liquid is extruded in the discharge direction of the extruder 2 by a screw, and the gas is a vent box of a back vent having a low pressure ( 8) to separate the polymer processing agent and the drug.

The vent box 8 is heated by a heating heater 10 such as an electrothermal heater, and is maintained at a temperature at which the polymer processed material has fluidity. The inside of the vent box 8 is maintained at slightly higher than normal pressure and at a pressure lower than the reaction vessel 100, whereby the polymer product is easily discharged out of the vent box 8.

In the vent box 8, the light gas is separated from the upper side of the tank, and the polymer treated material is stored below the tank even when it flows backward, and is sent to the degassing extruder 2 by weight from the hole provided in the lower part of the tank. The degassing extruder 2 can use a single screw or a twin screw extruder. Subsequently, the polymer treated product is molded as a threaded strand 5 by the die 3 of the tip portion of the degassing extruder 2, and cooled and solidified to almost room temperature by the cooler 4. The strands 5 become pellets 7 by the strand cutter 6.

The degassing extruder 2 is provided with a vent 9 to completely remove the drug from the resin. In the present embodiment, the pipe from the vent 9 is connected to the vacuum pump 19 via the pressure adjusting valve 91, but may be connected to the trap 16, for example.

On the other hand, the ethanol separated from the polymer processed material in the vent box 8 is at atmospheric pressure via the pressure adjusting valve 12, and is sent to the trap 16. In the trap 16, impurities, such as polyethylene mixed in ethanol, are separated by a filter and classified using a difference in boiling point. Ethanol is returned to the chemical tank 18, and impurities are sucked into the vacuum pump 19 to be incinerated by the combustion device 20.

The processing apparatus of the present embodiment is particularly effective when the vaporized drug flows back to the upstream side when the polymer compound and the gaseous drug are mixed in an extruder at a high temperature and high pressure.

Since the processing apparatus of patent documents 1 and 2 does not have the diffusion prevention mechanism of the backflow gas, when the sealing by a polymeric processing material is inadequate due to supply of unstable resin etc., the leaked high temperature gas or resin flows to the hopper periphery. There is a fear that it is ejected at once and spreads around.

In this embodiment, since the gas backflowed by the chemical | diffusion diffusion prevention box can be exhausted or collected, it can operate safely, without spreading high temperature gas and resin to the periphery.

In the case where the molten polymer processing material and the chemical agent of the gas are discharged intermittently without being continuously passed through the pressure reducing valve 11, the gas expands rapidly from the compressed state, so that the polymer processing material that is liquid is swept away to improve the momentum. Squirt. In this case, since the vent box 8 has a sufficiently large volume, it acts as a shock absorbing mechanism against pressure fluctuations and can suppress the pressure fluctuations in the discharge direction of the resin.

Therefore, the processing apparatus of this embodiment can shape the polymer treated product continuously and stably even when the gas flows back to the hopper 13 side.

In this embodiment, ethanol which is a drug was injected at 5 MPa. When the supply amount of the crosslinked polyethylene which is a raw material exceeds 50% with respect to the injection amount of ethanol, the ethanol mist is generated in the hopper 13 located upstream from the injection position, but it flows backward, but it does not diffuse at all by suction by local exhaust. Did. Further, as a result of continuing the operation with a small amount of raw material supplied, ethanol was ejected in a large amount from the hopper 13 side, but by opening the valve 23, the ethanol and the polymer treated product can be recovered by the trap 16, The operation was possible without scattering hot ethanol around.

[4th Embodiment]

Fig. 6 shows a fourth embodiment of the treatment apparatus for polymer compound according to the present invention.

In this embodiment, as shown in FIG. 6, the valve 11a is provided between the extruder 1 for material supply in FIG. 5, and the high pressure container 100 which consists of a flow-type reaction tube.

As a result of the operation as in the embodiment of Fig. 5, even when a mist of ethanol occurs, the valve 11a is closed to completely prevent backflow of ethanol in the high pressure vessel 100 to the hopper 13 side, thereby enabling safer operation. Could.

Third Comparative Example

7 shows a polymer processing apparatus of the third comparative example.

In the third comparative example, the drug diffusion prevention box is omitted in the processing apparatus shown in FIG. 5.

In the case of using the apparatus of the third comparative example, when ethanol was injected at 5 MPa, mist of ethanol was generated in the hopper 13 located upstream from the injection position, and ethanol was flowed back. Moreover, as a result of continuing operation, since a large amount of ethanol was ejected from the hopper 13 side, ethanol was scattered to around 10m, continuous operation was not able to continue.

According to the present invention, by attaching a large vent box to the degassing extruder, it becomes possible to treat the stable polymer under supercritical conditions.

In addition, by attaching a drug diffusion prevention box having a local exhaust means to the hopper of the material supply extruder, it is possible to prevent the gas from spreading around even when the high-pressure gas flows back to the hopper side of the extruder, thereby safely Can be processed.

Claims (26)

Reacting the polymer compound with a medicament in a reaction vessel to produce a polymer treated product, Introducing a polymer treated product including the drug from the reaction vessel into a degassing extruder; A vent box having a volume of one or more times the volume of the reaction vessel is connected to an upstream side of the degassing extruder, and a drug or the like contained in the polymer treated product supplied to the degassing extruder is introduced into the vent box and separated. Fair, Thereafter, the method for treating a high molecular compound consisting of the step of extruding the polymer to be processed from the extruder for degassing. The method of claim 1, wherein the extruder for degassing is a twin screw extruder. The method of processing a polymer compound according to claim 1, wherein a vent mechanism is provided on the discharge side of the degassing extruder, and the chemical agent remaining in the polymer processed material to be extruded is further removed through the vent mechanism. The method of processing a polymer compound according to claim 1, wherein the reaction vessel is composed of a flow-type reaction vessel connected to an extruder for supplying a polymer material and an extruder for supplying a polymer material. The polymer treatment product according to claim 1, wherein the polymer treatment product and the medicament are introduced into the degassing extruder from the reaction vessel under reduced pressure by a decompression means, and the polymer treatment product from which the medicament is separated from the vent box is carried out by the degassing extruder. Method of treating a polymer compound to be molded. The method according to claim 1, further comprising an impurity separation step of separating the drug from the drug in the vent box, and a drug storage step of storing the drug from which the impurity is separated and introducing the drug into the extruder for supplying the polymer material. Treatment method of having a high molecular compound. The method of processing a polymer compound according to claim 1, further comprising a cooling step of cooling the polymer processed material extruded from the degassing extruder, and a cutting step of cutting the cooled polymer processed material. The method of treating a polymer compound according to claim 1, wherein the reaction between the polymer compound and the medicament in the reaction vessel is a modification reaction, decomposition reaction or crosslinking reaction of the polymer compound. The method of treating a polymer compound according to claim 1, wherein the polymer compound is a crosslinked polymer and the drug is an alcohol or a mixture containing alcohols. The method of treating a polymer compound according to claim 1, wherein the polymer compound is pulverized in advance. In the processing apparatus of the high molecular compound which reacts a high molecular compound with a chemical | medical agent in a reaction container, and produces | generates a high molecular processed material, Decompression means for decompressing and discharging the polymer treated product including the medicament from the reaction vessel; A degassing extruder for introducing a polymer processing material containing a drug from the decompression means and extruding the polymer processing material; A back vent formed at an upstream side of the extruder for degassing; And a vent box which is connected to the back vent and has a volume of one or more times the volume of the reaction vessel and separates medicines and the like contained in the polymer treated product supplied to the degassing extruder. 12. The vent box according to claim 11, wherein an impurity separation tank for separating impurities from the separated medicine is connected to the vent box, and heating means for heating the vent box to a high temperature is provided at an outer circumference of the vent box. An apparatus for treating high molecular compounds, wherein a pressure adjustment means for maintaining a constant pressure in the impurity separation tank is provided between the tanks. The polymer compound processing apparatus according to claim 12, wherein the heating means is an electric heat heater provided at an outer circumferential portion of the polymer processed material storage part of the vent box. The polymer compound according to claim 12, wherein the heating means comprises a jacket provided at an outer periphery of the polymer treated material storage portion of the vent box, and a heating medium body circulating device for supplying the heating medium body to the jacket. Processing unit. The method of claim 12, wherein the impurity separation tank is connected to a storage tank for storing the drug is separated from the impurity, the drug of the storage tank is introduced into the polymer material supply extruder for supplying a high molecular compound by heating and boosted; And a polymer compound treating device supplied from the extruder for supplying the polymer material together with the polymer compound to the reaction vessel. The apparatus of claim 11, wherein the degassing extruder comprises a cooler for cooling the molded polymer processed material and a cutter for cutting the cooled polymer processed product. 12. The processing apparatus of claim 11, wherein the decompression means is a discharge valve. The processing apparatus for polymer compound according to claim 11, wherein the decompression means is a resistor having a plurality of holes. The processing apparatus for a polymer compound according to claim 11, wherein the decompression means is a resistor having a plurality of holes, a flow control valve, or a combination thereof. Injecting a polymer compound into an extruder for supplying materials through a hopper; Injecting a medicament into the material supply extruder while extruding a polymer compound; A polymer compound and a drug are kneaded in the extruder for supplying the material, and a mixture of the polymer compound and the drug is introduced into a reaction vessel at a high temperature and high pressure to react to produce a polymer processed product. The said hopper is equipped with the chemical | diffusion prevention box, and the chemical | medical agent process which generate | occur | produces in the said material supply extruder is exhausted locally via the said chemical | diffusion diffusion prevention box. An extruder for material supply for kneading a polymer compound and a drug and reacting with each other to produce a polymer processed product, A hopper for introducing a polymer compound into the extruder for supplying the material; Consists of a drug diffusion prevention box installed in the vicinity of the hopper, The said chemical | diffusion diffusion prevention box is a processing apparatus of the high molecular compound provided with the local exhaust apparatus which locally exhausts the chemical | medical agent gas which generate | occur | produces in the said material supply extruder via the said hopper. 22. The processing apparatus of claim 21, wherein the drug diffusion prevention box is connected to a trap via an open / close valve, and the trap is connected to a vacuum pump. 23. The on / off valve of claim 22, wherein the drug diffusion prevention box includes a gas sensor, and the gas sensor is provided between the drug diffusion prevention box and the trap when a drug gas flows back into the drug diffusion prevention box. Apparatus for processing a polymer compound to open the. The processing apparatus of a high molecular compound according to claim 21, wherein the material supply extruder has a reaction vessel connected in the extrusion direction, and a valve provided between the material supply extruder and the reaction vessel. The degassing extruder of Claim 21 connected to the rear end of the said material supply extruder, The processing apparatus of the high molecular compound which further has a vent box connected to the upstream of the said degassing extruder. 27. The processing apparatus of the polymer compound according to claim 25, wherein the drug diffusion prevention box is connected to the trap via an on / off valve, the trap is connected to a vacuum pump, and the vent box is connected to the trap via a pressure regulating valve. .

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